description
stringlengths 2.98k
3.35M
| abstract
stringlengths 94
10.6k
| cpc
int64 0
8
|
|---|---|---|
BACKGROUND OF THE INVENTION
[0001] This invention relates to Oxyindole Derivatives. These compounds have selective 5-HT 4 receptor agonistic activity. The present invention also relates to a pharmaceutical composition, method of treatment and use, comprising the above derivatives for the treatment of disease conditions mediated by 5-HT 4 receptor activity; in particular 5-HT 4 receptor agonistic activity.
[0002] In general, 5-HT 4 receptor agonists are found to be useful for the treatment of a variety of diseases such as gastroesophageal reflux disease, gastrointestinal disease, gastric motility disorder, non-ulcer dyspepsia, functional dyspepsia, irritable bowel syndrome (IBS), constipation, dyspepsia, esophagitis, gastroesophageal disease, nausea, central nervous system disease, Alzheimer's disease, cognitive disorder, emesis, migraine, neurological disease, pain, cardiovascular disorders, cardiac failure, heart arrhythmia, diabetes and apnea syndrome (See TiPs, 1992, 13, 141; Ford A. P. D. W. et al., Med. Res. Rev., 1993, 13, 633; Gullikson G. W. et al., Drug Dev. Res., 1992, 26, 405; Richard M. Eglen et al, TiPS, 1995, 16, 391; Bockaert J. Et al., CNS Drugs, 1, 6; Romanelli M. N. et al., Arzheim Forsch./Drug Res., 1993, 43, 913; Kaumann A. et al., Naunyn - Schmiedeberg's. 1991, 344, 150; and Romanelli M. N. et al., Arzheim Forsch./Drug Res., 1993, 43, 913).
[0003] U.S. Pat. No. 5,399,562A discloses indolone compounds as 5-HT 4 agonists or antagonists and/or 5-HT 3 antagonists. Especially, compounds represented by the following formula is disclosed as Example 5:
[0000]
[0004] There is a need to provide new 5-HT 4 agonists that are good drug candidates. In particular, preferred compounds should bind potently to the 5-HT 4 receptor whilst showing little affinity for other receptors and show functional activity as agonists. They should be well absorbed from the gastrointestinal tract, be metabolically stable and possess favorable pharmacokinetic properties. When targeted against receptors in the central nervous system, they should cross the blood brain barrier freely and when targeted selectively against receptors in the peripheral nervous system, they should not cross the blood brain barrier. They should be non-toxic and demonstrate few side-effects. Furthermore, the ideal drug candidate will exist in a physical form that is stable, non-hygroscopic and easily formulated.
SUMMARY OF THE INVENTION
[0005] In this invention, it has now been found out that replacing the quinuclidine ring with a piperidine ring significantly improves 5-HT 4 agonistic activity.
[0006] Therefore, it has now surprisingly been found that compounds of this invention have stronger selective 5-HT 4 agonistic compared with the prior art, and thus are useful for the treatment of disease conditions mediated by 5-HT 4 activity such as gastroesophageal reflux disease, gastrointestinal disease, gastric motility disorder, non-ulcer dyspepsia, functional dyspepsia, irritable bowel syndrome (IBS), constipation, dyspepsia, esophagitis, gastroesophageal disease, nausea, central nervous system disease, Alzheimer's disease, cognitive disorder, emesis, migraine, neurological disease, pain, cardiovascular disorders, cardiac failure, heart arrhythmia, diabetes and apnea syndrome (hereinafter these diseases are referred to as ‘5-HT 4 Diseases’).
[0007] The present invention provides a compound of the following formula (I):
[0000]
[0000] or a pharmaceutically acceptable salt thereof, wherein:
[0008] A represents a C 1 -C 4 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring being unsubstituted or substituted with a hydroxy group or a carboxy group;
[0009] R 1 represents a hydrogen atom, a halogen atom or a C 1 -C 4 alkyl group;
[0010] R 2 and R 3 independently represent a methyl or ethyl group, or R 2 and R 3 may together form a C 2 -C 4 alkylene bridge to yield 3 to 5 membered ring;
[0011] R 4 represents a hydrogen atom, a halogen atom or a hydroxy group; and
[0012] R 5 represents a hydroxy group, a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group;.
[0013] Also, the present invention provides the use of a compound of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, for the manufacture of a medicament for the treatment of a condition mediated by 5-HT 4 modulating activity; in particular, 5-HT 4 agonistic activity.
[0014] Preferably, the present invention also provides the use of a compound of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, for the manufacture of a medicament for the treatment of diseases selected from 5-HT 4 Diseases.
[0015] Also, the present invention provides a pharmaceutical composition comprising a compound of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, together with a pharmaceutically acceptable carrier for said compound.
[0016] Also, the present invention provides a pharmaceutical composition comprising a compound of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, together with a pharmaceutically acceptable carrier for said compound and another pharmacologically active agent.
[0017] Further, the present invention provides a method of treatment of a condition mediated by 5-HT 4 modulating activity, in a mammalian subject, which comprises administering to a mammal in need of such treatment a therapeutically effective amount of a compound of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein.
[0018] Examples of conditions mediated by 5-HT 4 modulating activity include, but are not limited to, 5-HT 4 Diseases.
[0019] The compounds of the present invention may show less toxicity, good absorption, distribution, good solubility, less protein binding affinity other than acid pump, less drug-drug interaction, and good metabolic stability.
DETAILED DESCRIPTION OF THE INVENTION
[0020] In the compounds of the present invention:
[0021] Where A is the C 1 -C 4 alkylene group, this C 1 -C 4 alkylene group may be a straight chain group having one to four carbon atoms, and examples include, but are not limited to, a methylene, ethylene, trimethylene and tetramethylene. Of these, methylene or ethylene is preferred; ethylene is more preferred.
[0022] Where R 2 and R 3 form the C 2 -C 4 alkylene bridge to yield the 3 to 5 membered ring, this 3 to 5 membered ring may be a cycloalkyl group having three to five carbon atoms, and examples include, but are not limited to, cyclopropyl, cyclobutyl and cyclopentyl. Of these, cyclopentyl is preferred.
[0023] Where R 1 and R 4 are the halogen atom, this may be a fluorine, chlorine, bromine or iodine atom. Of these, a fluorine atom and a chlorine atom are preferred; a fluorine atom is more preferred.
[0024] Where R 1 and the substituent of A are the C 1 -C 4 alkyl group, this C 1 -C 4 alkyl group may be a straight or branched chain group having one to four carbon atoms, and examples include, but are not limited to, a methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl and tert-butyl. Of these, methyl or ethyl is preferred; methyl is more preferred for R 1 .
[0025] Where the substituent of A is the hydroxy-C 1 -C 4 alkyl group, this represents the said C 1 -C 4 alkyl group substituted with hydroxy, and examples include, but are not limited to, a hydroxymethyl, 2-h yd roxyethyl, 1-hydroxyethyl, 3-hydroxypropyl, 2-hydroxypropyl, 2-hydroxy-1-methylethyl, 4-hydroxybutyl, 3-hydroxybutyl, 2-hydroxybutyl, 3-hydroxy-2-methylpropyl and 3-hydroxy-1-methylpropyl. Of these, hydroxy-alkyl groups having from 1 to 3 carbon atoms are preferred; hydroxymethyl, 2-hydroxyethyl, and 2-hydroxypropyl are more preferred.
[0026] Where the substituent of A is the C 1 -C 2 alkoxy-C 1 -C 4 alkyl group this represents the said C 1 -C 4 alkyl group substituted with methoxy or ethoxy, and examples include, but are not limited to, a methoxymethyl, ethoxymethyl, 2-methoxyethyl, 2-ethoxyethyl, 1-methoxyethyl, 3-methoxypropyl, 3-ethoxypropyl, 2-methoxypropyl, 2-methoxy-1-methylethyl, 4-methoxybutyl, 4-ethoxybutyl, 3-methoxybutyl, 2-methoxybutyl, 3-methoxy-2-methylpropyl and 3-methoxy-1-methylpropyl. Of these, alkyloxy-alkyl groups having from 2 to 4 carbon atoms are preferred; methoxymethyl, 2-methoxyethyl and 3-methoxypropyl are more preferred.
[0027] Where 2 of the substituent of A form the bridge to yield the 3 to 6 membered ring, this may be a cycloalkyl or heterocyclyl group and examples include a cyclopropyl, cyclopentyl, cyclobutyl, cyclohexyl, methylcyclopropyl, ethylcyclopropyl, methylcyclobutyl, methylcyclopentyl, methylcyclohexyl, ethylcyclohexyl, hydroxycyclopropyl, hydroxycyclobutyl, hydroxycyclopentyl, hydroxycyclohexyl, methoxycyclopropyl, methoxycyclobutyl, methoxycyclopentyl, methoxycyclohexyl, tetrahydrofuryl and tetrahydropyranyl, preferably cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, methoxycyclohexyl and tetrahydropyranyl, and most preferably cyclobutyl, cyclopentyl, cyclohexyl and tetrahydropyranyl.
[0028] The term “treating” and “treatment”, as used herein, refers to curative, palliative and prophylactic treatment, including reversing, alleviating, inhibiting the progress of, or preventing the disorder or condition to which such term applies, or one or more symptoms of such disorder or condition.
[0029] Preferred compounds of the present invention are those compounds of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, in which:
(A) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom, a halogen atom or a C 1 -C 4 alkyl group; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring; R 4 is a hydrogen atom, a halogen atom or a hydroxy group; and R 5 is a hydroxy group, a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (B) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy- C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom or a halogen atom; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield a 5 membered ring; R 4 is a hydrogen atom; and R 5 is a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (C) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group and a hydroxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom or a fluorine atom; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield a 5 membered ring; R 4 is a hydrogen atom; and R 5 is a carboxy group or a tetrazolyl group; (D) A is
[0000]
R 1 is a hydrogen atom or a fluorine atom; R 2 and R 3 is a methyl group; R 4 is a hydrogen atom; and R 5 is a carboxy group or a tetrazolyl group
(E) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 2 substituents independently selected from the group consisting of a C 1 -C 2 alkyl group and a hydroxy-C 1 -C 2 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 4 to 6 membered ring; R 1 is a hydrogen atom or a fluorine atom; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring; R 4 is a hydrogen atom; and R 5 is a carboxy group or a tetrazolyl group;
(F) A is
[0000]
[0000] R 1 is a hydrogen atom or a fluorine atom; R 2 and R 3 is a methyl group; R 4 is a hydrogen atom; and R 5 is a carboxy group or a tetrazolyl group
(G) A is a C 1 -C 4 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring being unsubstituted or substituted with a hydroxy group or a carboxy group; R 1 is a hydrogen atom, a halogen atom or a C 1 -C 4 alkyl group; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring; R 4 is a hydrogen atom, a halogen atom or a hydroxy group; and R 5 is a hydroxy group, a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (H) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy- C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom, or a halogen atom; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring; R 4 is a hydrogen atom, a halogen atom or a hydroxy group; and R 5 is a hydroxy group, a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (I) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy- C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom, or a halogen atom; R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring; R 4 is a hydrogen atom, a fluorine atom or a hydroxy group; and R 5 is a hydroxy group, a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (J) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom or a halogen atom; R 2 and R 3 is a methyl group; R 4 is a hydrogen atom; and R 5 is a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group; (K) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group and a hydroxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom or a fluorine atom; R 2 and R 3 is a methyl group; R 4 is a hydrogen atom; and R 5 is a carboxy group or a tetrazolyl group.
[0042] Preferred classes of compounds of the present invention are those compounds of formula (I) or a pharmaceutically acceptable salt thereof, each as described herein, in which:
(a) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; R 1 is a hydrogen atom, a halogen atom or a C 1 -C 4 alkyl group; (b) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; (c) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 2 substituents independently selected from the group consisting of a C 1 -C 4 alkyl group and a hydroxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 3 to 6 membered ring; (d) A is a C 1 -C 2 alkylene group, said alkylene group being unsubstituted or substituted with 2 substituents independently selected from the group consisting of a C 1 -C 2 alkyl group and a hydroxy-C 1 -C 2 alkyl group, wherein 2 of said substituents may optionally form a bridge to yield a 4 to 6 membered ring; R 1 is a hydrogen atom or a fluorine atom; (e) A is
[0000]
(f) A is
[0000]
(g) R 1 is a hydrogen atom or a halogen atom;
(h) R 1 is a hydrogen atom or a fluorine atom;
(i) R 2 and R 3 is a methyl group, or R 2 and R 3 may together form a tetramethylene bridge to yield 5 membered ring;
(j) R 2 and R 3 is a methyl group;
(k) R 4 is a hydrogen atom;
(l) R 5 is a carboxy group, a tetrazolyl group, a 5-oxo-1,2,4-oxadiazole-3-yl group or a 5-oxo-1,2,4-thiadiazole-3-yl group;
(m) R 5 is a carboxy group or a tetrazolyl group.
Of these classes of compounds, any combination among (a) to (m) is also preferred.
[0056] One embodiment of the invention provides a compound selected from the group consisting of:
1-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid; 1-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyppiperidin-1-yl]methyl}cyclobutanecarboxylic acid; 3-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl}piperidin-1-yl]-2,2-di methylpropanoic acid;
and a pharmaceutically acceptable salt thereof.
[0060] Pharmaceutically acceptable salts of a compound of formula (I) include the acid addition salts and base salts (including disalts) thereof.
[0061] Suitable acid addition salts are formed from acids which form non-toxic salts. Examples include the acetate, adipate, aspartate, benzoate, besylate, bicarbonate/carbonate, bisulphate/sulphate, borate, camsylate, citrate, cyclamate, edisylate, esylate, formate, fumarate, gluceptate, gluconate, glucuronate, hexafluorophosphate, hibenzate, hydrochloride/chloride, hydrobromide/bromide, hydroiodide/iodide, isethionate, lactate, malate, maleate, malonate, mesylate, methylsulphate, naphthylate, 2-napsylate, nicotinate, nitrate, orotate, oxalate, palmitate, pamoate, phosphate/hydrogen phosphate/dihydrogen phosphate, pyroglutamate, saccharate, stearate, succinate, tannate, tartrate, tosylate, trifluoroacetate and xinofoate salts.
[0062] Suitable base salts are formed from bases which form non-toxic salts. Examples include the aluminum, arginine, benzathine, calcium, choline, diethylamine, diolamine, glycine, lysine, magnesium, meglumine, olamine, potassium, sodium, tromethamine and zinc salts.
[0063] For a review on suitable salts, see “Handbook of Pharmaceutical Salts: Properties, Selection, and Use” by Stahl and Wermuth (Wiley-VCH, Weinheim, Germany, 2002). A pharmaceutically acceptable salt of a compound of formula (I) may be readily prepared by mixing together solutions of the compound of formula (I) and the desired acid or base, as appropriate. The salt may precipitate from solution and be collected by filtration or may be recovered by evaporation of the solvent. The degree of ionization in the salt may vary from completely ionized to almost non-ionized.
[0064] The compounds of the invention may exist in both unsolvated and solvated forms. The term “solvate” is used herein to describe a molecular complex comprising a compound of the invention and one or more pharmaceutically acceptable solvent molecules, for example, ethanol. The term ‘hydrate’ is employed when said solvent is water.
[0065] Pharmaceutically acceptable solvates in accordance with the invention include hydrates and solvates wherein the solvent of crystallization may be isotopically substituted, e.g. D 2 O, d 6 -acetone, d 6 -DMSO.
[0066] Included within the scope of the invention are complexes such as clathrates, drug-host inclusion complexes wherein, in contrast to the aforementioned solvates, the drug and host are present in stoichiometric or non-stoichiometric amounts. Also included are complexes of the drug containing two or more organic and/or inorganic components which may be in stoichiometric or non-stoichiometric amounts. The resulting complexes may be ionized, partially ionized, or non-ionized. For a review of such complexes, see J Pharm Sci, 64 (8), 1269-1288 by Haleblian (August 1975).
[0067] Hereinafter all references to a compound of formula (I) include references to salts and complexes thereof and to solvates and complexes of salts thereof.
[0068] The term “compound of the invention” or “compounds of the invention” refers to, unless indicated otherwise, a compound of formula (I) as hereinbefore defined, polymorphs, prodrugs, and isomers thereof (including optical, geometric and tautomeric isomers) as hereinafter defined and isotopically-labeled compounds of formula (I).
[0069] Also within the scope of the invention are so-called ‘prodrugs’ of the compounds of formula (I). Thus certain derivatives of compounds of formula (I) which may have little or no pharmacological activity themselves can, when administered into or onto the body, be converted into compounds of formula (I) having the desired activity, for example, by hydrolytic cleavage. Such derivatives are referred to as “prodrugs”. Further information on the use of prodrugs may be found in ‘Pro-drugs as Novel Delivery Systems, Vol. 14, ACS Symposium Series (T Higuchi and W Stella) and ‘Bioreversible Carriers in Drug Design’, Pergamon Press, 1987 (ed. E B Roche, American Pharmaceutical Association).
[0070] Prodrugs in accordance with the invention can, for example, be produced by replacing appropriate functionalities present in the compounds of formula (I) with certain moieties known to those skilled in the art as ‘pro-moieties’ as described, for example, in “Design of Prodrugs” by H Bundgaard (Elsevier, 1985). Some examples of prodrugs in accordance with the invention include:
(i) where the compound of formula (I) contains a carboxylic acid functionality, (—COON), an ester thereof, for example, replacement of the hydrogen with (C 1 -C 8 )alkyl; (ii) where the compound of formula (I) contains an alcohol functionality (—OH), an ether thereof, for example, replacement of the hydrogen with (C 1 -C 6 )alkanoyloxymethyl.
[0073] Further examples of replacement groups in accordance with the foregoing examples and examples of other prodrug types may be found in the aforementioned references.
[0074] Finally, certain compounds of formula (I) may themselves act as prodrugs of other compounds of formula (I).
[0075] Compounds of formula (I) containing one or more asymmetric carbon atoms can exist as two or more stereoisomers. Where the compound contains, for example, a keto or oxime group or an aromatic moiety, tautomeric isomerism (“tautomerism”) can occur. It follows that a single compound may exhibit more than one type of isomerism.
[0076] Included within the scope of the present invention are all stereoisomers, geometric isomers and tautomeric forms of the compounds of formula (I), including compounds exhibiting more than one type of isomerism, and mixtures of one or more thereof. Also included are acid addition or base salts wherein the counterion is optically active, for example, D-lactate or L-lysine, or racemic, for example, DL-tartrate or DL-arginine.
[0077] The present invention includes all pharmaceutically acceptable isotopically-labeled compounds of formula (I) wherein one or more atoms are replaced by atoms having the same atomic number, but an atomic mass or mass number different from the atomic mass or mass number usually found in nature.
[0078] Examples of isotopes suitable for inclusion in the compounds of the invention include isotopes of hydrogen, such as 2 H and 3 H, carbon, such as 11 C, 13 C and 14 C, chlorine, such as 36 Cl, fluorine, such as 18 F, iodine, such as 123 I and 125 I, nitrogen, such as 13 N and 15 N, oxygen, such as 15 O, 17 O and 18 O, phosphorus, such as 32 P, and sulphur, such as 35 S.
[0079] Certain isotopically-labeled compounds of formula (I), for example, those incorporating a radioactive isotope, are useful in drug and/or substrate tissue distribution studies. The radioactive isotopes tritium, i.e. 3 H, and carbon-14, i.e. 14 C, are particularly useful for this purpose in view of their ease of incorporation and ready means of detection.
[0080] Substitution with heavier isotopes such as deuterium, i.e. 2 H, may afford certain therapeutic advantages resulting from greater metabolic stability, for example, increased in vivo half-life or reduced dosage requirements, and hence may be preferred in some circumstances.
[0081] Substitution with positron emitting isotopes, such as 11 C, 18 F, 15 O and 13 N, can be useful in Positron Emission Topography (PET) studies for examining substrate receptor occupancy.
[0082] Isotopically-labeled compounds of formula (I) can generally be prepared by conventional techniques known to those skilled in the art or by processes analogous to those described in the accompanying Examples and Preparations using an appropriate isotopically-labeled reagents in place of the non-labeled reagent previously employed.
[0083] All of the compounds of the formula (I) can be prepared by the procedures described in the general methods presented below or by the specific methods described in the Examples section and the Preparations section, or by routine modifications thereof. The present invention also encompasses any one or more of these processes for preparing the compounds of formula (I), in addition to any novel intermediates used therein.
General Synthesis
[0084] The compounds of the present invention may be prepared by a variety of processes well known for the preparation of compounds of this type, for example as shown in the following Methods A to I.
[0085] The following Methods A and B illustrate the preparation of compounds of formula (I). Methods C through I illustrate the preparation of various intermediates.
[0086] Unless otherwise indicated, R 1 , R 2 , R 3 , R 4 , R 5 and A in the following Methods are as defined above. The term “protecting group”, as used hereinafter, means a hydroxy, carboxy or amino-protecting group which is selected from typical hydroxy, carboxy or amino-protecting groups described in Protective Groups in Organic Synthesis edited by T. W. Greene et al. (John Wiley & Sons, 1999). All starting materials in the following general syntheses may be commercially available or obtained by conventional methods known to those skilled in the art, such as Howard, Harry R. et al., J. Med. Chem., 1996, 39, 143; Joensson, N et al., Acta Chem. Scand. Ser. B, 1974, 28, 225; Robertson, David W et al., J. Med. Chem., 1986, 29, 1832; Quallich, George J et al., Synthesis, 1993, 351 and the disclosures of which are incorporated herein by references.
Method A
[0087] This illustrates the preparation of compounds of formula (I).
[0000]
[0088] In Reaction Scheme A, R 5a is R 5 as defined above or a group of formula —COOR 6 , wherein R 6 is a carboxy-protecting group.
[0089] The term “carboxy-protecting group”, as used herein, signifies a protecting group capable of being cleaved by chemical means, such as hydrogenolysis, hydrolysis, electrolysis or photolysis, and such carboxy-protecting groups are described in Protective Groups in Organic Synthesis edited by T. W. Greene et al. (John Wiley & Sons, 1999). Typical carboxy-protecting groups include, but are not limited to: methyl, ethyl, t-butyl, methoxymethyl, 2,2,2-trichloroethyl, benzyl, diphenylmethyl, trimethylsilyl, t-butyldimethylsilyl and allyl. Of these groups, t-butyl, ethyl or methyl is preferred.
Step A1
[0090] In this step, the desired compound of formula (I) of the present invention is prepared by carbonylation of the compound of formula (II) with the compound of formula (III). The compound of formula (II) is commercially available or can be prepared according to the Methods C and D set forth below. The compound of formula (III) can be prepared according to Methods E to G set forth below.
[0091] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; aromatic hydrocarbons, such as benzene, toluene and nitrobenzene; ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; and amides, such as N,N-dimethylformamide and N,N-dimethylacetamide. Of these solvents, dichloromethane is preferred.
[0092] There is likewise no particular restriction on the nature of the carbonylating agents used, and any carbonylating agent commonly used in reactions of this type may equally be used here. Examples of such carbonylating agents include, but are not limited to: an imidazole derivative such as N,N′-carbonyldiimidazole (CDI); a chloroformate such as trichloromethyl chloroformate and 4-nitrophenyl chloroformate; urea; and triphosgene. Of these, 4-nitrophenyl chloroformate is preferred.
[0093] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours will usually suffice.
[0094] In the case where R 5a is a group of formula —COOR 6 , the deprotection reaction will follow to yield a carboxy group. This reaction is described in detail by T. W. Greene et al., Protective Groups in Organic Synthesis, 369-453, (1999), the disclosures of which are incorporated herein by reference. The following exemplifies a typical reaction involving the protecting group t-butyl.
[0095] The deprotection reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; and aromatic hydrocarbons, such as benzene, toluene and nitrobenzene. Of these solvents, halogenated hydrocarbons are preferred.
[0096] The deprotection reaction is carried out in the presence of an acid. There is likewise no particular restriction on the nature of the acids used, and any acid commonly used in reactions of this type may equally be used here. Examples of such acids include, but are not limited to: acids, such as hydrochloric acid, acetic acid p-toluenesulfonic acid or trifluoroacetic acid. Of these, trifluoroacetic acid is preferred.
[0097] The deprotection reaction may be carried out in the presence of a radical scavenger. There is likewise no particular restriction on the nature of the radical scavenger used, and any radical scavenger commonly used in reactions of this type may equally be used here. Examples of such radical scavengers include, but are not limited to: HBr, dimethylsulfoxide or (CH 3 CH 2 ) 3 SiH. Of these, (CH 3 CH 2 ) 3 SiH is preferred.
[0098] The deprotection reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Method B
[0099] This illustrates the preparation of compounds of formula (I).
[0000]
[0100] In Reaction Scheme B, R 5a is as defined above; R 7 is an amino-protecting group; A a is A as defined above or a C 1 -C 3 alkylene group, said alkylene group being unsubstituted or substituted with 1 to 4 substituents independently selected from the group consisting of a halogen atom, a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 alkyl group and a C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein 2 of said substituents may optionally be taken together with the carbon atom(s) to form a 3 to 6 membered ring; and X is a halogen atom such as an iodine atom, a chlorine atom or a bromine atom.
[0101] The term “amino-protecting group”, as used herein, signifies a protecting group capable of being cleaved by chemical means, such as hydrogenolysis, hydrolysis, electrolysis or photolysis, and such amino-protecting groups are described in Protective Groups in Organic Synthesis edited by T. W. Greene et al. (John Wiley & Sons, 1999). Typical amino-protecting groups include, but are not limited to, benzyl, C 2 H 5 O(C═O)—, CH 3 (C═O)—, t-butyldimethylsilyl, t-butyldiphenylsilyl, benzyloxycarbonyl and t-butoxycarbonyl. Of these groups, t-butoxycarbonyl is preferred.
Step B1
[0102] In this step, the compound of formula (V) is prepared by the deprotection of the compound of formula (IV), which may be prepared, for example, by a method similar to that described in Method A for the preparation of the compound of formula (I) from a compound of formula (II). This deprotection method is described in detail by T. W. Greene et al. [ Protective Groups in Organic Synthesis, 494-653, (1999)], the disclosures of which are incorporated herein by reference. The following exemplifies a typical method involving the protecting group t-butoxycarbonyl.
[0103] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol. Of these solvents, alcohols are preferred.
[0104] The reaction is carried out in the presence of excess amount of an acid. There is likewise no particular restriction on the nature of the acids used, and any acid commonly used in reactions of this type may equally be used here. Examples of such acids include, but are not limited to: acids, such as hydrochloric acid, or trifluoroacetic acid. Of these, hydrochloric acid is preferred.
[0105] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Step B2
[0106] In this step, the desired compound of formula (I) is prepared by the coupling (B2-a) of the compound of formula (V) prepared as described in Step B1 with the compound of formula (VI) or by the reductive amination (B2-b) of the compound of formula (V) with the compound of formula (VII).
[0000] (B2-a) Coupling with the Compound of Formula (Vi):
[0107] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amines, such as N-methylmorpholine, triethylamine, tripropylamine, tributylamine, diisopropylethylamine, dicyclohexylamine, N-methylpiperidine, N-methylpyrrolidine, pyridine, 4-pyrrolidinopyridine, N,N-dimethylaniline and N,N-diethylaniline; and amides, such as N,N-dimethylformamide and N,N-dimethylacetamide. Of these, N,N-dimethylformamide or N-methylpyrrolidine is preferred.
[0108] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the base used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include, but are not limited to: amines, such as N-methylmorpholine, triethylamine, tripropylamine, tributylamine, diisopropylethylamine, dicyclohexylamine, N-methylpiperidine, pyridine, 4-pyrrolidinopyridine, picoline, 4-(N,N-dimethylamino)pyridine, 2,6-di(t-butyl)-4-methylpyridine, quinoline, N,N-dimethylaniline, N,N-diethylaniline, 1,5-diazabicyclo[4.3.0]non-5-ene (DBN), 1,4-diazabicyclo[2.2.2]octane (DABCO) and 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU); alkali metal hydrides, such as lithium hydride, sodium hydride and potassium hydride; and alkali metal alkoxides, such as sodium methoxide, sodium ethoxide, potassium t-butoxide. Of these, diisopropylethylamine is preferred.
[0109] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 48 hours will usually suffice.
(B2-b) Reductive Amination:
[0110] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; ethers, such as diethyl ether, diisopropyl ether, dimethoxyethane, tetrahydrofuran and dioxane; alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol; acetic acid; and water. Of these solvents, halogenated hydrocarbons are preferred.
[0111] The reaction is carried out in the presence of a reducing reagent. There is likewise no particular restriction on the nature of the reducing reagents used, and any reducing reagent commonly used in reactions of this type may equally be used here. Examples of such reducing reagent include, but are not limited to: sodium borohydride, sodium cyanoborohydride and sodium triacetoxyborohydride. Of these, sodium triacetoxyborohydride is preferred. The quantity of the reducing reagent required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, that the reaction is effected under preferred conditions, a chemical equivalent ratio of 1 to 3 of the reducing reagent to the starting material will usually suffice.
[0112] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about −20° C. to about 60° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
[0113] In the case where R 5a is a group of formula —COOR 6 , the deprotection reaction will follow to yield a carboxy group. The reaction may be carried out under the same conditions as described in Step A1 of Method A.
Method C
[0114] This illustrates the preparation of compounds of formula (II).
[0000]
[0115] In Reaction Scheme C, R 8 is a C 1 -C 4 alkyl group, preferably methyl or ethyl; and X is as defined above.
Step C1
[0116] In this step, the compound of formula (X) is prepared by coupling (C1-a) of the compound of formula (VIII) and the compound of formula (IX) followed by decarboxylation (C1-b) of the resulting compound. The compound of formula (VIII) and the compound of formula (IX) are commercially available.
[0000] (C1-a) Coupling with the Compound of Formula (VIII)
[0117] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include: ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide; and sulfoxides, such as dimethyl sulfoxide and sulfolane. Of these solvents, N,N-dimethylsulfoxide is preferred.
[0118] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the bases used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include: alkali metal hydrides, such as lithium hydride, sodium hydride and potassium hydride; alkali metal alkoxides, such as sodium methoxide, sodium ethoxide and potassium t-butoxide; alkali metal carbonates, such as lithium carbonate, sodium carbonate and potassium carbonate; and alkali metal amides, such as lithium amide, sodium amide, potassium amide, lithium diisopropyl amide, potassium diisopropyl amide, sodium diisopropyl amide, lithium bis(trimethylsilyl)amide and potassium bis(trimethylsilyl)amide. Of these, sodium hydride is preferred.
[0119] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 20° C. to about 200° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 10 minutes to about 24 hours, will usually suffice.
[0000] (C1-b)Decarboxylation
[0120] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include: ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide; and sulfoxides, such as dimethyl sulfoxide and sulfolane. Of these solvents, N,N-dimethylsulfoxide is preferred.
[0121] The reaction is effected in the presence of metal halide and water. There is no particular restriction on the nature of the metal halide to be employed, provided that it has no adverse effect on the reaction at least to some extent. Examples of metal halide include: lithium chloride, potassium chloride, sodium chloride and sodium iodide. Of these lithium chloride is preferred.
[0122] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 50° C. to about 200° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 10 minutes to about 24 hours, will usually suffice.
Step C2
[0123] In this step, the compound of formula (XI) is prepared by alkylation of the compound of formula (X) with the compounds of formula R 2 —X and R 3 —X.
[0124] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include: ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide; and sulfoxides, such as dimethyl sulfoxide and sulfolane. Of these solvents, N,N-dimethylformamide is preferred.
[0125] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the bases used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include: alkali metal hydrides, such as lithium hydride, sodium hydride and potassium hydride; alkali metal alkoxides, such as sodium methoxide, sodium ethoxide and potassium t-butoxide; alkali metal carbonates, such as lithium carbonate, sodium carbonate and potassium carbonate; alkali metal amides, such as lithium amide, sodium amide, potassium amide, lithium diisopropyl amide, potassium diisopropyl amide, sodium diisopropyl amide, lithium bis(trimethylsilyl)amide and potassium bis(trimethylsilyl)amide; and organic lithiums, such as n-butyl lithium, sec-butyl lithium, t-butyl lithium and phenyl lithium. Of these, sodium hydride or n-butyl lithium is preferred.
[0126] The reaction may be conducted in the presence or absence of additives such as 16-crown-6, N,N,N′,N′-tetramethylethylene diamine (TMEDA) and hexamethylphosphoric triamide (HMPA). Of these additives, 16-crown-6 or TMEDA is preferred.
[0127] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 50° C. to about 200° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 10 minutes to about 24 hours, will usually suffice.
Step C3
[0128] In this step, the compound of formula (II) is prepared by annealing of the compound of formula (XI) under the reductive condition.
[0129] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include: alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol; and esters, such as ethyl acetate and propyl acetate. Of these solvents, methanol is preferred.
[0130] The reaction is carried out in the presence of a reducing agent. There is likewise no particular restriction on the nature of the reducing agents used, and any reducing agent commonly used in reactions of this type may equally be used here. Examples of such reducing agents include: combinations of a hydrogen supplier, such as hydrogen gas and ammonium formate, and a catalyst, such as palladium-carbon, platinum and Raney nickel; and a combination of metals, such as zinc and iron, and acids, such as hydrochloric acid, acetic acid and acetic acid-ammonium chloride complex. Of these the combination of iron and acetic acid is preferred.
[0131] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 10° C. to about 50° C. in the case employing the combination of the hydrogen supplier and the catalyst as the reducing agent, or from about 50° C. to about 200° C. in the case employing the combination of the metals and acids as the reducing agent. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 10 minutes to about 24 hours, will usually suffice.
Method D
[0132] This illustrates the preparation of compounds of formula (II).
[0000]
[0133] In Reaction Scheme D, R 8 and X are each as defined above.
Step D1
[0134] In this step, the compound of formula (XII) is prepared by annealing of the compound of formula (X) which is commercially available or prepared according to Step C1 of Method C. The reaction may be carried out under the same conditions as described in Step C3 of Method C.
Step D2
[0135] In this step, the compound of formula (II) is prepared by alkylation of the compound of formula (XII) with the compounds of formula R 2 —X and R 3 —X. The reaction may be carried out under the same conditions as described in Step C2 of Method C.
Method E
[0136] This illustrates the preparation of the compound of formula (III).
[0000]
[0137] In Reaction Scheme E, X, A a , and R 3a are each as defined above; and R 9 is an amino-protecting group.
Step E1
[0138] In this step, the compound of formula (XIV) is prepared by the coupling of the compound of formula (XIII) with a compound of formula (VI) or by the reductive amination of the compound of formula (XIII) with the compound of formula (VII). The compound of formula (XIII) can be prepared according to Methods H and I set forth below or is commercially available.
Step E2
[0139] In this step, the compound of formula (III) is prepared by the deprotection of the compound of formula (XIV) prepared as described in Step E1. The reaction may be carried out under the same conditions as described in Step B1 of Method B.
Method F
[0140] This illustrates the preparation of the compound of formula (III) wherein A is A b .
[0000]
[0141] In Reaction Scheme F, R 5a , R 6 and R 9 are each as defined above; R 10 is a silyl group such as t-butyldimethylsilyl, t-butyldiphenylsilyl, triethylsilyl or trimethylsilyl, preferably trimethylsilyl; R 11 and R 12 independently represent a halogen atom, a C 1 -C 4 alkyl group, a hydroxy-C 1 -C 4 — alkyl group and an C 1 -C 2 alkoxy-C 1 -C 4 alkyl group, wherein R 11 and R 12 may optionally be taken together with the carbon atom to which they are attached to form a 3 to 6 membered ring; A b is A as defined above with proviso a methylene group and a substituted methylene group are excluded; and Y is an alkoxy group having 1 to 4 carbon atoms, an imidazolyl group or a pthalimidyl group.
Step F1
[0142] In this step, the compound of formula (XV) is prepared by condensation of the compound of formula (XIII) with the compound of formula H—Y in the presence of paraformaldehyde. A compound of formula (XIII) can be prepared according to Method H and I or is commercially available.
[0143] In the case that Y is not an alkoxy group, the reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol;. Of these, dichloromethane or ethanol is preferred.
[0144] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 48 hours, will usually suffice.
Step F2
[0145] In this step, the compound of formula (IIIa) is prepared by Mannnich reaction of the compound of formula (XV) with the compound of formula (XVI).
[0146] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; nitriles, such as acetonitrile and benzonitrile; and amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide. Of these solvents, dichloromethane is preferred.
[0147] The reaction is carried out in the presence of a Lewis acid. There is likewise no particular restriction on the nature of the Lewis acids used, and any Lewis acid commonly used in reactions of this type may equally be used here. Examples of such Lewis acid include, but are not limited to: BF 3 , AlCl 3 , FeCl 3 , MgCl 2 , AgCl, Fe(NO 3 ) 3 , CF 3 SO 3 Si(CH 3 ) 3 , Yb(CF 3 SO 3 ) 3 and SnCl 4 . Of these, Yb(CF 3 SO 3 ) 3 , CF 3 SO 3 Si(CH 3 ) 3 or MgCl 2 is preferred.
[0148] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Method G
[0149] This illustrates the preparation of the compound of formula (III) wherein R 4 is a hydrogen atom and A is A b .
[0000]
[0150] In Reaction Scheme G, A a , A b and R 5a are each as defined above; each of R and R′ is a C 1 -C 4 alkyl group, preferably a methyl group, or an aralkyl group such as a benzyl or phenethyl group, preferably a benzyl group.
Step G1
[0151] In this step, the compound of formula (XVI) is prepared by reduction of the cyano group of the compound of formula (XV), which is commercially available.
[0152] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; aromatic hydrocarbons, such as benzene, toluene and nitrobenzene; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol. Of these, methanol is preferred.
[0153] The reaction is carried out in the presence of a reducing agent. There is likewise no particular restriction on the nature of the reducing agents used, and any reducing agent commonly used in reactions of this type may equally be used here. Examples of such reducing agents include, but are not limited to: metal borohydrides such as sodium borohydride and sodium cyanoborohydride; combinations of hydrogen gas and a catalyst such as palladium-carbon, platinum and Raney nickel; and hydride compounds such as lithium aluminum hydride, and diisobutyl aluminum hydride. Of these, Raney nickel is preferred.
[0154] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Step G2
[0155] In this step, the compound of formula (XVIII) is prepared by reacting a compound of formula (XVII), which is commercially available, with a compound of formula (XVI).
[0156] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: water; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol. Of these, a mixture of water and ethanol is preferred.
[0157] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the base used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include, but are not limited to: alkali metal hydroxides, such as lithium hydroxide, sodium hydroxide and potassium hydroxide; alkali metal alkoxides, such as sodium methoxide, sodium ethoxide, potassium t-butoxide; and alkali metal carbonates, such as lithium carbonate, sodium carbonate and potassium carbonate. Of these, potassium carbonate is preferred.
[0158] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Step G3
[0159] In this step, the compound of formula (XIX) is prepared by converting the oxo group of the compound of formula (XVIII) to a cyano group in the presence of p-toluenesulfonylmethyl isocyanide.
[0160] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: ethers, such as diethyl ether, diisopropyl ether, ethylene glycol dimethyl ether, tetrahydrofuran and dioxane; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol. Of these, a mixture of ethylene glycol dimethyl ether and ethanol is preferred.
[0161] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the base used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include, but are not limited to: alkali metal alkoxides, such as sodium methoxide, sodium ethoxide and potassium t-butoxide. Of these, potassium t-butoxide is preferred.
[0162] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Step G4
[0163] In this step, the compound of formula (IIIb) is prepared by reduction of the cyano group of the compound of formula (XIX). The reaction may be carried out under the same conditions as described in Step G1 of Method G.
Method H
[0164] This illustrates the preparation of compounds of formula (XIII) wherein R 4 is a halogen atom.
[0000]
[0165] In Reaction Scheme H, R 4a is a halogen atom; R 9 is as defined above; and R 13 is an amino-protecting group, preferably a benzoyl group.
Step H1
[0166] In this step, the compound of formula (XXI) is prepared by converting the carbonyl group of the compound of formula (XX) into the epoxide group.
[0167] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide; sulfoxide such as dimethyl sulfoxide or sulfolane. Of these solvents, dimethyl sulfoxide is preferred.
[0168] The reaction is carried out in the presence of a base. There is likewise no particular restriction on the nature of the base used, and any base commonly used in reactions of this type may equally be used here. Examples of such bases include, but are not limited to: alkali metal alkoxides, such as sodium methoxide, sodium ethoxide and potassium t-butoxide; and alkali metal carbonates, such as lithium carbonate, sodium carbonate and potassium carbonate. Of these, potassium t-butoxide is preferred.
[0169] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours will usually suffice.
Step H2
[0170] In this step, the compound of formula (XXII) is prepared by reacting a hydrogen halide with the compound of formula (XXI).
[0171] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide. Of these solvents, tetrahydrofuran is preferred.
[0172] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours will usually suffice.
Step H3
[0173] In this step, the compound of formula (XXIII) is prepared by reaction of the compound of formula (XXII) with sodium azide (H3-a) followed by the reduction of the azide group (H3-b).
[0000] (H3-a) Reaction with Sodium Azide:
[0174] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; amides, such as formamide, N,N-dimethylformamide, N,N-dimethylacetamide and hexamethylphosphoric triamide; and sulfoxide such as dimethyl sulfoxide and sulfolane. Of these solvents, N,N-dimethylformamide is preferred.
[0175] Before adding sodium azide, the hydroxy group is converted to a leaving group, such as a methylsulfonyl group, a trifluoromethylsulfonyl group and 4-methyl phenylsulfonyl group by adding reagents, such as trifluoromethanelsulfonylchloride, mesyl chloride and tosyl chloride. Of these reagents, mesyl chloride is preferred.
[0176] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
(H3-b) Reduction:
[0177] The reaction may be carried out under the same conditions as described in Step G1 of Method G.
Step H4
[0178] In this step, the compound of formula (XIIIa) is prepared by introducing the amino-protecting group R 9 to the primary amino group (H4-a) and selectively deprotecting the amino-protecting group R 13 of the secondary amino group (H4-b).
(H4-a) Introduction of the Amino-Protecting Group:
[0179] This reaction is described in detail by T. W. Greene et al. [ Protective Groups in Organic Synthesis, 494-653, (1999)], the disclosures of which are incorporated herein by reference. The following exemplifies a typical reaction involving the protecting group t-butoxycarbonyl.
[0180] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: water; ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane; and sulfoxide such as dimethyl sulfoxide and sulfolane. Of these solvents, tetrahydrofuran is preferred.
[0181] The reaction is carried out in the presence of reagent. There is likewise no particular restriction on the nature of the reagents used, and any reagent commonly used in reactions of this type may equally be used here. Examples of such reagents include, but are not limited to: di-t-butyl carbonate and 1-(t-butoxycarbonyl)benztriazole. Of these, di-t-butyl carbonate is preferred.
[0182] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120°. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
(H4-b) Deprotection:
[0183] This method is described in detail by T. W. Greene et al., Protective Groups in Organic Synthesis, 494-653, (1999), the disclosures of which are incorporated herein by reference. The following exemplifies a typical method involving the benzoyl protecting group in the presence of combinations of hydrogen gas and a catalyst such as palladium-carbon or platinum.
[0184] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol; and ethers, such as diethyl ether, diisopropyl ether, tetrahydrofuran and dioxane. Of these solvents, methanol is preferred.
[0185] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 120° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Method I
[0186] This illustrates the preparation of compounds of formula (XIII) wherein R 4 is a hydroxy group.
[0000]
[0187] In Reaction Scheme I, R 9 and R 13 are each as defined above.
Step 11
[0188] In this step, the compound of formula (XXIV) is prepared by reacting the carbonyl group of the compound of formula (XX), which is commercially available, with trimethylsilyl cyanide.
[0189] The reaction is normally and preferably effected in the presence of solvent. There is no particular restriction on the nature of the solvent to be employed, provided that it has no adverse effect on the reaction or the reagents involved and that it can dissolve reagents, at least to some extent. Examples of suitable solvents include, but are not limited to: aromatic hydrocarbons, such as benzene, toluene and nitrobenzene; halogenated hydrocarbons, such as dichloromethane, chloroform, carbon tetrachloride and 1,2-dichloroethane; ethers, such as diethyl ether, diisopropyl ether, ethylene glycol dimethyl ether, tetrahydrofuran and dioxane; nitriles, such as acetonitrile and benzonitrile; and alcohols, such as methanol, ethanol, propanol, 2-propanol and butanol. Of these, toluene is preferred.
[0190] The reaction is carried out in the presence of a reagent. There is likewise no particular restriction on the nature of the reagents used, and any reagent commonly used in reactions of this type may equally be used here. Examples of such reagent include, but are not limited to: Lewis acids, such as BF 3 , AlCl 3 , FeCl 3 , AgCl, ZnI 2 , Fe(NO 3 ) 3 , CF 3 SO 3 Si(CH 3 ) 3 , Yb(CF 3 SO 3 ) 3 and SnCl 4 ; bases, such as CaO; ethers, such as 18-crown-6; acids, such as Amberlite XAD-4 resin. Of these, Znl 2 is preferred.
[0191] The reaction can take place over a wide range of temperatures, and the precise reaction temperature is not critical to the invention. The preferred reaction temperature will depend upon such factors as the nature of the solvent, and the starting materials. However, in general, it is convenient to carry out the reaction at a temperature of from about 0° C. to about 100° C. The time required for the reaction may also vary widely, depending on many factors, notably the reaction temperature and the nature of the starting materials and solvent employed. However, provided that the reaction is effected under the preferred conditions outlined above, a period of from about 5 minutes to about 24 hours, will usually suffice.
Step I2
[0192] In this step, the compound of formula (XXV) is prepared by converting the cyano group of the compound of formula (XXII) to an amino group. The reaction may be carried out under the same conditions as described in Step G1 of Method.
Step I3
[0193] In this step, the compound of formula (XIIIa) is prepared by protecting and deprotecting the amino groups of the compound of formula (XXV). The reaction may be carried out under the same conditions as described in Step H4 of Method H.
[0194] The compounds of formula (I), and the intermediates above-mentioned preparation methods can be isolated and purified by conventional procedures, such as distillation, recrystallization or chromatographic purification.
[0195] Compounds of the invention intended for pharmaceutical use may be administered as crystalline or amorphous products. They may be obtained, for example, as solid plugs, powders, or films by methods such as precipitation, crystallization, freeze drying, spray drying, or evaporative drying. Microwave or radio frequency drying may be used for this purpose.
[0196] Conventional techniques for the preparation/isolation of individual enantiomers include chiral synthesis from a suitable optically pure precursor or resolution of the racemate (or the racemate of a salt or derivative) using, for example, chiral high pressure liquid chromatography (HPLC).
[0197] Alternatively, a method of optical resolution of a racemate (or a racemic precursor) can be appropriately selected from conventional procedures, for example, preferential crystallization, or resolution of diastereomeric salts between a basic moiety of the compound of formula (I) and a suitable optically active acid such as tartaric acid.
[0198] Compounds of the invention intended for pharmaceutical use may be administered as crystalline or amorphous products. They may be obtained, for example, as solid plugs, powders, or films by methods such as precipitation, crystallization, freeze drying, spray drying, or evaporative drying. Microwave or radio frequency drying may be used for this purpose.
[0199] They may be administered alone or in combination with one or more other compounds of the invention or in combination with one or more other drugs (or as any combination thereof). Generally, they will be administered as a pharmaceutical composition or formulation in association with one or more pharmaceutically acceptable carriers or excipients. The term “carrier” or “excipient” is used herein to describe any ingredient other than the compound(s) of the invention. The choice of carrier or excipient will to a large extent depend on factors such as the particular mode of administration, the effect of the excipient on solubility and stability, and the nature of the dosage form.
[0200] Pharmaceutical compositions suitable for the delivery of compounds of the present invention and methods for their preparation will be readily apparent to those skilled in the art. Such compositions and methods for their preparation may be found, for example, in ‘Remington's Pharmaceutical Sciences’, 19th Edition (Mack Publishing Company, 1995).
Oral Administration
[0201] The compounds of the invention may be administered orally. Oral administration may involve swallowing, so that the compound enters the gastrointestinal tract, or buccal or sublingual administration may be employed by which the compound enters the blood stream directly from the mouth.
[0202] Formulations suitable for oral administration include solid formulations such as, for example, tablets, capsules containing particulates, liquids, or powders, lozenges (including liquid-filled), chews, multi- and nano-particulates, gels, solid solution, liposome, films (including muco-adhesive), ovules, sprays and liquid formulations.
[0203] Liquid formulations include, for example, suspensions, solutions, syrups and elixirs. Such formulations may be employed as fillers in soft or hard capsules and typically comprise a carrier, for example, water, ethanol, polyethylene glycol, propylene glycol, methylcellulose, or a suitable oil, and one or more emulsifying agents and/or suspending agents. Liquid formulations may also be prepared by the reconstitution of a solid, for example, from a sachet.
[0204] The compounds of the invention may also be used in fast-dissolving, fast-disintegrating dosage forms such as those described in Expert Opinion in Therapeutic Patents, 11 (6), 981-986 by Liang and Chen (2001).
[0205] For tablet dosage forms, depending on dose, the drug may make up from about 1 wt % to about 80 wt % of the dosage form, more typically from about 5 wt % to about 60 wt % of the dosage form. In addition to the drug, tablets generally contain a disintegrant. Examples of disintegrants include sodium starch glycolate, sodium carboxymethyl cellulose, calcium carboxymethyl cellulose, croscarmellose sodium, crospovidone, polyvinylpyrrolidone, methyl cellulose, microcrystalline cellulose, lower alkyl-substituted hydroxypropyl cellulose, starch, pregelatinised starch and sodium alginate. Generally, the disintegrant will comprise from about 1 wt % to about 25 wt %, preferably from about 5 wt % to about 20 wt % of the dosage form.
[0206] Binders are generally used to impart cohesive qualities to a tablet formulation. Suitable binders include microcrystalline cellulose, gelatin, sugars, polyethylene glycol, natural and synthetic gums, polyvinylpyrrolidone, pregelatinised starch, hydroxypropyl cellulose and hydroxypropyl methylcellulose.
[0207] Tablets may also contain diluents, such as lactose (monohydrate, spray-dried monohydrate, anhydrous and the like), mannitol, xylitol, dextrose, sucrose, sorbitol, microcrystalline cellulose, starch and dibasic calcium phosphate dihydrate.
[0208] Tablets may also optionally comprise surface active agents, such as sodium lauryl sulfate and polysorbate 80, and glidants such as silicon dioxide and talc. When present, surface active agents may comprise from about 0.2 wt % to about 5 wt % of the tablet, and glidants may comprise from about 0.2 wt % to about 1 wt % of the tablet.
[0209] Tablets also generally contain lubricants such as magnesium stearate, calcium stearate, zinc stearate, sodium stearyl fumarate, and mixtures of magnesium stearate with sodium lauryl sulphate. Lubricants generally comprise from about 0.25 wt % to about 10 wt %, preferably from about 0.5 wt % to about 3 wt % of the tablet.
[0210] Other possible ingredients include anti-oxidants, colorants, flavoring agents, preservatives and taste-masking agents.
[0211] Exemplary tablets contain up to about 80% drug, from about 10 wt % to about 90 wt % binder, from about 0 wt % to about 85 wt % diluent, from about 2 wt % to about 10 wt % disintegrant, and from about 0.25 wt % to about 10 wt % lubricant.
[0212] Tablet blends may be compressed directly or by roller to form tablets. Tablet blends or portions of blends may alternatively be wet-, dry-, or melt-granulated, melt congealed, or extruded before tabletting. The final formulation may comprise one or more layers and may be coated or uncoated; it may even be encapsulated.
[0213] The formulation of tablets is discussed in “ Pharmaceutical Dosage Forms: Tablets, Vol. 1”, by H. Lieberman and L. Lachman, Marcel Dekker, N.Y., N.Y., 1980 (ISBN 0-8247-6918-X).
[0214] Solid formulations for oral administration may be formulated to be immediate and/or modified release. Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted and programmed release.
[0215] Suitable modified release formulations for the purposes of the invention are described in U.S. Pat. No. 6,106,864. Details of other suitable release technologies such as high energy dispersions and osmotic and coated particles are to be found in Verma et al, Pharmaceutical Technology On-line, 25(2), 1-14 (2001). The use of chewing gum to achieve controlled release is described in WO 00/35298.
Parenteral Administration
[0216] The compounds of the invention may also be administered directly into the blood stream, into muscle, or into an internal organ. Suitable means for parenteral administration include intravenous, intraarterial, intraperitoneal, intrathecal, intraventricular, intraurethral, intrasternal, intracranial, intramuscular and subcutaneous. Suitable devices for parenteral administration include needle (including microneedle) injectors, needle-free injectors and infusion techniques.
[0217] Parenteral formulations are typically aqueous solutions which may contain excipients such as salts, carbohydrates and buffering agents (preferably to a pH of from about 3 to about 9), but, for some applications, they may be more suitably formulated as a sterile non-aqueous solution or as a dried form to be used in conjunction with a suitable vehicle such as sterile, pyrogen-free water.
[0218] The preparation of parenteral formulations under sterile conditions, for example, by lyophilization, may readily be accomplished using standard pharmaceutical techniques well known to those skilled in the art.
[0219] The solubility of compounds of formula (I) used in the preparation of parenteral solutions may be increased by the use of appropriate formulation techniques, such as the incorporation of solubility-enhancing agents.
[0220] Formulations for parenteral administration may be formulated to be immediate and/or modified release. Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted and programmed release. Thus compounds of the invention may be formulated as a solid, semi-solid, or thixotropic liquid for administration as an implanted depot providing modified release of the active compound. Examples of such formulations include drug-coated stents and PGLA microspheres.
Topical Administration
[0221] The compounds of the invention may also be administered topically to the skin or mucosa, that is, dermally or transdermally. Typical formulations for this purpose include gels, hydrogels, lotions, solutions, creams, ointments, dusting powders, dressings, foams, films, skin patches, wafers, implants, sponges, fibers, bandages and microemulsions. Liposomes may also be used. Typical carriers include alcohol, water, mineral oil, liquid petrolatum, white petrolatum, glycerin, polyethylene glycol and propylene glycol. Penetration enhancers may be incorporated—see, for example, J Pharm Sci, 88 (10), 955-958 by Finnin and Morgan (October 1999).
[0222] Other means of topical administration include delivery by electroporation, iontophoresis, phonophoresis, sonophoresis and microneedle or needle-free (e.g. Powderject™, Bioject™, etc.) injection.
[0223] Formulations for topical administration may be formulated to be immediate and/or modified release. Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted and programmed release.
Inhaled/Intranasal Administration
[0224] The compounds of the invention can also be administered intranasally or by inhalation, typically in the form of a dry powder (either alone, as a mixture, for example, in a dry blend with lactose, or as a mixed component particle, for example, mixed with phospholipids, such as phosphatidylcholine) from a dry powder inhaler or as an aerosol spray from a pressurized container, pump, spray, atomizer (preferably an atomizer using electrohydrodynamics to produce a fine mist), or nebulizer, with or without the use of a suitable propellant, such as 1,1,1,2-tetrafluoroethane or 1,1,1,2,3,3,3-heptafluoropropane. For intranasal use, the powder may comprise a bioadhesive agent, for example, chitosan or cyclodextrin. The pressurized container, pump, spray, atomizer, or nebulizer contains a solution or suspension of the compound(s) of the invention comprising, for example, ethanol, aqueous ethanol, or a suitable alternative agent for dispersing, solubilizing, or extending release of the active, a propellant(s) as solvent and an optional surfactant, such as sorbitan trioleate, oleic acid, or an oligolactic acid.
[0225] Prior to use in a dry powder or suspension formulation, the drug product is micronized to a size suitable for delivery by inhalation (typically less than 5 microns). This may be achieved by any appropriate comminuting method, such as spiral jet milling, fluid bed jet milling, supercritical fluid processing to form nanoparticles, high pressure homogenization, or spray drying.
[0226] Capsules (made, for example, from gelatin or HPMC), blisters and cartridges for use in an inhaler or insufflator may be formulated to contain a powder mix of the compound of the invention, a suitable powder base such as lactose or starch and a performance modifier such as l-leucine, mannitol, or magnesium stearate. The lactose may be anhydrous or in the form of the monohydrate, preferably the latter. Other suitable excipients include dextran, glucose, maltose, sorbitol, xylitol, fructose, sucrose and trehalose.
[0227] A suitable solution formulation for use in an atomizer using electrohydrodynamics to produce a fine mist may contain from about 1 μg to about 20 mg of the compound of the invention per actuation and the actuation volume may vary from about 1 μl to about 100 μl. A typical formulation may comprise a compound of formula (I), propylene glycol, sterile water, ethanol and sodium chloride. Alternative solvents which may be used instead of propylene glycol include glycerol and polyethylene glycol.
[0228] Suitable flavors, such as menthol and levomenthol, or sweeteners, such as saccharin or saccharin sodium, may be added to those formulations of the invention intended for inhaled/intranasal administration. Formulations for inhaled/intranasal administration may be formulated to be immediate and/or modified release using, for example, poly(DL-lactic-coglycolic acid (PGLA). Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted and programmed release.
[0229] In the case of dry powder inhalers and aerosols, the dosage unit is determined by means of a valve which delivers a metered amount. Units in accordance with the invention are typically arranged to administer a metered dose or “puff” containing from about 1 to about 100 μg of the compound of formula (I). The overall daily dose will typically be in the range about 50 μg to about 20 mg which may be administered in a single dose or, more usually, as divided doses throughout the day.
Rectal/Intravaginal Administration
[0230] The compounds of the invention may be administered rectally or vaginally, for example, in the form of a suppository, pessary, or enema. Cocoa butter is a traditional suppository base, but various alternatives may be used as appropriate.
[0231] Formulations for rectal/vaginal administration may be formulated to be immediate and/or modified release. Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted and programmed release.
Ocular/Aural Administration
[0232] The compounds of the invention may also be administered directly to the eye or ear, typically in the form of drops of a micronized suspension or solution in isotonic, pH-adjusted, sterile saline. Other formulations suitable for ocular and aural administration include ointments, biodegradable (e.g. absorbable gel sponges, collagen) and non-biodegradable (e.g. silicone) implants, wafers, lenses and particulate or vesicular systems, such as niosomes or liposomes. A polymer such as crossed-linked polyacrylic acid, polyvinylalcohol, hyaluronic acid, a cellulosic polymer, for example, hydroxypropylmethylcellulose, hydroxyethylcellulose, or methyl cellulose, or a heteropolysaccharide polymer, for example, gelan gum, may be incorporated together with a preservative, such as benzalkonium chloride. Such formulations may also be delivered by iontophoresis.
[0233] Formulations for ocular/aural administration may be formulated to be immediate and/or modified release. Modified release formulations include delayed-, sustained-, pulsed-, controlled-, targeted, or programmed release.
Other Technologies
[0234] The compounds of the invention may be combined with soluble macromolecular entities, such as cyclodextrin and suitable derivatives thereof or polyethylene glycol-containing polymers, in order to improve their solubility, dissolution rate, taste-masking, bioavailability and/or stability for use in any of the aforementioned modes of administration.
[0235] Drug-cyclodextrin complexes, for example, are found to be generally useful for most dosage forms and administration routes. Both inclusion and non-inclusion complexes may be used. As an alternative to direct complexation with the drug, the cyclodextrin may be used as an auxiliary additive, i.e. as a carrier, diluent, or solubilizer. Most commonly used for these purposes are alpha-, beta- and gamma-cyclodextrins, examples of which may be found in WO 91/11172, WO 94/02518 and WO 98/55148.
Kit-of-Parts
[0236] Inasmuch as it may be desirable to administer a combination of active compounds, for example, for the purpose of treating a particular disease or condition, it is within the scope of the present invention that two or more pharmaceutical compositions, at least one of which contains a compound in accordance with the invention, may conveniently be combined in the form of a kit suitable for coadministration of the compositions.
[0237] Thus the kit of the invention comprises two or more separate pharmaceutical compositions, at least one of which contains a compound of formula (I) in accordance with the invention, and means for separately retaining said compositions, such as a container, divided bottle, or divided foil packet. An example of such a kit is the familiar blister pack used for the packaging of tablets, capsules and the like.
[0238] The kit of the invention is particularly suitable for administering different dosage forms, for example, oral and parenteral, for administering the separate compositions at different dosage intervals, or for titrating the separate compositions against one another. To assist compliance, the kit typically comprises directions for administration and may be provided with a so-called memory aid.
Dosage
[0239] For administration to human patients, the total daily dose of the compounds of the invention is typically in the range of about 0.05 mg to about 100 mg depending, of course, on the mode of administration, preferred in the range of about 0.1 mg to about 50 mg and more preferred in the range of about 0.5 mg to about 20 mg. For example, oral administration may require a total daily dose of from about 1 mg to about 20 mg, while an intravenous dose may only require from about 0.5 mg to about 10 mg. The total daily dose may be administered in single or divided doses.
[0240] These dosages are based on an average human subject having a weight of about 65 kg to about 70 kg. The physician will readily be able to determine doses for subjects whose weight falls outside this range, such as infants and the elderly.
[0241] As discussed above, a compound of the invention exhibits 5-HT 4 agonist activity. A 5-HT 4 agonist of the present invention may be usefully combined with at least one other pharmacologically active agent or compound, particularly in the treatment of gastroesophageal reflux disease. For example, a 5-HT 4 agonist, particularly a compound of the formula (I), or a pharmaceutically acceptable salt or solvate thereof, as defined above, may be administered simultaneously, sequentially or separately in combination with one or more pharmacologically active agents selected from:
[0000] (i) histamine H 2 receptor antagonists, e.g. ranitidine, lafutidine, nizatidine, cimetidine, famotidine and roxatidine;
(ii) proton pump inhibitors, e.g. omeprazole, esomeprazole, pantoprazole, rabeprazole, tenatoprazole, ilaprazole and lansoprazole;
(iii) Acid pump antagonists, e.g. soraprazan, revaprazan (YH-1885), AZD-0865, CS-526, AU-2064 and YJA-20379-8;
(iv) oral antacid mixtures, e.g. Maalox®, Aludrox® and Gaviscon®;
(v) mucosal protective agents, e.g. polaprezinc, ecabet sodium, rebamipide, teprenone, cetraxate, sucralfate, chloropylline-copper and plaunotol;
(vi) GABA B agonists, e.g. baclofen and AZD-3355;
(vii) α2 agonists, e.g. clonidine, medetomidine, lofexidine, moxonidine, tizanidine, guanfacine, guanabenz, talipexole and dexmedetomidine;
(viii) Xanthin derivatives, e.g. Theophylline, aminophylline and doxofylline;
(ix) calcium channel blockers, e.g. aranidipine, lacidipine, falodipine, azelnidipine, clinidipine, lomerizine, diltiazem, gallopamil, efonidipine, nisoldipine, amlodipine, lercanidipine, bevantolol, nicardipine, isradipine, benidipine, verapamil, nitrendipine, barn idipine, propafenone, manidipine, bepridil, nifedipine, nilvadipine, nimodipine, and fasudil;
(x) benzodiazepine agonists, e.g. diazepam, zaleplon, zolpidem, haloxazolam, clonazepam, prazepam, quazepam, flutazolam, triazolam, lormetazepam, midazolam, tofisopam, clobazam, flunitrazepam and flutoprazepam;
(xi) prostaglandin analogues, e.g. Prostaglandin, misoprostol, treprostinil, esoprostenol, latanoprost, iloprost, beraprost, enprostil, ibudilast and ozagrel;
(xii) histamine H 3 agonists, e.g. R-alpha-methylhistamine and BP-294;
(xiii) anti-gastric agents, e.g. Anti-gastrin vaccine, itriglumide and Z-360;
(xiv) 5-HT 3 antagonists, e.g. dolasetron, palonosetron, alosetron, azasetron, ramosetron, mitrazapine, granisetron, tropisetron, E-3620, ondansetron and indisetron;
(xv) tricyclic antidepressants, e.g. imipramine, amitriptyline, clomipramine, amoxapine and lofepramine;
(xvi) GABA agonists, e.g. gabapentin, topiramate, cinolazepam, clonazepam, progabide, brotizolam, zopiclone, pregabalin and eszopiclone;
(xvii) opioid analgesics, e.g. morphine, heroin, hydromorphone, oxymorphone, levorphanol, levallorphan, methadone, meperidine, fentanyl, cocaine, codeine, dihydrocodeine, oxycodone, hydrocodone, propoxyphene, nalmefene, nalorphine, naloxone, naltrexone, buprenorphine, butorphanol, nalbuphine and pentazocine;
(xviii) somatostatin analogues, e.g. octreotide, AN-238 and PTR-3173;
(xix) CI Channel activator: e.g. lubiprostone;
(xx) selective serotonin reuptake inhibitors, e.g. sertraline, escitalopram, fluoxetine, nefazodone, fluvoxamine, citalopram, milnacipran, paroxetine, venlafaxine, tramadol, sibutramine, duloxetine, desvenlafaxine and dapoxetine;
(xxi) anticholinergics, e.g. dicyclomine and hyoscyamine;
(xxii) laxatives, e.g. Trifyba®, Fybogel®, Konsyl®, Isogel®, Regulan®, Celevac® and Normacol®;
(xxiii) fiber products, e.g. Metamucil®;
(xxiv) antispasmodics, e.g.: mebeverine;
(xxv) dopamine antagonists, e.g. metoclopramide, domperidone and levosulpiride;
(xxvi) cholinergics, e.g. neostigmine
(xxvii) AChE inhibitors, e.g. galantamine, metrifonate, rivastigmine, itopride and donepezil;
(xxviii) Tachykinin (NK) antagonists, particularly NK-3, NK-2 and NK-1 antagonists e.g. nepadutant, saredutant, talnetant,
(αR,9R)-7-[3,5-bis(trifluoromethyl)benzyl]-8,9,10,11-tetrahydro-9-methyl-5-(4-methylphenyl)-7H-[1,4]d iazocino[2,1-g][1,7]naphthridine-6-13-dione (TAK-637), 5-[[(2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy-3-(4-fluorophenyl)-4-morpholinyl]methyl]-1,2-dihydro-3H-1,2,4-triazol-3-one (MK-869), lanepitant, dapitant and 3-[2-methoxy-5-(trifluoromethoxy)phenyl]methylamino]-2-phenyl-piperidine (2S,3S).
Method for Assessing Biological Activities:
[0245] The 5-HT 4 receptor binding affinities of the compounds of this invention are determined by the following procedures.
Human 5-HT 4 Binding (1)
[0246] Human 5-HT 4(d) transfected HEK293 cells were prepared and grown in-house. The collected cells were suspended in 50 mM HEPES (pH 7.4 at 4° C.) supplemented with protease inhibitor cocktail (Boehringer, 1:1000 dilution) and homogenized using a hand held Polytron PT 1200 disruptor set at full power for 30 sec on ice. The homogenates were centrifuged at 40,000×g at 4° C. for 30 min. The pellets were then resuspended in 50 mM HEPES (pH 7.4 at 4° C.) and centrifuged once more in the same manner. The final pellets were resuspended in an appropriate volume of 50 mM HEPES (pH 7.4 at 25° C.), homogenized, aliquoted and stored at −80° C. until use. An aliquot of membrane fractions was used for protein concentration determination using BCA protein assay kit (PIERCE) and ARVOsx plate reader (Wallac).
[0247] For the binding experiments, 25 μl of test compounds were incubated with 25 μl of [ 3 H]-GR113808 (Amersham, final 0.2 nM) and 150 μl of membrane homogenate and WGA-SPA beads (Amersham) suspension solutions (10 μg protein and 1 mg SPA beads/well) for 60 minutes at room temperature. Nonspecific binding was determined by 1 μM GR113808 (Tocris) at the final concentration. Incubation was terminated by centrifugation at 1000 rpm.
[0248] Receptor-bound radioactivity was quantified by counting with MicroBeta plate counter (Wallac).
[0249] All compounds of Examples showed 5HT 4 receptor affinity.
Human 5-HT 4 Binding (2)
[0250] Human 5-HT 4(d) transfected HEK293 cells were prepared and grown in-house. The collected cells were suspended in 50 mM Tris buffer (pH 7.4 at 4° C.) supplemented with protease inhibitor cocktail (Boehringer, 1:1000 dilution) and homogenized using a hand held Polytron PT 1200 disruptor set at full power for 30 sec on ice. The homogenates were centrifuged at 40,000×g at 4° C. for 10 min. The pellets were then resuspended in 50 mM Tris buffer (pH 7.4 at 4° C.) and centrifuged once more in the same manner. The final pellets were resuspended in an appropriate volume of 50 mM Tris buffer (pH 7.4 at 25° C.) containing 10 mM MgCl 2 , homogenized, aliquoted and stored at −80° C. until use. An aliquot of membrane fractions was used for protein concentration determination using BCA protein assay kit (PIERCE) and ARVOsx plate reader (Wallac).
[0000] For the binding experiments, 50 μl of test compounds were incubated with 50 μl of [ 3 H]5-HT (Amersham, final 8.0 nM) and 400 μl of membrane homogenate (300 μg protein/tube) for 60 minutes at room temperature. Nonspecific binding was determined by 50 μM GR113808 (Tocris) at the final concentration. All incubations were terminated by rapid vacuum filtration over 0.2% PEI soaked glass fiber filter papers using BRANDEL harvester followed by three washes with 50 mM Tris buffer (pH 7.4 at 25° C.). Receptor-bound radioactivity was quantified by liquid scintillation counting using Packard LS counter.
[0251] All compounds of Examples showed 5HT 4 receptor affinity.
[0000] Aqonist-Induced cAMP Elevation in Human 5-HT 4(d) Transfected HEK293 Cells
[0252] Human 5-HT 4(d) transfected HEK293 cells were established in-house. The cells were grown at 37° C. and 5% CO 2 in DMEM supplemented with 10% FCS, 20 mM HEPES (pH 7.4), 200 μg/ml hygromycin B (Gibco), 100 units/ml penicillin and 100 μg/ml streptomycin.
[0000] The cells were grown to 60-80% confluence. On the previous day before treatment with compounds dialyzed FCS (Gibco) was substituted for normal and the cells were incubated overnight. Compounds were prepared in 96-well plates (12.5 μl/well). The cells were harvested with PBS/1 mM EDTA, centrifuged and washed with PBS. At the beginning of the assay, cell pellet was resuspended in DMEM supplemented with 20 mM HEPES, 10 μM pargyline (Sigma) and 1 mM 3-isobutyl-1-methylxanthine (Sigma) at the concentration of 1.6×10 5 cells/ml and left for 15 minutes at room temperature. The reaction was initiated by addition of the cells into plates (12.5 μl/well). After incubation for 15 minutes at room temperature, 1% Triton X-100 was added to stop the reaction (25 μl/well) and the plates were left for 30 minutes at room temperature. Homogenous time-resolved fluorescence-based cAMP (Schering) detection was made according to the manufacturer's instruction. ARVOsx multilabel counter (Wallac) was used to measure HTRF (excitation 320 nm, emission 665 nm/620 nm, delay time 50 μs, window time 400 μs). Data was analyzed based on the ratio of fluorescence intensity of each well at 620 nm and 665 nm followed by cAMP quantification using cAMP standard curve. Enhancement of cAMP production elicited by each compound was normalized to the amount of cAMP produced by 1000 nM serotonin (Sigma).
[0253] All compounds of Examples showed 5HT 4 receptor agonistic activity.
TMM Functional Assay
[0254] The presence of 5-HT 4 receptors in the rat esophagus and the ability to demonstrate partial agonism in the TMM preparation are reported in the literature (See G. S. Baxter et al. Naunyn-Schmiedeberg's Arch Pharmacol (1991) 343: 439-446; M. Yukiko et al. JPET (1997) 283: 1000-1008; and J. J. Reeves et al. Br. J. Pharmacol. (1991) 103: 1067-1072). More specifically, partial agonist activity can be measured according to the following procedures.
[0255] Male SD rats (Charles River) weighing 250-350 g were stunned and then killed by cervical dislocation. The esophagus was dissected from immediately proximal to the stomach (including piece of stomach to mark distal end) up to the level of the trachea and then placed in fresh Krebs' solution.
[0256] The outer skeletal muscle layer was removed in one go by peeling it away from the underlying smooth muscle layer using forceps (stomach to tracheal direction). The remaining inner tube of smooth muscle was known as the TMM. This was trimmed to 2 cm from the original ‘stomach-end’ and the rest discarded.
[0257] The TMMs were mounted as whole ‘open’ tubes in longitudinal orientation in 5 ml organ baths filled with warm (32° C.) aerated Krebs. Tissues were placed under an initial tension of 750 mg and allowed to equilibrate for 60 minutes. The tissues were re-tensioned twice at 15 minute intervals during the equilibration period. The pump flow rate was set to 2 ml/min during this time.
[0258] Following equilibration, the pump was switched off. The tissues were exposed to 1 μM carbachol and contracted and reached a steady contractile plateau within 15 minutes. Tissues were then subject to 1 μM 5-HT (this was to prime the tissues). The tissues relaxed in response to 5-HT fairly rapidly—within 1 minute. As soon as maximal relaxation has occurred and a measurement taken, the tissues were washed at maximum rate (66 ml/min) for at least 1 minute and until the original baseline (pre-carbachol and 5-HT) has returned (usually, the baseline drops below the original one following initial equilibration). The pump flow rate was reduced to 2 ml/min and the tissues left for 60 minutes.
[0259] A cumulative concentration-effect-curve (CEC) to 5-HT was constructed across the range 0.1 nM to 1 μM, in half-log unit increments (5-HT curve 1 for data analysis). Contact time between doses was 3 minutes or until plateau established. Tissues responded quicker as concentration of 5-HT in the bath increases. At the end of the curve, the tissues were washed (at maximum rate) as soon as possible to avoid desensitization of receptors. Pump rate was reduced to 2 ml/min and the tissues left for 60 minutes.
[0260] A second CEC was carried out—either to 5-HT (for time control tissues), another 5-HT 4 agonist (standard) or a test compound (curve 2 for data analysis). Contact time varied for other 5-HT 4 agonists and test compounds and was tailored according to the tissues' individual responses to each particular agent. In tissues exposed to a test compound, a high concentration (1 μM) of a 5-HT 4 antagonist (SB 203,186: 1H-Indole-3-carboxylic acid, 2-(1-piperidinyl)ethyl ester, Tocris) was added to the bath following the last concentration of test compound. This was to see if any agonist-induced relaxation (if present) could be reversed. SB 203,186 reversed 5-HT induced relaxation, restoring the tissue's original degree of carbachol-induced tone.
[0261] Agonist activity of test compounds was confirmed by pre-incubating tissues with 100 nM standard 5HT 4 antagonist such as SB 203,186. SB 203,186 was added to the bath 5 minutes before the addition of carbachol prior to curve 2. Tissues must be ‘paired’ for data analysis i.e. the test compound in the absence of SB 203,186 in one tissue was compared with the test compound in the presence of SB 203,186 in a separate tissue. It was not possible to carry out a curve 3 i.e. 5-HT curve 1, followed by the test compound curve 2 (−SB 203,186), followed by the test compound curve 3 (+SB 203,186).
[0262] All compounds of Examples showed 5HT 4 receptor agonistic activity.
Human Dofetilide Binding
[0263] Human HERG transfected HEK293S cells were prepared and grown in-house. The collected cells were suspended in 50 mM Tris-HCl (pH 7.4 at 4° C.) and homogenized using a hand held Polytron PT 1200 disruptor set at full power for 20 sec on ice. The homogenates were centrifuged at 48,000×g at 4° C. for 20 min. The pellets were then resuspended, homogenized, and centrifuged once more in the same manner. The final pellets were resuspended in an appropriate volume of 50 mM Tris-HCl, 10 mM KCl, 1 mM MgCl 2 (pH 7.4 at 4° C.), homogenized, aliquoted and stored at −80° C. until use. An aliquot of membrane fractions was used for protein concentration determination using BCA protein assay kit (PIERCE) and ARVOsx plate reader (Wallac).
[0264] Binding assays were conducted in a total volume of 200 μl in 96-well plates. Twenty μl of test compounds were incubated with 20 μl of [ 3 H]-dofetilide (Amersham, final 5 nM) and 160 μl of membrane homogenate (25 μg protein) for 60 minutes at room temperature. Nonspecific binding was determined by 10 μM dofetilide at the final concentration. Incubation was terminated by rapid vacuum filtration over 0.5% presoaked GF/B Betaplate filter using Skatron cell harvester with 50 mM Tris-HCl, 10 mM KCl, 1 mM MgCl 2 , pH 7.4 at 4° C. The filters were dried, put into sample bags and filled with Betaplate Scint. Radioactivity bound to filter was counted with Wallac Betaplate counter.
Caco-2 Permeability
[0265] Caco-2 permeability was measured according to the method described in Shiyin Yee, Pharmaceutical Research, 763 (1997).
[0266] Caco-2 cells were grown on filter supports (Falcon HTS multiwell insert system) for 14 days. Culture medium was removed from both the apical and basolateral compartments and the monolayers were preincubated with pre-warmed 0.3 ml apical buffer and 1.0 ml basolateral buffer for 0.5 hour at 37° C. in a shaker water bath at 50 cycles/min. The apical buffer consisted of Hanks Balanced Salt Solution, 25 mM D-glucose monohydrate, 20 mM MES Biological Buffer, 1.25 mM CaCl 2 and 0.5 mM MgCl 2 (pH 6.5). The basolateral buffer consisted of Hanks Balanced Salt Solution, 25 mM D-glucose monohydrate, 20 mM HEPES Biological Buffer, 1.25 mM CaCl 2 and 0.5 mM MgCl 2 (pH 7.4). At the end of the preincubation, the media was removed and test compound solution (10 μM) in buffer was added to the apical compartment. The inserts were moved to wells containing fresh basolateral buffer at 1 hr. Drug concentration in the buffer was measured by LC/MS analysis.
[0267] Flux rate (F, mass/time) was calculated from the slope of cumulative appearance of substrate on the receiver side and apparent permeability coefficient (P app ) was calculated from the following equation.
[0000] P app ( cm/sec )=( F*VD )/( SA*MD )
[0268] where SA is surface area for transport (0.3 cm 2 ), VD is the donor volume (0.3 ml), MD is the total amount of drug on the donor side at t=0. All data represent the mean of 2 inserts. Monolayer integrity was determined by Lucifer Yellow transport.
Half-Life in Human Liver Microsomes (HLM)
[0269] Test compounds (1 μM) were incubated with 3.3 mM MgCl 2 and 0.78 mg/mL HLM (HL101) in 100 mM potassium phosphate buffer (pH 7.4) at 37° C. on the 96-deep well plate. The reaction mixture was split into two groups, a non-P450 and a P450 group. NADPH was only added to the reaction mixture of the P450 group. An aliquot of samples of P450 group was collected at 0, 10, 30, and 60 min time point, where 0 min time point indicated the time when NADPH was added into the reaction mixture of P450 group. An aliquot of samples of non-P450 group was collected at −10 and 65 min time point. Collected aliquots were extracted with acetonitrile solution containing an internal standard. The precipitated protein was spun down in centrifuge (2000 rpm, 15 min). The compound concentration in supernatant was measured by LC/MS/MS system.
[0270] The half-life value was obtained by plotting the natural logarithm of the peak area ratio of compounds/internal standard versus time. The slope of the line of best fit through the points yields the rate of metabolism (k). This was converted to a half-life value using following equations:
[0000] Half-life= In 2 /k
EXAMPLES
[0271] The invention is illustrated in the following non-limiting examples in which, unless stated otherwise: all operations were carried out at room or ambient temperature, that is, in the range of 18-25° C.; evaporation of solvent was carried out using a rotary evaporator under reduced pressure with a bath temperature of up to 60° C.; reactions were monitored by thin layer chromatography (TLC) and reaction times are given for illustration only; melting points (mp) given are uncorrected (polymorphism may result in different melting points); the structure and purity of all isolated compounds were assured by at least one of the following techniques: TLC (Merck silica gel 60 F 254 precoated TLC plates or Merck NH 2 gel (an amine coated silica gel) F 254s precoated TLC plates), mass spectrometry, nuclear magnetic resonance spectra (NMR), infrared absorption spectra (IR) or microanalysis. Yields are given for illustrative purposes only. Workup with a cation-exchange column was carried out using SCX cartridge (Varian BondElute), which was preconditioned with methanol. Flash column chromatography was carried out using Merck silica gel 60 (63-200 μm), Wako silica gel 300HG (40-60 μm), Fuji Silysia NH gel (an amine coated silica gel) (30-50 μm), Biotage KP-SIL (32-63 μm) or Biotage AMINOSILICA (an amine coated silica gel) (40-75 μm). Preparative TLC was carried out using Merck silica gel 60 F 254 precoated TLC plates (0.5 or 1.0 mm thickness). Low-resolution mass spectral data (EI) were obtained on an Integrity (Waters) mass spectrometer. Low-resolution mass spectral data (ESI) were obtained on ZMD™ or ZQ™ (Waters) and mass spectrometer. NMR data were determined at 270 MHz (JEOL JNM-LA 270 spectrometer), 300 MHz (JEOL JNM-LA300 spectrometer) or 600 MHz (Bruker AVANCE 600 spectrometer) using deuterated chloroform (99.8% D) or dimethylsulfoxide (99.9% D) as solvent unless indicated otherwise, relative to tetramethylsilane (TMS) as internal standard in parts per million (ppm); conventional abbreviations used are: s=singlet, d=doublet, t=triplet, q=quartet, quint=quintet, m=multiplet, br.=broad, etc. IR spectra were measured by a Fourier transform infrared spectrophotometer (Shimazu FTIR-8300). The powder X-ray diffraction (PXRD) pattern was determined using a Rigaku RINT-TTR powder X-ray diffractometer fitted with an automatic sample changer, a 2 theta-theta goniometer, beam divergence slits, a secondary monochromator and a scintillation counter. The sample was prepared for analysis by packing the powder on to an aluminum sample holder. The specimen was rotated by 60.00 rpm and scanned by 4°/min at room temperature with Cu-ka radiation. Chemical symbols have their usual meanings; by (boiling point), mp (melting point), L (liter(s)), mL (milliliter(s)), g (gram(s)), mg (milligram(s)), mol (moles), mmol (millimoles), eq. (equivalent(s)), quant. (quantitative yield).
Example 1
4-{[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)-YL)CARBONYL]AMINO}METHYL)PIPERI DIN-1-YL]METHYL}TETRAHYDRO-2H-PYRAN-4-CARBOXYLIC ACID
[0272]
Step 1. tert-Butyl 4-cyanotetrahydro-2H-pyran-4-carboxylate
[0273] To a stirred suspension of NaH (17.7 g, 0.443 mol) in N,N-dimethylformamide (200 mL) was added dropwise a solution of tert-butyl cyanoacetate (25.0 g, 0.177 mol) in N,N-dimethylformamide (100 mL) at 0° C. under N 2 . The mixture was allowed to warm up to ambient temperature, and stirred for 1 h. Then, bis(2-bromoethyl)ether (49.3 g, 0.177 mol) was added to the mixture, and the resulting mixture was stirred at 90° C. for 24 h. After cooling to 0° C., the mixture was washed with water (100 mL). The volatile components were removed by evaporation and the residue was precipitated with a mixture of ethyl acetate-toluene (1:2, 500 mL) and water (500 mL). The organic phase was washed with water (500 mL) three times, dried over Na 2 SO 4 , filtered and evaporated. The solid was washed with hexane, collected by filtration and dried in vacuo to give 19.0 g (57%) of the title compound as white crystal.
[0274] 1 H-NMR (CDCl 3 ) δ: 3.96 (2H, dt, J=3.9 Hz, 12.3 Hz), 3.73 (2H, dt, J=2.6 Hz, 12.3 Hz), 2.20-1.94 (4H, m), 1.52 (9H, s).
Step 2. tert-Butyl 4-(aminomethyOtetrahydro-2H-pyran-4-carboxylate
[0275] A mixture of tert-butyl 4-cyanotetrahydro-2H-pyran-4-carboxylate (18.95 g, 0.0897 mol, step1 of Example 1) and Raney Ni (1.00 g) in methanol (200 mL) was hydrogenated (3 atm) at room temperature for 12 h. Then, the mixture was filtered through a pad of Celite, and the filtrate was concentrated in vacuo to give 16.01 g (83%) of the title compound as yellow syrup.
[0276] 1 H-NMR (CDCl 3 ) δ: 3.86 (2H, dt, J=4.1 Hz, 11.4 Hz), 3.48 (2H, dt, J=2.5 Hz, 11.5 Hz), 2.75 (2H, s), 2.03 (2H, br d, J=10.7 Hz), 1.55-1.35 (13H, m, including 9H, s, 1.49 ppm).
Step 3. tert-Butyl 4-(4-oxopiperidin-1-vnmethylltetrahydro-2H-pyran-4-carboxylate
[0277] To a refluxing mixture of tert-butyl 4-(aminomethyl)tetrahydro-2H-pyran-4-carboxylate (8.00 g, 0.0372 mol, step2 of Example 1) and K 2 CO 3 (0.51 g, 0.0372 mol) in ethanol-H 2 O (2:1, 240 mL) was added dropwise 1-ethyl-1-methyl-4-oxopiperidinium iodide (12.0 g, 0.0445 mol, J. Org. Chem. 1995, 60, 4324) in ethanol-H 2 O (2:1, 150 mL), and the resulting mixture was stirred at the same temperature for 1 h. After cooling to room temperature, the solvent was removed in vacuo. The residue was poured into sat. NaHCO 3 aq. (200 mL), and the mixture was extracted with CH 2 Cl 2 (200 mL×3). The extracts were dried over Na 2 SO 4 , filtered and concentrated. The residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (3:1 to 2:1) to give 10.77 g (98%) of the title compound as colorless syrup.
[0278] MS (ESI) m/z: 298 (M+H) + .
[0279] 1 H NMR (CDCl 3 ) δ 3.84 (2H, br d, J=11.4 Hz), 3.50 (2H, dt, J=2.0 Hz, 11.7 Hz), 2.85 (4H, t, J=5.9 Hz), 2.61 (2H, s), 2.39 (4H, t, J=6.1 Hz), 2.05 (2H, d, J=11.5 Hz), 1.75-1.45 (11H, m, including 9H, s, 1.49 ppm).
Step 4. tert-Butyl 4-[{4-cyanopiperidin-1-yl)methylltetrahydro-2H-pyran-4-carboxylate
[0280] To a stirred solution of tert-butyl4-[(4-oxopiperidin-1-yl)methyl]tetrahydro-2H-pyran-4-carboxylate (8.77 g, 0.0295 mol, step 3 of Example 3) in 1,2-dimethoxyethane (250 mL) was added p-toluenesulfonylmethylisocyanide (11.51 g, 0.0590 mol), ethanol (3.96 mL, 0.0678 mol) and potassium t-butoxide (11.58 g, 0.1032 mol) at 0° C. The resulting mixture was stirred at 50° C. for 16 h. After cooling, the reaction mixture was poured into sat. NaHCO 3 aq. (200 mL), and the mixture was extracted with CH 2 Cl 2 (200 mL×3). The extracts were dried over Na 2 SO 4 , filtered and concentrated. The residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (2:1) to give 5.76 g (63%) of the title compound as yellow syrup.
[0281] MS (ESI) m/z: 309 (M+H) + .
[0282] 1 H-NMR (CDCl 3 ) δ: 3.81 (2H, dt, J=3.1 Hz, 11.0 Hz), 3.48 (2H, dt, J=2.1 Hz, 11.7 Hz), 2.76-2.64 (2H, m), 2.64-2.52 (1H, m), 2.50-2.35 (4H, m, including 2H, s, 2.46 ppm), 1.98 (2H, br d, J=11.9 Hz), 1.92-1.70 (4H, m), 1.65-1.40 (11H, m, including 9H, s, 1.47 ppm).
Step 5. tert-Butyl4-{[4-(aminomethyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylate
[0283] A mixture of tert-butyl 4-[(4-cyanopiperidin-1-yl)methyl]tetra hydro-2H-pyran-4-carboxylate (5.76 g, 0.0187 mol, step 4 of Example 1) and Raney Ni (3.00 g) in methanol (100 mL) was hydrogenated (3 atm) at room temperature for 12 h. Then, the mixture was filtered through a pad of Celite, and the filtrate was concentrated in vacuo to give 5.72 g (98%) of the title compound as yellow syrup.
[0284] MS (ESI) m/z: 313 (M+H) + .
[0285] 1 H-NMR (CDCl 3 ) δ: 3.80 (2H, dt, J=3.1 Hz, 11.5 Hz), 3.49 (2H, dt, J=2.1 Hz, 12.2 Hz), 2.80 (2H, br d, J=11.5 Hz), 2.58-2.40 (4H, m, including 2H, s, 2.43 ppm), 2.15 (2H, br t, J=7.3 Hz), 1.98 (2H, br d, J=13.7 Hz), 1.70-1.40 (16H, m, including 9H, s, 1.47 ppm), 1.30-1.10 (2H, m).
Step 6. tert-Butyl 4-{[4-(W2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylate
[0286] To a stirred solution of spiro[cyclopentane-1,3′-indol]-2′(1′H)-one (600 mg, 3.2 mmol, Howard, Harry R. et al., J. Med. Chem., 1996, 39, 143) and triethylamine (972 mg, 9.6 mmol) in CH 2 Cl 2 (20 mL) was added 4-nitrochloroformate (677 mg, 3.4 mmol) at room temperature, and stirred at ambient temperature for 3 h. Then, a solution of tert-butyl 4-{[4-(aminomethyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylate (1.0 g, 3.2 mmol, step 5 of Example 1) in CH 2 Cl 2 (5 mL) was added at room temperature, and stirred for 18 h. Then, sat. NaHCO 3 aq. (20 mL) was added, extracted with CH 2 Cl 2 (30 mL×3), dried over MgSO 4 , filtered and concentrated gave yellow brown oil. The residue was chromatographed on a column of aminopropyl-silica gel eluting with hexane/ethyl acetate (11:1) to give 1.3 g (75%) of the title compound as clear yellow oil.
[0287] MS (ESI) m/z: 526 (M+H) + .
[0288] 1 H-NMR (CDCl 3 ) δ: 8.70 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.41-7.10 (3H, m), 3.83-3.75 (2H, m), 3.52-3.47 (2H, m), 3.29-3.20 (2H, m), 2.83-2.75 (2H, m), 2.44 (2H, s), 2.25-1.20 (28H, m).
Step 7. 4-{[4-({[(2′-Oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]meth yl}tetrahydro-2H-pyran-4-carboxylic acid
[0289] To a solution of tert-butyl 4-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylate (2.3 g, 4.38 mmol, step 6 of Example 1) in CH 2 Cl 2 (14 mL), trifluoroacetic acid (18 mL) was added at room temperature, and the mixture was stirred overnight at room temperature. The mixture was concentrated to give yellow oil, CH 2 Cl 2 (200 mL) was added and washed with sat. NaHCO 3 aq. (80 mL), dried over MgSO 4 , filtered and concentrated gave a syrup, which was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol (15:1) to give 2.1 g (quant.) of the title compound as white solid. Recrystallization from ethyl acetate/n-heptane gave white powder.
[0290] MS (ESI) m/z: 470 (M+H) + .
[0291] m.p.: 146.3° C.
[0292] IR (KBr) ν: 2943, 2864, 1733, 1558, 1465, 1352, 1151, 1109, 759 cm −1
[0293] 1 H-NMR (CDCl 3 ) δ: 8.85 (1H, br s), 8.21 (1H, d, J=8.1 Hz), 7.30-7.15 (3H, m), 3.95-3.72 (4H, m), 3.40-3.25 (2H, m), 3.20-3.06 (2H, m), 2.65-2.45 (4H, m), 2.25-1.85 (13H, m), 1.60-1.40 (4H, m).
[0294] Signal due to CO 2 H was not observed.
[0295] Anal. Calcd. for C 26 H 35 N 3 O 5 .0.25H 2 O: C, 65.87; H, 7.55; N, 8.86. Found: C, 65.58; H, 7.39; N, 8.86.
Example 2
2,2-DIMETHYL-3-[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL[-1′(2′H)—YL)CARBONYL]AMINO}M ETHYL)PIPERIDIN-1-YL]PROPANOIC ACID
[0296]
Step 1. tert-Butyl 4-({{[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidine-1-carboxylate
[0297] The title compound was prepared according to the procedure described in step 6 of Example 1 from tert-butyl 4-(aminomethyl)piperidine-1-carboxylate.
[0298] Rf=0.2 (hexane/ethyl acetate (8/1))
[0299] 1 H-NMR (CDCl 3 ) δ: 8.78 (1H, br s), 8.23 (1H, d, J=9 Hz), 7.31-7.10 (3H, m), 4.20-4.05 (2H, m), 3.35-3.25 (2H, m), 2.80-2.60 (2H, m), 2.25-1.80 (9H, m), 1.80-1.65 (2H, m), 1.46 (9H, s), 1.30-1.10 (2H, m).
Step 2. 2′-Oxo-N-(piperidin-4-ylmethyl)spiro[cyclopentane-1,3′-indole]-1′(2′H)-carboxamide
[0300] tert-Butyl 4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidine-1-carboxylate (750 mg, 1.8 mmol, step 1 of Example 2) was dissolved in 10% HCl in methanol (20 mL) and the mixture was stirred for 7 h at room temperature. Concentrated gave a colorless oil, which was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol/NH 4 OH (12/1/0.1) to give 570 mg (quant.) of the title compound as colorless oil.
[0301] MS (ESI) m/z: 328 (M+H) + .
[0302] 1 H-NMR (CDCl 3 ) δ: 8.76 (1H, br s), 8.24 (1H, d, J=9.0 Hz), 7.31-7.10 (3H, m), 3.32-3.25 (2H, m), 3.15-3.09 (2H, m), 2.67-2.60 (2H, m), 2.30-1.60 (12H, m), 1.32-1.10 (2H, m).
Step 3. Methyl 2,2-dimethyl-3-[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoate
[0303] To a stirred solution of 2′-oxo-N-(piperidin-4-ylmethyl)spiro[cyclopentane-1,3′-indole]-1′(2′H)-carboxamide (480 mg, 1.5 mmol, step 2 of Example 2) and methyl 2,2-dimethyl-3-oxopropanoate (248 mg, 1.7 mmol, Kim, Hwa-Ok et al., Synth. Commun., 1997, 27, 2505) in CH 2 Cl 2 (40 mL) was added sodium triacetoxyborohydride (623 mg, 2.9 mmol) in one portion at room temperature. The mixture was stirred for 20 h at ambient temperature. To the mixture was added sat. NaHCO 3 aq. (10 mL), extracted with CH 2 Cl 2 (30 mL×2), dried over MgSO 4 , filtered and concentrated gave yellow oil. The residue was chromatographed on a column of aminopropyl-silica gel eluting with hexane/ethyl acetate (9:1) to give 150 mg (23%) of the title compound as clear colorless oil.
[0304] MS (ESI) m/z: 442 (M+H) + .
[0305] 1 H-NMR (CDCl 3 ) δ: 8.72 (1H, br s), 8.24 (1H, d, J=8.1 Hz), 7.31-7.10 (3H, m), 3.65 (3H, s), 3.27-3.20 (2 H, m), 2.85-2.75 (2H, m), 2.46 (2H, s), 2.23-1.90 (11H, m), 1.70-1.60 (2H, m), 1.35-1.28 (2H, m), 1.15 (6H, s).
Step 4. 2,2-Dimethyl-3-[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)-carbonyl]amino}methyl)piperidin-1-yl]propanoic acid
[0306] To a stirred solution of methyl 2,2-dimethyl-3-[4-({[(2′-oxospiro [cyclopentane-1,3′-indol]-[(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoate (170 mg, 0.38 mmol, step 3 of Example 2) in acetic acid (2 mL), H 2 SO 4 (113 mg) in water (2 mL) was added, and the mixture was refluxed for 36 h. The mixture was cooled to room temperature and solid NaHCO 3 (500 mg) was added slowly. The resulting mixture was concentrated to give white solid. To the solid, CH 2 Cl 2 (40 mL) was added and stirred for 10 min, dried over MgSO 4 . The solution was filtered and concentrated and then resulted yellow oil. The oil was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol (14:1) to give 130 mg (80%) of the title compound as white solid. Recrystallization from ethyl acetate/diethyl ether gave white powder.
[0307] MS (ESI) m/z: 427 (M+H) + .
[0308] m.p.: 189.1° C.
[0309] IR (KBr) ν: 2950, 1732, 1600, 1537, 1475, 1348, 1321, 1280, 1153, 964, 873, 758 cm −1
[0310] 1 H-NMR (CDCl 3 ) δ: 8.80 (1H, br s), 8.21 (1H, d, J=8.1 Hz), 7.35-7.10 (3H, m), 3.36-3.20 (2H, m), 3.20-3.10 (2H, m), 2.56 (2H, s), 2.54-2.40 (2H, m), 2.30-1.60 (11H, m), 1.58-1.35 (2H, m), 1.24 (6H, s). A signal due to CO 2 H was not observed
[0311] Anal. Calcd. for C 24 H 33 N 3 O 4 .0.3H 2 O: C, 66.58; H, 7.82; N, 9.71. Found: C, 66.33; H, 7.72; N, 9.51.
Example 3
1-{[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)—YL)CARBONYL]AMINO}METHYL)PIPERI DIN-1-YL]METHYL}CYCLOPROPANECARBOXYLIC ACID
[0312]
Step 1. tert-Butyl 1-(iodomethyl)cyclopropanecarboxylate
[0313] To a stirred solution of diisopropylamine (7.7 mL, 0.055 mol) in tetrahydrofuran (80 mL), n-butyl lithium (1.59 M in cyclohexane, 34 mL, 0.055 mol) was added slowly at −70° C. and the mixture was stirred for 20 min at 0° C. The mixture was cooled to −78° C. and tert-butyl cyclopropanecarboxylate (6.5 g, 0.046 mol, Kohlrausch et al., Z. Elektrochem. Angew. Phys. Chem., 1937, 70, 392) in tetrahydrofuran (10 mL) was added dropwise, and the mixture was stirred for 3 h. Then, diiodomethane (4.0 mL, 0.050 mol) in tetrahydrofuran (10 mL) was added dropwise, and the mixture was allowed to warm up to room temperature overnight. Saturated aqueous NH 4 Cl (80 mL) was added to the solution and it was extracted with diethyl ether (50 mL), washed with brine (20 mL), dried over MgSO 4 , filtered and concentrated to give brown oil. The oil was chromatographed on a column of silica gel eluting with hexane/diethyl ether (40:1) to give 1.9 g of the title compound as a crude product. The crude product was used without further purification. Rf: 0.3 (hexane/diethyl ether (40:1))
Step 2. tert-Butyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclopropanecarboxylate
[0314] A mixture of tent-butyl 1-(iodomethyl)cyclopropanecarboxylate (1.9 g 6.7 mmol, step 1 of Example 3), tert-butyl(piperidin-4-ylmethyl)carbamate (3.0 g, 14 mmol), N,N-diisopropylethylamine (5.8 mL, 34 mmol) in N,N-dimethylformamide (25 mL) was heated at 120° C. for 20 h. After cooled to room temperature, water (50 mL) was added, extracted with ethyl acetate/toluene (1:2, 60 mL×2), washed with water (50 mL×2), brine (50 mL), dried over MgSO 4 , filtered and concentrated to give brown oil. The oil was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol (10:1) to give 560 mg (11%) of the title compound as clear brown oil. MS (ESI) m/z: 369 (M+H) + . 1 H-NMR (CDCl 3 ) δ: 4.60 (1H, br), 3.08-2.82 (4H, m), 2.59 (2H, s), 2.10-1.90 (2H, m), 1.75-1.55 (4H, m), 1.50-1.05 (23H, m).
Step 3. 1-{[4-(Aminomethyl)piperidin-1-yl]methyl}cyclopropanecarboxylic acid
[0315] tert-Butyl 1-[(4-{](tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclopropanecarboxylate (211 mg, 0.57 mmol, step 2 of Example 3) was dissolved in 10% HCl in dioxane (5 mL) and the mixture was stirred for 4 h at room temperature. Resultant brown suspension was concentrated to give 150 mg (quant.) of the title compound as a pale brown solid. This was used without further purification.
[0316] MS (ESI) m/z: 211 (M−H) − .
Step 4. 1-{[4-({[(2′-Oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclopropanecarboxylic acid
[0317] The title compound was prepared according to the procedure described in step 6 of Example 1 from 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclopropanecarboxylic acid (step 3 of Example 3). Purification was performed by silica gel column eluting with CH 2 Cl 2 /methanol (18:1˜10:1) to give 130 mg (53%) of the title compound as white solid. The solid was triturated with hexane/diethyl ether, and collected by filtration to give the title compound as white solid.
[0318] MS (ESI) m/z: 426 (M+H) + . m.p.: 186.5° C.
[0319] IR (KBr) ν: 3300, 2960, 2908, 1743, 1697, 1542, 1463, 1348, 1267, 1161, 1143, 1105, 779 cm−1
[0320] 1 H-NMR (CDCl 3 ) δ: 8.81 (1H, br s), 8.21 (1H, d, J=8.1 Hz), 7.32-7.14 (3H, m), 3.43-3.15 (4H, m), 2.59 (2 H, s), 2.30-1.60 (17H, m), 0.65-0.56 (2H, m). A signal due to CO 2 H was not observed. Anal. Calcd. for C 24 H 31 N 3 O 4 : C, 67.74; H, 7.34; N, 9.88. Found: C, 67.45; H, 7.36; N, 9.80.
Example 4
1-{[4-({[(2′-OXOSPIROICYCLOPENTANE-1,3′-INDOL]-1′(2′H)-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOPENTANECARBOXYLIC ACID
[0321]
Step 1. Methyl 1-(iodomethyl)cyclopentanecarboxylate
[0322] The title compound was prepared according to the procedure described in step 1 of Example 3 from methyl cyclopentanecarboxylate.
[0323] 1 H-NMR (CDCl 3 ) δ 3.73 (3H, s), 3.42 (2H, s), 2.30-2.15 (2H, m), 1.80-1.55 (6H, m).
Step 2. Methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidine-1-yl)methyl]cyclopentanecarboxylate
[0324] The title compound was prepared according to the procedure described in step 2 of Example 3 from methyl 1-(iodomethyl)cyclopentanecarboxylate.
[0325] MS (ESI) m/z: 355(M+H) + .
[0326] 1 H-NMR (CDCl 3 ) δ 4.58 (1H, br s), 3.66 (3H, s), 2.97 (2H, t, J=6.3 Hz), 2.77 (2H, br d, J=11.5 Hz), 2.55 (2H, s), 1.70-1.50 (9H, m), 1.44 (9H, s), 1.25-1.08 (2H, m).
Step 3. Methyl 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclopentanecarboxylate
[0327] A solution of methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidine-1-yl)methyl]cyclopentanecarboxylate (1.16 g, 3.27 mmol, step 2 of Example 4) in CH 2 Cl 2 (25 mL) and trifluoroacetic acid (5 mL) was stirred at room temperature for 1.5 h. The reaction mixture was then concentrated, basified with sat. NaHCO 3 aq. (100 mL) and extracted with CHCl 3 (100 mL) five times. The combined extracts were dried over MgSO 4 , filtered and concentrated to give 0.831 g (100%) of title compound as yellow syrup.
[0328] MS (ESI) m/z: 255 (M+H) + .
[0329] 1 H-NMR (CDCl 3 ) δ 3.66 (3H, s), 2.78 (2H, d, J=11.5 Hz), 2.62-2.50 (4H, m), 2.15-1.98 (4H, m), 1.80-1.40 (9H, m), 1.30-1.05 (2H, m).
Step 4. Methyl 1-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclopentanecarboxylate
[0330] The title compound was prepared according to the procedure described in step 6 of Example 1 from methyl 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclopentane carboxylate (step 3 of Example 4).
[0331] MS (ESI) m/z: 468 (M+H) + .
[0332] 1 H-NMR (CDCl 3 ) δ: 8.71 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.34-7.10 (3H, m), 3.66 (3H, s), 3.28-3.20 (2 H, m), 2.82-2.75 (2H, m), 2.56 (2H, s), 2.25-1.40 (21H, m), 1.38-1.12 (2H, m).
Step 5. 1-{[4-({[(2′-Oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclopentanecarboxylic acid
[0333] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 1-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl) carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclopentanecarboxylate (step 4 of Example 4).
[0334] MS (ESI) m/z: 454 (M+H) + .
[0335] m.p.: 188.1° C.
[0336] IR (KBr) ν: 3301, 2935, 2869, 1730, 1602, 1531, 1469, 1278, 1147, 758 cm −1
[0337] 1 H-NMR (CDCl 3 ) δ: 8.80 (1H, br s), 8.21 (1H, d, J=8.1 Hz), 7.32-7.14 (3H, m), 3.31 (2H, t, J=5.4 Hz), 3.23-3.12 (2H, m), 2.67 (2H, s), 2.50-2.32 (2H, m), 2.31-1.56 (17H, m), 1.55-1.32 (4H, m). A signal due to CO 2 H was not observed.
[0338] Anal. Calcd. for C 26 H 35 N 3 O 4 .0.5H 2 O: C, 67.51; H, 7.84; N, 9.08. Found: C, 67.17; H, 7.83; N, 8.85.
Example 5
1-{[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)—YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID
[0339]
Step 1. Methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutanecarboxylate
[0340] To a stirred mixture of tert-butyl(piperidin-4-ylmethyl)carbamate (12.8 g, 60 mmol) and methyl 1-formylcyclobutanecarboxylate (2.13 g, 15 mmol, Davis, Charles R.; Swenson, Dale C.; Burton, Donald J., J. Org. Chem., 1993, 58, 6843) in tetrahydrofuran (50 mL) was added acetic acid (8.6 mL, 150 mmol) at ambient temperature. After 30 min, sodium triacetoxyborohydride (12.7 g, 60 mmol) was added to the mixture. Then, the mixture was heated to 60° C. for 2 h. After cooling, the reaction miture was poured into sat. NaHCO 3 aq. The aqueous layer was extracted with CH 2 Cl 2 for 3 times. The combined organic phase were washed with brine, dried over MgSO 4 , filtered and concentrated. The residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (1:1) to give 4.25 g (83%) of the title compound as white solid.
[0341] MS (ESI) m/z: 341 (M+H) + .
[0342] 1 H-NMR (CDCl 3 ) δ: 3.69 (3H, s), 2.96 (2H, t, J=6.2 Hz), 2.75 (2H, d, J=11.4 Hz), 2.67 (2H, s), 2.37-2.46 (2H, m), 1.78-2.05 (6H, m), 1.45-1.65 (2H, m), 1.43 (9H, s), 1.09-1.21 (2H, m),
Step 2. Methyl 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclobutanecarboxylate
[0343] The title compound was prepared according to the procedure described in step 3 of Example 4 from methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutanecarboxylate (step 1 of Example 5).
[0344] MS (ESI) m/z: 241 (M+H) + .
[0345] 1 H-NMR (CDCl 3 ) δ: 3.67 (3H, s), 2.72-2.78 (2H, m), 2.66 (2H, s), 2.54 (2H, d, J=6.2 Hz), 2.34-2.47 (2H, m), 1.79-2.04 (8H, m), 1.54-1.64 (2H, m), 1.05-1.35 (3H, m).
Step 3. Methyl 1-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylate
[0346] The title compound was prepared according to the procedure described in step 6 of Example 1 from methyl 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclobutane carboxylate (step 2 of Example 5).
[0347] MS (ESI) m/z: 454 (M+H) + .
[0348] 1 H-NMR (CDCl 3 ) δ: 8.71 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.35-7.10 (3H, m), 3.70 (3H, s), 3.27-3.21 (2H, m), 2.88-2.70 (2H, m), 2.68 (2H, s), 2.49-2.35 (2H, m), 2.28-2.15 (2H, m), 2.14-1.75 (13H, m), 1.70-1.62 (2H, m), 1.34-1.15 (2H, m).
Step 4. 1-{[4-({[(2′-Oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid
[0349] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 1-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylate (step 3 of Example 5).
[0350] MS (ESI) m/z: 440 (M+H) + .
[0351] m.p.: 171.0° C.
[0352] IR (KBr) ν: 3303, 2937, 2868, 1728, 1537, 1461, 1280, 1226, 1145, 765, 750 cm −1
[0353] 1 H-NMR (CDCl 3 ) δ: 8.80 (1H, br s), 8.20 (1H, d, J=8.0 Hz), 7.32-7.12 (3H, m), 3.30 (2H, t, J=6.1 Hz), 3.14-3.00 (2H, m), 2.77 (2H, s), 2.60-2.46 (2H, m), 2.45-1.70 (17H, m), 1.54-1.35 (2H, m). A signal due to CO 2 H was not observed.
[0354] Anal. Calcd. for C 25 H 33 N 3 O 4 .0.5H 2 O: C, 66.94; H, 7.64; N, 9.37. Found: C, 66.95; H, 7.75; N, 9.32.
Example 6
2-ETHYL-2-{[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1-′(2′H)—YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}BUTANOIC ACID
[0355]
Step 1. Methyl 2-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]-2-ethylbutanoate
[0356] The title compound was prepared with the similar method shown in the step 1 of Example 5 by using methyl 2-ethyl-2-formylbutanoate (Okano, K.; Morimoto, T.; Sekiya, M. Journal of the Chemical Society, Chemical Communications, 1985, 3, 119)
[0357] MS (ESI) m/z: 357 (M+H) + .
[0358] 1 H-NMR (CDCl 3 ) δ: 4.62-4.48 (1H, br), 3.65 (3H, s), 3.01-2.93 (2H, m), 2.73-2.65 (2H, m), 2.46 (2H, s), 2.13-2.02 (2H, m), 1.73-1.50 (6H, m), 1.44 (9H, s), 1.28-1.10 (3H, m), 0.76 (6H, t, J=7.5 Hz).
Step 2. Methyl 2-{[4-(aminomethyl)piperidin-1-yl]methyl}-2-ethylbutanoate
[0359] The title compound was prepared according to the procedure described in step 3 of Example 4 from methyl 2-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]-2-ethylbutanoate (step 1 of Example 6).
[0360] MS (ESI) m/z: 459 (M+H) + .
[0361] 1 H-NMR (CDCl 3 ) δ: 8.92-8.86 (1H, m), 8.28-8.23 (1H, m), 7.20-7.12 (3H, m), 4.77-4.61 (1H, m), 3.65 (3 H, s), 3.27 (2H, t, J=6.4 Hz), 2.75-2.66 (2H, m), 2.47 (2H, s), 2.16-2.05 (2H, m), 1.72-1.49 (10H, m), 1.38-1.21 (5H, m), 0.76 (6H, d, J=7.5 Hz).
Step 3. Methyl 2-ethyl-2-{[4-({[(2′-oxospiroicyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}butanoate
[0362] The title compound was prepared according to the procedure described in step 6 of Example 1 from methyl 2-{[4-(aminomethyl)piperidin-1-yl]methyl}-2-ethyl butanoate (step 2 of Example 6).
[0363] MS (ESI) m/z: 470 (M+H) + .
[0364] 1 H-NMR (CDCl 3 ) δ: 8.72 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.30-7.13 (3H, m), 3.65 (3H, s), 3.24 (2H, t, J=5.4 Hz), 2.75-2.69 (2H, m), 2.47 (2H, m), 2.30-1.50 (20H, m), 1.35-1.20 (2H, m), 0.76 (3H, t, J=6.0 Hz).
Step 4. 2-Ethyl-2-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}butanoic acid
[0365] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 2-ethyl-2-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}butanoate (step 3 of Example 6).
[0366] MS (ESI) m/z: 456 (M+H) + .
[0367] IR (KBr) ν: 3323, 2937, 1732, 1596, 1539, 1463, 1348, 1147, 746 cm −1
[0368] 1 H-NMR (CDCl 3 ) d: 8.80 (1H, br s), 8.22 (1H, d, J=8.1 Hz), 7.35-7.15 (3H, m), 3.31 (2H, t, J=6.0 Hz), 3.18-3.05 (2H, m), 2.61 (2H, s), 2.57-2.40 (2H, m), 2.30-1.25 (17H, m), 0.88 (6H, t, J=9.0 Hz). Signal due to CO 2 H was not observed.
[0369] Anal. Calcd. for C 26 H 37 N 3 O 4 .0.4H 2 O: C, 67.48; H, 8.23; N, 9.08. Found: C, 67.87; H, 8.13; N, 8.95.
Example 7
1-{[4-({[(6′-FLUORO-2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)—YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID
[0370]
Step 1. Ethyl 1-(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutanecarboxylate
[0371] The title compound was prepared according to the procedure described in step 3 of Example 8 from [cyclobutylidene(ethoxy)methoxy](trimethyl)silane (Kuo. Y.-N. et al., J, Chem. Soc. D., 1971, 136).
[0372] MS (ESI) m/z: 355 (M+H) + .
[0373] 1 H-NMR (CDCl 3 ) δ: 4.55 (1H, br), 4.17 (2H, q, J=7.1 Hz), 2.96 (2H, t, J=6.3 Hz), 2.76 (2H, d, J=11.4 Hz), 2.48-2.33 (2H, m), 2.05-1.80 (6H, m), 1.43 (9H, s), 1.25 (3H, q, J=7.1 Hz), 1.40-1.05 (7H, m).
Step 2. 1-[(4-{[(tert-Butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutanecarboxylic acid
[0374] A mixture of ethyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutanecarboxylate (4.2 g, 11.9 mmol, step 1 of Example 7), 2N NaOH (18 mL) and ethanol (12 mL) was heated at 50° C. for 4 h. The resulting solution was cooled in ice bath and 2N HCl (ca 19 mL) was added until pH of the mixture was ca 5-6. The whole was extracted with CH 2 Cl 2 /i-propanol (3:1, 30 mL×3). Combined organic layers were dried (Na 2 SO 4 ) and filtered. The filtrate was concentrated to give 3.8 g (98%) of the titled compound as yellow solid.
[0375] 1 H-NMR (CDCl 3 ) δ: 4.08 (1H, m), 3.20-3.10 (2H, m), 3.08-2.99 (2H, m), 2.91 (2H, s), 2.60-2.38 (4H, m), 2.35-2.16 (2H, m), 2.05-1.76 (6H, m), 1.65 (1H, m), 1.44 (9H, s)
Step 3. 1-{[4-(Aminomethyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid 4-methylbenzenesulfonate
[0376] In a 500 mL, 3-necked round bottom flask under N 2 , a mixture of 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclobutane carboxylic acid (30 g, 92 mmol, step 2 of Example 7) in tetrahydrofuran (150 mL) was stirred at room temperature for 10 min. To this suspension, a solution of p-toluensulfonic acid monohydrate (52.4 g, 276 mmol) in tetrahydrofuran (150 mL) was added at room temperature. After stirring at that temp for 10 min, the resulting solution was heated under reflux condition for 3 h. After cooling down to room temperature, triethylamine (28.1 mL, 202 mmol) was added very slowly during the period of 1 h with seeding. The white precipitate was formed during the addition of triethylamine. The resulting white suspension was stirred at room temperature for 6 h and it was filtered and the obtained solid was washed with tetrahydrofuran (100 mL×2), dried at 50° C. for 5 h to give 35 g (96%) of the titled compound as white powder.
[0377] m.p.: 210° C.
[0378] 1 H-NMR (D 2 O) δ: 7.40 (2H, d, J=7.2 Hz), 7.07 (2H, d, J=7.2 Hz), 3.28-3.00 (4H, m), 2.80-2.57 (4H, m), 2.09 (3H, s), 2.18-1.97 (2H, m), 1.85-1.58 (8H, m), 1.36-1.12 (2H, m)
Step 4. 1-{[4-({[(6′-Fluoro-2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid
[0379] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6′-fluorospiro[cyclopentane-1,3′-indol]-2′(1′H)-one (Joensson, N et al., Acta Chem. Scand. Ser. B, 1974, 28, 225) and 1-{[4-(aminomethyl)piperidine-1-yl]methyl}cyclobutanecarboxylic acid 4-methylbenzene sulfonate (step 3 of Example 7).
[0380] MS (ESI) m/z: 458 (M+H) + .
[0381] m.p.: 150.3° C.
[0382] IR (KBr) ν: 3305, 2935, 1735, 1602, 1492, 1440, 1357, 1296, 1228, 1157, 1095, 869 cm −1
[0383] 1 H-NMR (CDCl 3 ) δ: 8.73 (1H, br s), 8.01 (1H, dd, J=5.4, 8.1 Hz), 6.92-6.83 (1H, m), 3.30 (2H, t, J=5.4
[0384] Hz), 3.15-3.03 (2H, m), 2.78 (3H, s), 2.64-2.50 (2H, m), 2.45-1.70 (16H, m), 1.55-1.36 (2H, m). A signal due to CO 2 H was not observed.
[0385] Anal. Calcd. for C 25 H 32 FN 3 O 4 .0.4H 2 O: C, 64.61; H, 7.11; N, 9.01. Found: C, 64.31; H, 7.11; N, 9.05.
Example 8
4-{[4-({[(6′-FLUORO-2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)—YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}TETRAHYDRO-2H-PYRAN-4-CARBOXYLIC ACID
[0386]
Step 1. tert-Butyl {[1-(ethoxymethyl)piperidin-4-yl]methyl}carbamate
[0387] To a stirred solution of tert-butyl(piperidin-4-ylmethyl)carbamate (7.0 g, 33 mmol) in ethanol (19 mL), paraformaldehyde (1.2 g, 39 mmol) and K 2 CO 3 (5.4 g, 39 mmol) were added at ambient temperature. The mixture was stirred at ambident temperature for 4 h. The mixture was filtered and the filter cake was washed with ethanol (50 mL). The volatile components were removed by evaporation to give 8.9 g (quant.) of the title compound as a white powder.
[0388] 1 H-NMR (CDCl 3 ) δ: 4.60 (1H, br s), 4.07 (2H, s), 3.49 (2H, q, J=7.1 Hz), 3.08-2.83 (4H, m), 2.50-2.36 (2 H, m), 1.75-1.60 (2H, m), 1.44 (9H, s), 1.52-1.35 (1H, m), 1.19 (3H, t, J=7.1 Hz), 1.31-1.12 (2H, m).
Step 2. [Methoxy(tetrahydro-4H-pyran-4-ylidene)methoxy](trimethyl)silane
[0389] To a stirred solution of diisopropylamine (1.6 g, 0.016 mol) in tetrahydrofuran (4 mL) was added dropwise n-butyllithium (1.59 M in hexane, 9.2 mL, 0.014 mol) at 0° C. under nitrogen, and stirred for 20 min. Then, the reaction mixture was cooled to −40° C., methyl tetrahydro-2H-pyran-4-carboxylate (1.9 g, 0.013 mol) and trimethylsilyl chloride (2.0 mL, 0.015 mol) in tetrahydrofuran (1 mL) was added, and the resulting mixture was gradually warmed to room temperature over 3 h. The volatile components were removed by evaporation and the residue was filtered through a pad of Celite washing with hexane. The filtrate was dried in vacuo to give 2.9 g (quant.) of the title compound as a clear yellow oil.
[0390] 1 H-NMR (CDCl 3 ) δ: 3.64-3.59 (4H, m), 3.52 (3H, s), 2.24 (2H, t, J=5.2 Hz), 2.15 (2H, t, J=5.3 Hz), 0.22 (9H, s).
Step 3. Methy 4-[(4-}[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]tetrahydro-2H-pyran-4-carboxylate
[0391] To a stirred solution of tert-butyl {[1-(ethoxymethyl)piperidin-4-yl]methyl}carbamate (4 g, 14 mmol, step 1 of Example 8) and [methoxy(tetrahydro-4H-pyran-4-ylidene)methoxy](trimethyl)silane (2.9 g, 13 mmol, step 2 of Example 8) in CH 2 Cl 2 (30 mL) was added dropwise trimethylsilyl trifluoromethanesulfonate (0.24 mL, 1.3 mmol) at 0° C., and the resulting mixture was stirred at room temperature for 12 h. The reaction mixture was quenched with saturated aqueous sodium bicarbonate (150 mL), extracted with CH 2 Cl 2 (30 mL×2), and the combined organic layer was dried over sodium sulfate and filtered. Removal of the solvent gave a residue, which was chromatographed on a column of silica gel eluting with ethyl acetate/hexane (1:1) to give 6.3 g (64%) of the title compound as clear colorless oil.
[0392] MS (ESI) m/z: 371 (M+H) + .
[0393] 1 H-NMR (CDCl 3 ) δ: 4.57 (1H, br s), 3.84-3.78 (2H, m), 3.70 (3H, s), 3.49-3.41 (2H, m), 2.99-2.95 (2H, m), 2.73-2.68 (2H, m), 2.47 (2H, s), 2.19-2.11 (2H, m), 2.06-2.01 (2H, m), 1.61-1.51 (5H, m), 1.44 (9H, s), 1.24-1.11 (2H, m).
Step 4. 4-[(4-}[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]tetrahydro-2H-pyran-4-carboxylic acid
[0394] To a solution of methyl 4-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidine-1-yl)methyl]tetrahydro-2H-pyran-4-carboxylate (6.47 g, 17.5 mmol, step 3 of Example 8) in methanol (32 mL), 5 N NaOH aq (10 mL) was added at room temperature (exothermic). The resulting solution was stirred at 60° C. for 7 h, then cooled to 5-10° C. in ice-cold bath. To this solution, 5 N HCl aq (10 mL) was added and the resulting solution (pH value was ca.6) was concentrated. To the residue, 2-propanol (80 mL) was added. This solution was concentrated. To the residue, 2-propanol (80 mL) was added and it was concentrated again. The residue was diluted with ethanol (80 mL) and the mixture was stirred at room temperature for 2 h. It was filtered through a Celite pad (5.0 g) to remove NaCl. The Celite pad was washed with ethanol (20 mL) and the combined filtrate was concentrated. To the residue, CH 3 CN (40 mL) was added and it was concentrated. During this procedure, the formation of white precipitate was noticed. To the residue, CH 3 CN (40 mL) was added and the resulting suspension was stirred at room temperature for 2 h. This mixture was filtered and obtained solid was washed with CH 3 CN (10 mL), then dried under reduced pressure to give 4.1 g (65%) of the titled compound as white powder.
[0395] m.p.: 129° C.
[0396] 1 H NMR (CDCl 3 ) δ: 4.66 (1H, m), 3.93-3.82 (3H, m), 3.15-2.99 (4H, m), 2.58 (2H, s), 2.58-2.45 (2H, m), 1.98-1.76 (4H, m), 1.55-1.35 (6H, m), 1.44 (9H, s).
Step 5. 4-{[4-(aminomethyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylic acid 4-methylbenzenesulfonate
[0397] In a 300 mL, 3-necked round bottom flask under N 2 , 4-[(4-{[(tert-butoxy carbonyl)amino]methyl}piperidin-1-yl)methyl]tetrahydro-2H-pyran-4-carboxylic acid (10 g, 28 mmol, step 4 of Example 8) was placed and a solution of p-toluenesulfonic acid monohydrate (16 g, 84 mmol) in i-propanol (150 mL) was poured at room temperature. The resulting mixture was stirred at 60° C. for 7 h under N 2 and triethylamine (8.6 mL, 62 mmol) was added dropwise slowly during the period of 2 hr with seeding. The white precipitate was formed during the addition of triethylamine. The resulting white suspension was stirred at 60° C. for 3 h, at 50° C. for 5 h and at room temperature for 10 h. The suspension was filtered and the obtained solid was washed with i-propanol (100 mL), dried at 50° C. for 5 h to give 10.5 g (87%) of the titled compound as white powder.
[0398] m.p.: 247° C.
[0399] 1 H-NMR (D 2 O) δ: 7.54 (2H, d, J=7.4 Hz), 7.22 (2H, J=7.4 Hz), 3.80-3.65 (2H, m), 3.55-3.40 (4H, m), 3.20-2.75 (6H, m), 2.24 (3H, s), 1.90-1.80 (6H, m), 1.55-1.35 (4H, m)
Step 6. 4-{[4-({[(6′-Fluoro-2′-oxospiro[cyclopentane-1,3′-indol[-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylic acid
[0400] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6′-fluorospiro[cyclopentane-1,3′-indol]-2′(1′H)-one (Joensson, N et al., Acta Chem. Scand. Ser. B, 1974, 28, 225) and 4-{[4-(amino methyl)piperidine-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylic acid 4-methyl benzenesulfonate (step 5 of Example 8).
[0401] MS (ESI) m/z: 488 (M+H) + .
[0402] m.p.: 161.3° C.
[0403] IR (KBr) ν: 3315, 2943, 2869, 1733, 1604, 1541, 1473, 1359, 1298, 1228, 1157, 1099, 867 cm −1
[0404] 1 H-NMR (CDCl 3 ) δ: 7.16-7.11 (1H, m), 6.90-6.84 (1H, m), 3.90-3.75 (4H, m), 3.31 (2H, t, J=6.0 Hz), 3.18-3.06 (2H, m), 2.65-2.45 (4H, m), 2.25-1.75 (13H, m), 1.58-1.40 (4H, m). Signal due to CO 2 H was not observed.
[0405] Anal. Calcd. for C 26 H 34 FN 3 O 5 .0.4H 2 O: C, 63.12; H, 7.09; N, 8.49. Found: C, 62.83; H, 7.09; N, 8.45.
Example 9
1-{[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID
[0406]
[0407] The title compound was prepared according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid 4-methylbenzenesulfonate (step 3 of Example 7).
[0408] MS (ESI) m/z: 414 (M+H) + .
[0409] m.p.: 170.9° C.
[0410] IR (KBr) ν: 3440, 3296, 2933, 1735, 1705, 1608, 1541, 1382, 1346, 1271, 1159, 966, 773 cm −1
[0411] 1 H-NMR (CDCl 3 ) δ: 8.78 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.35-7.18 (2H, m), 3.31 (2H, t, J=5.4 Hz), 3.12-3.01 (2H, m), 2.78 (2H, s), 2.61-2.48 (2H, m), 2.45-2.25 (3H, m), 2.00-1.75 (6H, m), 1.44 (3H, s), 1.55-1.40 (6H, m). A signal due to CO 2 H was not observed.
[0412] Anal. Calcd. for C 23 H 31 N 3 O 4 .0.4H 2 O: C, 65.66; H, 7.62; N, 9.99. Found: C, 65.82; H, 7.64; N, 9.89.
Example 10
3-[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]PROPANOIC ACID
[0413]
Step 1. Ethyl 3-(4-{[(tert-butoxycarbonynamino]methyl}piperidin-1-yl)propanoate
[0414] A mixture of tert-butyl(piperidin-4-ylmethyl)carbamate (3.0 g, 14 mmol) and ethyl acrylate (1.7 g, 17 mmol) in ethanol (30 mL) was refluxed for 1 h. After cooled to room temperature, the solution was concentrated to give clear colorless oil. The residue was chromatographed on a silica gel column eluting with CH 2 Cl 2 /methanol (14:1) to give 4.0 g (91%) of the title compound as clear colorless oil.
[0415] MS (ESI) m/z: 315 (M+H) + .
[0416] 1 H-NMR (CDCl 3 ) δ: 4.61 (1H, br s), 4.13 (2H, q, J=8.1 Hz), 3.01 (2H, t, J=5.4 Hz), 2.98-2.80 (2H, m), 2.05-1.90 (2H, m), 1.70-1.60 (2H, m), 1.44 (9H, s), 1.25 (3H, t, J=8.1H), 1.55-1.20 (4H, m).
Step 2. Ethyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoate
[0417] To a stirred solution of ethyl 3-(4-{[(tert-butoxycarbonypamino]methyl}piperidin-1-yl)propanoate (500 mg, 1.6 mmol, step 1 of Example 10) in CH 2 Cl 2 (5 mL), trifluoroacetic acid (1.2 mL, 16 mmol) was added and stirred overnight at room temperature. The mixture was concentrated, and the residual oil was dissolved in CH 2 Cl 2 (60 mL) and solid K 2 CO 3 (5 g) was added, and stirred for 10 min. The mixture was filtered, and the filtrate was concentrated to give ethyl 3-[4-(aminomethyl)piperidin-1-yl]propanoate as a pale yellow oil. Following coupling reaction was carried out according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and ethyl 3-[4-(aminomethyl)piperidin-1-yl]propanoate.
[0418] MS (ESI) m/z: 428 (M+H) + .
[0419] 1 H-NMR (CDCl 3 ) δ: 8.73 (1H, br s), 8.25 (1H, d, J=8.1 Hz), 7.34-7.10 (2H, m), 4.13 (2H, q, J=8.1 Hz), 3.29 (2H, t, J=5.4 Hz), 2.98-2.85 (2H, m), 2.69 (2H, t, J=8.1 Hz), 2.49 (2H, t, J=8.1 Hz), 2.05-1.95 (2H, m), 1.81-1.70 (2H, m), 1.50-1.20 (13H, m).
Step 3. 3-[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoic acid
[0420] The title compound was prepared according to the procedure described in step 4 of Example 2 from ethyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl) carbonyl]amino}methyl)piperidin-1-yl]propanoate (step 2 of Example 10).
[0421] MS (ESI) m/z: 374 (M+H) + .
[0422] IR (KBr) ν: 3315, 1733, 1606, 1541, 1460, 1379, 1344, 1269, 1163, 958, 769 cm −1
[0423] 1 H-NMR (CDCl 3 ) δ: 8.79 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.40-7.15 (3H, m), 3.40-3.24 (2H, m), 3.20-3.18 (2H, m), 2.85-2.73 (2H, m), 2.39-2.21 (2H, m), 2.00-1.75 (3H, m), 1.55-1.30 (10H, m). Signal due to CO 2 H was not observed.
[0424] Anal. Calcd. for C 20 H 27 N 3 O 4 .1.0H 2 O.0.5MeOH.0.2CH 2 Cl 2 ; C, 58.57; H, 7.46; N, 9.90. Found: C, 58.94; H, 7.16; N, 9.81.
Example 11
3-[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]-2,2-DIMETHYLPROPANOIC ACID
[0425]
Step 1. tert-Butyl 4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidine-1-carboxylate
[0426] The title compound was prepared according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and tert-butyl 4-(aminomethyl)piperidine-1-carboxylate.
[0427] MS (ESI) m/z: 402 (M+H) + .
[0428] 1 H-NMR (CDCl 3 ) δ: 8.76 (1H, br s), 8.24 (1H, d, J=8.1 Hz), 7.34-7.15 (3H, m), 4.25-4.03 (2H, m), 3.36-3.23 (2H, m), 2.79-2.60 (2H, m), 1.85-1.69 (2H, m), 1.55-1.36 (16H, m), 1.30-1.10 (2H, m).
Step 2. 3,3-Dimethyl-2-oxo-N-(piperidin-4-ylmethyl)indoline-1-carboxamide
[0429] The title compound was prepared according to the procedure described in step 2 of Example 2 from tert-butyl 4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl) carbonyl]amino}methyl)piperidine-1-carboxylate (step 1 of Example 11).
[0430] MS (ESI) m/z: 302 (M+H)+.
[0431] 1 H-NMR (CDCl 3 ) δ: 8.74 (1H, br s), 8.25 (2H, d, J=8.1 Hz), 7.34-7.15 (3H, m), 3.29 (2H, t, J=5.4 Hz), 3.15-3.05 (2H, m), 2.67-2.55 (2H, m), 1.80-1.74 (2H, m), 1.43 (6H, s), 1.28-1.18 (2H, m). A signal due to N H (piperidine) was not observed.
Step 3. Methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl-2,2-dimethylpropanoate
[0432] The title compound was prepared according to the procedure described in step 3 of Example 2 from 3,3-dimethyl-2-oxo-N-(piperidin-4-ylmethyl)indoline-1-carboxamide (step 2 of Example 11).
[0433] MS (ESI) m/z: 416 (M+H) + .
[0434] 1 H-NMR (CDCl 3 ) δ: 8.70 (1H, br s), 8.25 (1H, d, J=6.0 Hz), 7.33-7.15 (3H, m), 3.65 (3H, s), 3.25 (2H, t, J=6.0 Hz), 2.84-2.72 (2H, m), 2.46 (2H, s), 2.23-2.10 (3H, m), 1.73-1.54 (2H, m), 1.43 (6H, m), 1.38-1.24 (2H, m), 1.15 (6H, s).
Step 4. 3-[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-di methylpropanoic acid
[0435] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl) carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate (step 3 of Example 11).
[0436] MS (ESI) m/z: 402 (M+H) + .
[0437] m.p.: 164.5° C.
[0438] IR (KBr) ν: 3402, 3317, 2943, 2858, 1616, 1596, 1541, 1498, 1307, 1263, 1105, 985 cm −1
[0439] 1 H-NMR (CDCl 3 ) δ: 8.78 (1H, br s), 8.24 (1H, d, J=8.1 Hz), 7.34-7.18 (3H, m), 3.32 (2H, t, J=6.0 Hz), 3.24-3.06 (2H, m), 2.60-2.38 (4H, m), 1.97-1.65 (3H, m), 1.60-1.28 (8H, m), 1.24 (6H, s). A signal due to CO 2 H was not observed.
[0440] Anal. Calcd. for C 22 H 31 N 3 O 4 : C, 65.81; H, 7.78; N, 10.47. Found: C, 65.56; H, 7.83; N, 10.36.
Example 12
3-[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)-4-HYDRO XYPIPERIDIN-1-YL]-2,2-DIMETHYLPROPANOIC ACID
[0441]
Step 1. N-[(1-benzyl-4-hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide
[0442] The title compound was prepared according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and 4-(aminomethyl)-1-benzylpiperidin-4-ol (Somanathan, R. et al., Synth. Commun., 1994, 24, 1483)
[0443] MS (ESI) m/z: 408 (M+H) + .
[0444] 1 H-NMR (CDCl 3 ) δ: 8.93 (1H, br s), 8.23 (1H, d, J=8.1 Hz), 7.35-7.16 (8H, m), 5.30 (2H, s), 3.54 (2H, s), 3.45 (2H, d, J=5.4 Hz), 2.70-2.56 (2H, m), 2.46-2.33 (2H, m), 2.27 (1H, s), 1.80-1.67 (2H, m), 1.43 (6H, m).
Step 2. N-[(4-Hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide
[0445] A mixture of N-[(1-benzyl-4-hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide (280 mg, 0.68 mmol, step 1 of Example 12) and palladium hydroxide (80 mg, 20 wt. % Pd on carbon,) in 10% HCl in methanol was stirred under H 2 atmosphere for 20 h. The mixture was filtered through a pad of Celite, washed with methanol and the filtrate was concentrated to give pale yellow oil. The residue was chromatographed on silica gel column eluting with CH 2 Cl 2 /methanol/NH 4 OH (10:1:0.2) to give 73 mg (34%) of the title compound as clear yellow oil.
[0446] MS (ESI) m/z: 318 (M+H) + .
[0447] 1 H-NMR (CDCl 3 ) δ: 8.95 (1H, br s), 8.25-8.16 (1H, m), 7.35-7.12 (3H, m), 3.51-3.40 (4H, m), 3.05-2.80 (4H, m), 1.75-1.55 (2H, m), 1.44 (6H, s).
Step 3. Methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidin-1-yl-2,2-dimethylpropanoate
[0448] The title compound was prepared according to the procedure described in step 3 of Example 2 from N-[(4-hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide (step 2 of Example 12).
[0449] Rf: 0.25 (aminopropyl-silica gel; hexane/ethyl acetate (2/1))
[0450] MS (ESI) m/z: 432 (M+H) f .
Step 4. 3-[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidin-1-yl]-2,2-dimethylpropanoic acid
[0451] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate (step 3 of Example 12).
[0452] MS (ESI) m/z: 418 (M+H) + .
[0453] 1 H-NMR (CDCl 3 ) δ: 9.01 (1H, br s), 8.20 (1H, d, J=8.1 Hz), 7.33-7.15 (3H, m), 3.50-3.45 (2H, m), 3.00-2.85 (4H, m), 2.65-2.55 (2H, m), 1.81-1.45 (4H, m), 1.45 (6H, s), 1.25 (6H, s). Signals due to OH and CO 2 H were not observed.
[0454] HRMS (FAB) (M+H) + calcd for C 22 H 32 O 5 N 3 418.2342, found 418.2356
Example 13
1-{[4-({[(2′-OXOSPIRO[CYCLOPENTANE-1,3′-INDOL]-1′(2′H)-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOHEXANECARBOXYLIC ACID
[0455]
Step 1. Methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclohexanecarboxylate
[0456] The title compound was prepared with the similar method shown in the step 3 of Example 8 by using [cyclohexylidene(methoxy)methoxy](trimethyl)silane (Hannaby, Malcolm et al., J. Chem. Soc. Perkin Trans. 1, 1989, 303)
[0457] MS (ESI) m/z: 369 (M+H) + .
[0458] 1 H-NMR (CDCl 3 ) δ: 4.56 (1H, br s), 3.66 (3H, s), 2.97 (2H, t, J=6.1 Hz), 2.71 (2H, br d, J=11.7 Hz), 2.43 (2H, s), 2.11 (2H, br t, J=11.5 Hz), 2.03 (2H, br d, J=11.4 Hz), 1.65-1.10 (22H, m).
Step 2. Methyl 1-{[4-({[(2′-oxospiroicyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclohexanecarboxylate
[0459] The title compound was prepared with the similar method shown in the step 2 of Example 10 from methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclohexanecarboxylate (step 1 of Example 13).
[0460] MS (ESI) m/z: 482 (M+H) + .
[0461] 1 H-NMR (CDCl 3 ) δ: 8.71 (1H, br s), 8.23 (1H, d, J=9.0 Hz), 7.34-7.15 (3H, m), 3.66 (3H, s), 3.24 (2H, t, J=6.0 Hz), 2.80-2.68 (2H, m), 2.44 (2H, s), 2.25-1.15 (25H, m).
Step 3. 1-{[4-({[(2′-Oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl]piperidin-1-yl]meth yl}cyclohexanecarboxylic acid
[0462] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 1-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclohexanecarboxylate (step 2 of Example 13).
[0463] MS (ESI) m/z: 468 (M+H) + .
[0464] m.p.: 160.4° C.
[0465] IR (KBr) ν: 3300, 2923, 2862, 1728, 1600, 1552, 1469, 1346, 1265, 1222, 1143, 752 cm −1
[0466] 1 H-NMR (CDCl 3 ) δ: 8.80 (1H, br s), 8.21 (1H, d, J=9.0 Hz), 7.32-7.13 (3H, m), 3.30 (2H, t, J=6.0 Hz), 3.16-3.03 (2H, m), 2.60 (2H, s), 2.55-2.40 (2H, m), 2.27-1.26 (23H, m). A signal due to CO 2 H was not observed.
[0467] Anal. Calcd. for C 27 H 37 N 3 O 4 .0.8H 2 O: C, 67.28; H, 8.07; N, 8.72. Found: C, 67.46; H, 8.05; N, 8.66.
Example 14
2′-OXO-N-[(1-{[1-(1H-TETRAZOL-5-YL)CYCLOPENTYL]METHYL}PIPERIDIN-4-YL)METHYL]SPIRO[CYCLOPENTANE-1,3′-INDOLE]-1′(2′H)-CARBOXAMIDE
[0468]
Step 1. α-Cyclopentyltetrazole-5-acetic acid ethyl ester
[0469] To a stirred solution of 1-cyano-1-cyclopentanecarboxylic acid ethyl ester (6.19 g, 37.0 mmol, Bioorg. Med. Chem. Lett. 1999, 9, 369-374) in 1,4-dioxane (100 mL) was added (CH 3 CH 2 CH 2 CH 2 ) 3 SnN 3 (12.3 g, 37.0 mmol) at ambient temperature. The resulting mixture was refluxed for 15 h and concentrated under reduced pressure. To the resulting residue was added 4 M HCl in 1,4-dioxane (50 mL) and concentrated under reduced pressure. The resulting oil was washed twice with hexane to give crude product of the title compound as a yellow oil, which was used for next step without further purification.
Step 2. 2-Benzyl-α-cyclopentyl-2H-tetrazole-5-acetic acid, ethyl ester
[0470] To a stirred mixture of α-cyclopentyltetrazole-5-acetic acid, ethyl ester (step 1 of Example 14) and K 2 CO 3 (12.3 g, 89.0 mmol) in acetone (200 mL) was added benzyl bromide (4.84 mL, 40.7 mmol) at ambient temperature. The resulting mixture was stirred at 50° C. for 14 h and concentrated under reduced pressure. The resulting residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (10:1) to give 2.95 g (27% in 2 steps) of the title compound.
[0471] MS (ESI) m/z: 301 (M+H) + .
[0472] 1 H NMR (CDCl 3 ) δ 7.45-7.23 (5H, m), 5.73 (2H, s), 4.11 (2H, q, J=7.1 Hz), 2.55-2.35 (4H, m), 1.88-1.56 (4H, m), 1.12 (3H, t, J=7.1 Hz).
Step 3. 2-Benzyl-α-cyclopentyl-2H-tetrazole-5-acetaldehyde
[0473] To a stirred mixture of 2-benzyl-α-cyclopentyl-2H-tetrazole-5-acetic acid, ethyl ester (2.92 g, 9.72 mmol, step 2 of Example 14) in CH 2 Cl 2 (50 mL) at −78° C. was added diisobutylaluminium hydride (1.0 M in toluene, 22.5 mL, 22.5 mmol). The resulting mixture was stirred at −78° C. for 5 h. To the mixture were added 2 M aqueous HCl (50 mL) and saturated aqueous NH 4 Cl (10 mL). The organic layer was separated, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was chromatographed on a column of silica gel eluting with Hexane/ethyl acetate (10:1) to give 862 mg (35%) of the title compound.
[0474] MS (ESI) m/z: 257 (M+H) + .
[0475] 1 H NMR (CDCl 3 ) δ 9.71 (1 H, s), 7.50-7.30 (5 H, m), 5.74 (2 H, s), 2.45-2.18 (4 H, m), 1.85-1.66 (4 H, m).
Step 4. tert-Butyl[{1-(2-(2-benzyltetrazole)-2-cyclopentylmethyl)piperidin-4-yl}methyl]carbamate
[0476] To a stirred solution of 2-benzyl-α-cyclopentyl-2H-tetrazole-5-acetaldehyde (850 mg, 3.32 mmol, step 3 of Example 14) and tert-butyl(piperidin-4-ylmethyl)carbamate (7.11 g, 33.2 mmol) in tetrahydrofuran (500 mL) were added NaBH(O(CO)CH 3 ) 3 (3.52 g, 16.6 mmol) and acetic acid (1.03 g, 16.9 mmol). The resulting mixture was stirred at 60° C. for 13 h and concentrated under reduced pressure. To the stirred residue were added saturated aqueous NaHCO 3 and CH 2 Cl 2 . The organic layer was separated, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (1:1) to give 1.19 g (79%) of the title compound.
[0477] MS (ESI) m/z: 455 (M+H) + .
[0478] 1 H NMR (CDCl 3 ) δ 7.43-7.23 (5H, m), 5.72 (2H, s), 4.67 (1H, br t), 2.88 (2H, m), 2.66 (2H, br s), 2.48 (2H, m), 2.24 (2H, m), 1.93 (2H, m), 1.83 (2H, m), 1.78-1.48 (4H, m), 1.43 (9H, s), 1.37 (2H, m), 1.23 (1H, m), 0.94 (2H, m).
Step 5. ({1-[1-(2-Benzyl-2H-tetrazol-5-yl)cyclopentyl]piperidin-4-yl}methyl)amine
[0479] A mixture of tert-butyl[{1-(2-(2-benzyltetrazole)-2-cyclopentylethyl)piperidin-4-yl}methyl]carbamate (150 mg, 0.34 mmol, step 4 of Example 14) and 10% HCl in methanol (10 mL) was stirred for 3 h at 60° C., and the mixture was concentrated to give yellow oil. The residue was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol/NH 4 OH (12:1:0.1) to give 115 mg (quant.) of the title compound as clear yellow solid.
[0480] 1 H NMR (CDCl 3 ) δ 7.50-7.25 (5H, m), 5.73 (2H, s), 2.67 (2H, s), 2.60-2.40 (4H, m), 2.35-2.16 (2H, m), 2.05-1.78 (4H, m), 1.75-1.34 (6H, m), 1.20-0.85 (3H, m).
Step 6. N-[(1-{[1-(2-Benzyl-2H-tetrazol-5-yl)cyclopentyl]methyl}piperidin-4-yl)methyl]-2′-oxospiro[cyclopentane-1,3′-indole]-1′(2′H)-carboxamide
[0481] The title compound was prepared according to the procedure described in step 6 of Example 1 from ({1-[1-(2-benzyl-2H-tetrazol-5-yl)cyclopentyl]piperidin-4-yl}methyl)amine (step 5 of Example 14).
[0482] MS (ESI) m/z: 568 (M+H) + .
[0483] 1 H NMR (CDCl 3 ) δ 8.66 (1H, br s), 8.23 (1H, d, J=9.0 Hz), 7.40-7.15 (3H, m), 5.73 (2H, s), 3.15 (2H, t, J=6.0 Hz), 2.67 (2H, s), 2.54-2.44 (2H, m), 2.26-2.11 (4H, m), 2.10-1.76 (10H, m), 1.70-0.90 (14H, m).
Step 7. 2′-Oxo-N-[(1-{[1-(2H-tetrazol-5-yl)cyclopentyl]methyl}piperidin-4-yl)methyl}spiro[cyclopentane-1,3′-indole]-1′(2′H)-carboxamide
[0484] A mixture of N-[(1-{[1-(2-benzyl-2H-tetrazol-5-yl)cyclopentyl]methyl}piperidin-4-yl)methyl]-2′-oxospiro[cyclopentane-1,3′-indole]-1′(2′H)-carboxamide (120 mg, 0.21 mmol, step 6 of Example 14) and palladium hydroxide (20 mg, 20 wt. % palladium on carbon) in methanol (10 mL) was stirred for 8 h under H 2 atmosphere. The mixture was filtered through a pad of Celite, and washed with methanol and the filtrate was concentrated to give a clear colorless oil. The residue was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /methanol (16:1) to give 80 mg (80%) of the title compound as a white solid. The solid was triturated with ethyl acetate/hexane and collected by filtration to give 72 mg (72%) of the title compound as a white solid.
[0485] MS (ESI) m/z: 478 (M+H) + .
[0486] IR (KBr) ν: 3417, 2958, 1732, 1703, 1548, 1465, 1282, 1161, 769 cm −1
[0487] 1 H NMR (CDCl 3 ) δ 8.81 (1H, br s), 8.22 (1H, d, J=9.0 Hz), 7.34-7.12 (3H, m), 3.40-3.27 (2H, m), 3.16-3.05 (2H, m), 2.45-2.31 (2H, m), 3.00-1.65 (21H, m), 1.58-1.41 (2H, m). A signal due to tetrazole-H was not observed.
[0488] Anal. Calcd. for C 26 H 35 N 7 O 2 .1.0H 2 O: C, 63.01; H, 7.52; N, 19.78. Found: C, 62.90; H, 7.35; N, 19.40.
Example 15
1-{[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID
[0489]
Step 1. Methyl 2-(4-fluoro-2-nitrophenyl)-2-methylpropanoate
[0490] A stirred mixture of methyl (4-fluoro-2-nitrophenyl)acetate (3.0 g, 0.014 mol, Quallich, George J et al., Synthesis, 1993, 351), methyl iodide (2 ml, 0.032 mol) and 18-crown-6 (925 mg, 3.5 mmol) in N,N-dimethylformamide (75 mL) was treated portion wise with NaH (1.28 g, 0.032 mol, 60% dispersion in mineral oil) at 0° C. Then the reaction mixture was stirred at room temperature for 2 h. It was quenched by addition of water. The aqueous layer was extracted with diethylether (25 mL×3). The organic layer was washed with water and brine, dried over sodium sulfate and concentrated in vacuo. The residue was chromatographed on a column of silica gel eluting with ethyl acetate/hexane (1:20 to 1:4) to give 2.52 g (75%) of the title compound as oil.
[0491] 1 H-NMR (CDCl 3 ) δ: 7.67 (1H, dd, J=8.3, 2.9 Hz), 7.59 (1H, dd, J=8.9, 5.4 Hz), 7.39-7.29 (1H, m), 3.66 (3 H, s), 1.66 (6H, s).
Step 2. 6-Fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one
[0492] A mixture of methyl 2-(4-fluoro-2-nitrophenyl)-2-methylpropanoate (2.53 g, 0.010 mol, step 1 of Example 15) and iron powder (2.34 g, 0.042 mol) in acetic acid (30 mL) was stirred at 100° C. for 5.5 h. The reaction mixture was rinsed with methanol and it was filtered through a pad of Celite. The filtrate was concentrated. It was added water and the aqueous layer was extracted with ethyl acetate (20 mL×3). The organic layer was washed with brine, dried over sodium sulfate and concentrated. The residue was chromatographed on a column of silica gel eluting with ethyl acetate/hexane (1:6 to 1:4) to give 1.67 g (89%) of the title compound as a white solid.
[0493] MS (ESI) m/z: 180 (M+H) + , 178 on-Hy.
[0494] 1 H-NMR (CDCl 3 ) δ: 7.84 (1H, br s), 7.12 (1H, dd, J=8.1, 5.3 Hz), 6.73 (1H, ddd, J=9.2, 8.1, 2.4 Hz), 6.65 (1H, dd, J=8.8, 2.4 Hz), 1.39 (6H, s).
Step 3. 1-{[4-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid
[0495] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 of Example 15) and 1-{[4-(aminomethyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid 4-methylbenzenesulfonate (step 3 of Example 7).
[0496] MS (ESI) m/z: 432 (M+H) + .
[0497] m.p.: 193° C.
[0498] IR (KBr) ν: 3300, 2934, 1740, 1605, 1547, 1477, 1385, 1352, 1304, 1236, 1151 cm −1 .
[0499] 1 H-NMR (CDCl 3 ) δ: 8.71 (1H, t, J=5.9 Hz), 8.03 (1H, dd, J=10.2, 2.5 Hz), 7.15 (1H, dd, J=8.2, 5.4 Hz), 6.94-6.84 (1H, m), 3.31 (2H, t, J=5.9 Hz), 3.13-3.00 (2H, m), 2.78 (2H, s), 2.61-2.44 (2H, m), 2.44-2.24 (3H, m), 2.01-1.80 (5H, m), 1.82-1.65 (1H, m), 1.54-1.42 (2H, m), 1.42 (6H, s). A signal due to CO 2 H was not observed.
[0500] Anal. Calcd. for C 23 H 30 N 3 O 4 F.0.7 H 2 O: C, 62.20; H, 7.13; N, 9.46. Found: C, 61.85; H, 7.14; N, 9.34.
Example 16
3-[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]PROPANOIC ACID
[0501]
Step 1. Ethyl 3-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoate
[0502] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 in Example 15) and ethyl 3-[4-(aminomethyl)piperidin-1-yl]propanoate (step 2 in Example 10).
[0503] MS (ESI) m/z: 420 (M+H) + .
[0504] 1 H-NMR (CDCl 3 ) δ: 8.67 (1H, br s), 8.05 (1H, dd, J=10.2, 2.6 Hz), 7.14 (1H, dd, J=7.7, 5.4 Hz), 6.93-6.84 (1H, m), 4.14 (2H, dd, J=14.3, 7.2 Hz), 3.29 (2H, t, J=6.2 Hz), 2.96-2.86 (2H, m), 2.70 (2H, t, J=7.5 Hz), 2.50 (2H, t, J=7.5 Hz), 2.06-1.93 (2H, m), 1.82-1.65 (2H, m), 1.43-1.28 (2H, m), 1.42 (6H, s), 1.27 (3H, t, J=14.3 Hz). A signal due to C H was not observed.
Step 2. 3-[4-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoic acid
[0505] The title compound was prepared according to the procedure described in step 4 of Example 2 from ethyl 3-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]propanoate (step 1 of Example 16).
[0506] MS (ESI) m/z: 392 (M+H) + .
[0507] IR (KBr) ν: 3317, 2972, 2937, 1728, 1603, 1545, 1493, 1385, 1354, 1304, 1273, 1155, 1111, 1072 cm −1 .
[0508] 1 H-NMR (CDCl 3 ) δ: 8.72 (1H, br s), 8.03 (1H, dd, J=10.5, 2.5 Hz), 7.15 (1H, dd, J=8.5, 5.4 Hz), 8.89 (1H, dt, J=8.5, 2.5 Hz), 3.23 (2H, t, J=6.3 Hz), 3.25-3.12 (2H, m), 2.79 (2H, t, J=6.3 Hz), 2.53 (2H, t, J=6.3 Hz), 2.38-2.24 (2H, m), 1.99-1.86 (2H, m), 1.90-1.70 (1H, m), 1.56-1.35 (2H, m), 1.43 (6H, s). A signal due to CO 2 H was not observed.
[0509] HRMS (ESI) m/z calcd for C 20 H 27 FN 3 O 4 ([M+H] + ) 392.1986, found 392.1993.
Example 17
3-[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]-2,2-DIMETHYLPROPANOIC ACID
[0510]
Step 1. tert-Butyl 4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidine-1-carboxylate
[0511] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 of Example 15) and tert-butyl 4-(aminomethyl)piperidine-1-carboxylate.
[0512] 1 H-NMR (CDCl 3 ) δ: 8.69 (1H, t, J=5.5 Hz), 8.04 (1H, dd, J=10.2, 2.4 Hz), 7.15 (1H, dd, J=8.3, 5.5 Hz), 6.92-6.84 (1H, m), 4.24-4.03 (2H, m), 3.34-3.24 (2H, m), 2.78-2.60 (2H, m), 1.80-1.64 (3H, m), 1.46 (9H, s), 1.42 (6H, s), 1.29-1.10 (2H, m).
Step 2. 6-Fluoro-3,3-dimethyl-2-oxo-N-(piperidin-4-ylmethyl)indoline-1-carboxamide
[0513] The title compound was prepared according to the procedure described in step 2 of Example 2 from tert-butyl 4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidine-1-carboxylate (step 1 of Example 17).
[0514] MS (ESI) m/z: 320 (M+H) + .
[0515] 1 H-NMR (CDCl 3 ) δ: 8.68 (1H, br s), 8.05 (1H, dd, J=10.3, 2.4 Hz), 7.15 (1H, dd, J=8.3, 5.5 Hz), 6.93-6.83 (1H, m), 3.29 (2H, t, J=6.0 Hz), 3.25-3.08 (2H, m), 2.65 (2H, dt, J=12.2, 2.3 Hz), 1.89-1.65 (3H, m) 1.42 (6H, s), 1.40-1.15 (2H, m).
Step 3. Methyl 3-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate
[0516] The title compound was prepared according to the procedure described in step 3 of Example 2 from 6-fluoro-3,3-dimethyl-2-oxo-N-(piperidin-4-ylmethyl)indoline-1-carboxamide (step 2 of Example 17).
[0517] MS (ESI) m/z: 434 (M+H) + .
[0518] 1 H-NMR (CDCl 3 ) δ: 8.63 (1H, br s), 8.05 (1H, dd, J=10.4, 2.5 Hz), 7.14 (1H, dd, J=8.3, 5.5 Hz), 6.92-6.83 (1H, m), 3.66 (3H, s), 3.25 (2H, t, J=6.3 Hz), 2.83-2.73 (2H, m), 2.47 (2H, s) 2.16 (2H, dt, J=11.6, 2.0 Hz), 1.71-1.56 (2H, m) 1.56-1.44 (1H, m), 1.42 (6H, s), 1.36-1.22 (2H, m), 1.15 (6H, s).
Step 4. 3-[4-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoic acid
[0519] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 3-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate (step 3 of Example 17).
[0520] m.p.: 134° C.
[0521] MS (ESI) m/z: 420 (M+H) + .
[0522] IR (KBr) y: 3319, 2974, 2930, 1736, 1605, 1545, 1497, 1439, 1350, 1302, 1275, 1231, 1153 cm −1 .
[0523] 1 H-NMR (DMSO) δ: 8.55 (1H, t, J=6.1 Hz), 7.83 (1H, dd, J=10.6, 2.6 Hz), 7.48 (1H, dd, J=8.3, 5.8 Hz), 7.03 (1H, ddd, J=9.4, 8.3, 2.6 Hz), 3.18 (2H, t, J=6.1 Hz), 2.91-2.80 (2H, m), 2.45 (2H, s), 2.24-2.12 (2H, m), 1.67-1.56 (2H, m) 1.60-1.45 (1H, m), 1.36 (6H, s), 1.28-1.10 (2H, s), 1.06 (6H, s). A signal due to
[0524] CO 2 H was not observed.
[0525] Anal. Calcd. for C 22 H 30 FN 3 O 4 : C, 62.99; H, 7.21; N, 10.02. Found: C, 62.66; H, 7.27; N, 9.90.
Example 18
[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL) PIPERIDIN-1-YL]-ACETIC ACID
[0526]
Step 1. tert-Butyl[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]acetate
[0527] A solution of 6-fluoro-3,3-dimethyl-2-oxo-N-(piperidin-4-ylmethyl)indoline-1-carboxamide (200 mg, 0.63 mmol, step 2 in Example 17) and triethylamine (114 μL, 0.82 mmol) in tetrahydrofuran (3 mL) was stirred at 0° C., it was slowly added tert-butyl bromoacetate (111 μL, 0.75 mmol). The reaction mixture was stirred at room temperature for 5 h and at 35° C. for 4 h. It was further added triethylamine (17 μL, 0.12 mmol) and tert-butyl bromoacetate (18 μL, 0.12 mmol). The solution was stirred at room temperature overnight. The resulting solution was added sat. sodium bicarbonate. It was extracted with ethyl acetate (10 mL×3). The organic phase was washed with brine, dried over sodium sulfate and concentrated. The residue was chromatographed on a column of aminopropyl-silica gel eluting with ethyl acetate/hexane (1:10 to 1:6) to give 203 mg (74%) of the titled compound.
[0528] MS (ESI) m/z: 434 (M+H) + .
[0529] 1 H-NMR (CDCl 3 ) δ: 8.67 (1H, t, J=6.1 Hz), 8.05 (1H, dd, J=10.4, 2.5 Hz), 7.14 (1H, dd, J=8.3, 5.6 Hz), 6.87 (1H, dt, J=8.7, 2.5 Hz), 3.30 (2H, t, J=6.1 Hz), 3.11 (2H, s), 3.02-2.92 (2H, m), 2.16 (2H, dt, J=11.6, 2.3 Hz), 1.80-1.69 (2H, m), 1.54-1.33 (3H, m), 1.46 (9H, s), 1.42 (6H, s).
Step 2. [4-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]acetic acid
[0530] A mixture of tert-butyl[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]acetate (200 mg, 0.46 mmol, step 1 of Example 18) and trifluoroacetic acid (106 μL, 1.38 mmol) in CH 2 Cl 2 (1 mL) was stirred at room temperature overnight. The resulting solution was neutralized by addition of sodium bicarbonate (116 mg) and it was concentrated. The desired product was dissolved with CH 2 Cl 2 /methanol=8/1 solution and filtrated. The filtrate was concentrated. The residue was chromatographed on preparative TLC eluting with methanol/dichloromethane (1:7) to give 115 mg (66%) as white gum.
[0531] MS (ESI) m/z: 378 (M+H) + .
[0532] IR (KBr) ν: 3315, 2937, 2872, 1732, 1686, 1638, 1543, 1497, 1408, 1304, 1275, 1304, 1205, 1130 cm −1 .
[0533] 1 H-NMR (CDCl 3 ) δ: 8.69 (1H, t, J=5.9 Hz), 7.96 (1H, dd, J=10.3, 2.4 Hz), 7.11 (1H, dd, J=8.5, 5.6 Hz), 6.83 (1H, dt, J=8.5, 2.4 Hz), 3.75-3.54 (3H, br), 3.37-3.23 (2H, br), 2.90-2.64 (2H, br), 2.55-1.53 (6H, br), 1.38 (6H, s). A signal due to CO 2 H was not observed.
[0534] HRMS (ESI) m/z calcd for C 19 H 25 FN 3 O 4 ([M+H] +) 378.1829, found 378.1816.
Example 19
2-[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]-2-METHYLPROPANOIC ACID
[0535]
Step 1. tert-Butyl 2-methyl-2-(4-oxopiperidin-1-yl)propanoate
[0536] The title compound was prepared according to the procedure described in step 3 of Example 1 from tert-butyl 2-methylalaninate.
[0537] 1 H-NMR (CDCl 3 ) δ: 2.95-2.85 (4H, m), 2.48-2.40 (4H, m), 1.47 (9H, s), 1.35 (6H, s).
Step 2. tert-Butyl 2-(4-cyanopiperidin-1-yl)-2-methylpropanoate
[0538] The title compound was prepared according to the procedure described in step 4 of Example 1 from tert-butyl 2-methyl-2-(4-oxopiperidin-1-yl)propanoate (step 1 of Example 19).
[0539] 1 H-NMR (CDCl 3 ) δ: 2.93-2.76 (2H, m), 2.68-2.45 (3H, m), 2.00-1.75 (4H, m), 1.47 (9H, s), 1.27 (6H, s).
Step 3. tert-Butyl 2-[4-(aminomethyl)piperidin-1-yl]-2-methylpropanoate
[0540] The title compound was prepared according to the procedure described in step 5 of Example 1 from tert-butyl 2-(4-cyanopiperidin-1-yl)-2-methylpropanoate (step 2 of Example 19).
[0541] MS (ESI) m/z: 257 (M+H) + .
[0542] 1 H-NMR (CDCl 3 ) δ: 3.07-2.96 (2H, m), 2.56 (2H, d, J=5.9 Hz), 2.25-2.13 (2H, m), 1.80-1.65 (3H, m), 1.46 (9H, s), 1.27 (6H, s), 1.30-1.10 (2H, m). Signal due to N H 2 were not observed.
Step 4. tert-Butyl 2-[4-({[6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2-methylpropanoate
[0543] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 of Example 15) and tert-butyl 2-[4-(aminomethyl)piperidin-1-yl]-2-methylpropanoate (step 3 of Example 19).
[0544] MS (ESI) m/z: 462 (M+H) + .
[0545] 1 H-NMR (CDCl 3 ) δ: 8.65 (1H, br s), 8.05 (1H, dd, J=10.5, 2.5 Hz), 7.14 (1H, dd, J=8.3, 5.5 Hz), 6.88 (1H, dt, J=8.6, 2.5 Hz), 3.28 (2H, t, J=6.2 Hz), 3.10-2.98 (2H, m), 2.28-2.13 (2H, m), 1.83-1.64 (3H, m), 1.46 (9H, s), 1.42 (6H, s), 1.45-1.25 (2 H, m), 1.27 (6H, s).
Step 5. 2-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2-methylpropanoic acid
[0546] The title compound was prepared according to the procedure described in step 4 of Example 2 from tert-butyl 2-[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2-methylpropanoate (step 4 of Example 19).
[0547] m.p.: 213° C.
[0548] IR (KBr) ν: 3271, 2934, 1736, 1632, 1560, 1495, 1441, 1346, 1302, 1231, 1151 cm −1 .
[0549] MS (ESI) m/z: 406 (M+H) + .
[0550] 1 H-NMR (DMSO) δ: 8.59 (1H, t, J=6.0 Hz), 7.83 (1H, dd, J=10.7, 2.5 Hz), 7.47 (1H, dd, J=8.3, 5.8 Hz), 7.04 (1H, ddd, J=9.4, 8.3, 2.5 Hz), 3.23-3.53 (4H, m), 2.70-2.56 (2H, m), 1.85-1.65 (3H, m), 1.63-1.40 (2H, m), 1.55-1.42 (1H, m), 1.37 (6H, s), 1.23 (6H, s). A signal due to CO 2 H was not observed.
[0551] Anal. Calcd. for C 21 H 28 FN 3 O 4 .0.2H 2 O: C, 61.66; H, 7.00; N, 10.27. Found: C, 61.26; H, 6.90; N, 10.14.
Example 20
3-[4-FLUORO-4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]-2,2-DIMETHYLPROPANOIC ACID
[0552]
Step 1. N-benzoyl-4-tert-butoxycarbonylaminomethyl-4-fluoropiperidine
[0553] A mixture of N-benzoyl-4-aminomethyl-4-fluoropiperidine ( J. Med. Chem. 1999, 42, 1648-1660.) (3.54 g, 15.0 mmol) and di-tert-butyl dicarbonate (4.91 g, 22.5 mmol) in methanol (80 mL) was stirred at room temperature for 15 h and concentrated in vacuo. The resulting residue was chromatographed on a column of silica gel eluting with hexane/ethyl acetate (1:1) to give 4.52 g (89%) of the title compound as colorless oil.
[0554] MS (ESI) m/z: 337 (M+H) + .
[0555] 1 H NMR (CDCl 3 ) δ 7.55-7.25 (5H, m), 5.16 (1H, br t, J=6.3 Hz), 4.51 (1H, m), 3.62 (1H, m), 3.55-3.00 (4H, m), 2.10-1.25 (4H, m), 1.43 (9H, s).
Step 2. 4-tert-Butoxycarbonylaminomethyl-4-fluoropiperidine
[0556] A mixture of N-benzoyl-4-tert-butoxycarbonylaminomethyl-4-fluoro piperidine (step 3 of Example 15) (4.42 g, 13.1 mmol), NaOH (2.62 g, 65.5 mmol), H 2 O (9.00 mL) and ethanol (90.0 mL) was refluxed for 15 h and concentrated in vacuo. To the resulting residue were added water and chloroform. The organic layer was separated, dried over magnesium sulfate, and concentrated under reduced pressure. Recrystallization of the resulting solid with hexane-CH 2 Cl 2 afforded colorless solid 1.77 g (58%) as the title compound.
[0557] MS (ESI) m/z: 233 (M+H) + .
[0558] 1 H NMR (CDCl 3 ) δ 4.93 (1H, m), 3.30 (2H, dd, J=21.5, 6.3 Hz), 2.91 (4H, m), 1.88-1.34 (4H, m), 1.45 (9H, s). A signal due to N H and was not observed.
Step 3. Methyl 3-(4-{[(tert-butoxycarbonyl)amino]methyl}-4-fluoropiperidin-1-yl)-2,2-dimethyl propanoate
[0559] The title compound was prepared according to the procedure described in step 3 of Example 2 from 4-tert-Butoxycarbonylaminomethyl-4-fluoropiperidine (step 2 of Example 20).
[0560] 1 H-NMR (CDCl 3 ) δ: 4.78 (1H, br s), 3.66 (3H, s), 3.27 (2H, dd, J=22.1, 6.3 Hz), 2.50 (2H, s), 2.64-2.35 (4H, m), 1.77-1.50 (4H, m), 1.44 (9H, s), 1.15 (6H, s). A signal due to N H was not observed.
Step 4. Methyl 3-[4-(aminomethyl)-4-fluoropiperidin-1-yl]-2,2-dimethylpropanoate
[0561] The title compound was prepared according to the procedure described in step 2 of Example 2 from methyl 3-(4-{[(tert-butoxycarbonyl)amino]methyl}-4-fluoro piperidin-1-yl)-2,2-dimethylpropanoate (step 3 of Example 20).
[0562] MS (ESI) m/z: 247 (M+H) + .
[0563] 1 H-NMR (CDCl 3 ) δ: 3.66 (3H, s), 2.74 (2H, d, J=20.4 Hz), 2.65-2.41 (4H, m), 2.51 (2H, s), 1.87-1.20 (4H, m), 1.16 (6H, s). A signal due to N H 2 was not observed.
Step 5. Methyl 3-[4-fluoro-4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)-carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate
[0564] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 Example 15) and methyl 3-[4-(aminomethyl)-4-fluoropiperidin-1-yl]-2,2-dimethyl propanoate (step 4 of Example 20).
[0565] MS (ESI) m/z: 452 (M+H) + .
[0566] 1 H-NMR (CDCl 3 ) δ: 8.81 (1H, t, J=5.3 Hz), 8.03 (1H, dd, J=10.6, 2.5 Hz), 7.15 (1H, dd, J=8.4, 5.6 Hz), 6.88 (1H, dt, J=8.4, 2.5 Hz), 3.66 (3H, s), 3.56 (2H, dd, J=21.1, 5.9 Hz), 2.68-2.45 (4H, m), 2.51 (2H, s), 1.89-1.58 (4H, m), 1.43 (6H, s) 1.15 (6H, s).
Step 6. 3-[4-Fluoro-4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoic acid
[0567] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 3-[4-fluoro-4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]-2,2-dimethylpropanoate (step 5 of Example 20).
[0568] m.p.: 176° C.
[0569] IR (KBr) ν: 3319, 2974, 2937, 1734, 1607, 1543, 1497, 1352, 1304, 1273, 1232, 1153, 1092 cm −1 .
[0570] MS (ESI) m/z: 438 (M+H) + .
[0571] 1 H-NMR (CDCl 3 ) δ: 8.87 (1H, t, J=6.3 Hz), 8.02 (1H, dd, J=10.2, 2.5 Hz), 7.16 (1H, dd, J=8.4, 5.6 Hz), 6.90 (1H, dt, J=8.4, 2.5 Hz), 3.63 (2H, dd, J=20.7, 6.3 Hz), 3.04-2.94 (2H, m), 2.86-2.72 (2H, m), 2.59 (2H, s), 2.05-1.74 (4H, m), 1.44 (6H, s), 1.24 (6H, s). A signal due to CO 2 H was not observed.
[0572] Anal. Calcd. for C 22 H 29 F 2 N 3 O 4 .0.1H 2 O: C, 60.15; H, 6.70; N, 9.57. Found: C, 59.95; H, 6.67; N, 9.37.
Example 21
3-[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)-4-FLUOROPIPERIDIN-1-YL]-2,2-DIMETHYLPROPANOIC ACID
[0573]
Step 1. Methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-fluoropiperidin-1-yl]-2,2-dimethylpropanoate
[0574] The title compound was prepared according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and methyl 3-[4-(aminomethyl)-4-fluoropiperidin-1-yl]-2,2-dimethylpropanoate (step 4 of Example 20).
[0575] MS (ESI) m/z: 434 (M+H) + .
[0576] 1 H-NMR (CDCl 3 ) δ: 8.88 (1H, t, J=5.9 Hz), 8.24 (1H, d, J=7.9 Hz), 7.34-7.14 (3H, m), 3.66 (3H, s), 3.57 (2H, dd, J=21.1, 5.9 Hz), 2.67-2.45 (4H, m), 2.51 (2H, s), 1.90-1.53 (4H, m), 1.44 (6H, s) 1.15 (6H, s).
Step 2. 3-[4-(}[(3,3-Dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-fluoropiperidin-1-yl]-2,2-dimethylpropanoic acid
[0577] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 3-[4-({[(3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-fluoropiperidin-1-yl]-2,2-dimethylpropanoate (step 1 of Example 21).
[0578] m.p.: 156° C.
[0579] IR (KBr) ν: 3306, 2972, 1736, 1543, 1460, 1344, 1271, 1229, 1159, 770 cm −1 .
[0580] MS (ESI) m/z: 420 (M+H) + .
[0581] 1 H-NMR (CDCl 3 ) δ: 8.94 (1H, t, J=4.9 Hz), 8.23 (1H, d, J=8.6 Hz), 7.36-7.15 (3H, m), 3.64 (2H, dd, J=21.1, 5.9 Hz), 3.04-2.92 (2H, m), 2.86-2.69 (2H, m), 2.59 (2H, s), 2.15-1.65 (4H, m), 1.45 (6H, s), 1.24 (6H, s). A signal due to CO 21 H was not observed.
[0582] Anal. Calcd. for C 22 H 30 FN 3 O 4 .0.1H 2 O: C, 62.72; H, 7.23; N, 9.97. Found: C, 62.32; H, 7.22; N, 9.74.
Example 22
1-{[4-({[(6-FLUORO-3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)-4-HYDROXYPIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID
[0583]
Step 1. tert-Butyl 4-cyano-4-hydroxypiperidine-1-carboxylate
[0584] To a suspension of tert-butyl 4-oxopiperidine-1-carboxylate (2.0 g, 10 mmol) in diethyl ether (40 mL), a solution of NaCN (0.54 g, 11 mmol) and NaHCO 3 (1.7 g, 20 mmol) in water (25 mL) was added slowly with vigorous stirring at room temperature. The mixture was stirred overnight, and extracted with Et 2 O (30 mL×2). The organic phase was washed with water (50 mL), brine (50 mL) and dried over MgSO 4 , filtered and evaporated gave 2.1 g of the title compound as clear colorless oil.
[0585] 1 H-NMR (CDCl 3 ) δ: 3.81-3.72 (2H, m), 3.42-3.32 (2H, m), 2.18-2.00 (2H, m), 1.88-1.77 (2H, m), 1.46 (9 H, s).
[0586] 13 C-NMR (CDCl 3 ) δ: 154.67, 121.13, 80.57, 67.15, 36.57, 28.23.
Step 2. tert-Butyl 4-(aminomethyl)-4-hydroxypiperidine-1-carboxylate
[0587] To a suspension of lithium aluminium hydride (84 mg, 2.2 mmol) in THF (5 mL), a solution of tert-butyl 4-cyano-4-hydroxypiperidine-1-carboxylate (200 mg, 0.88 mmol, step 1 of Example 22) in THF (1 mL) was added dropwise at 0° C. The mixture was stirred for 1 h at that temperature and Na 2 SO 4 .10H 2 O (400 mg) was added slowly, and the mixture was stirred for 5 h at room temperature. The mixture was filtered though a pad of Celite, washed with CH 2 Cl 2 (20 mL×2), the filtrate was concentrated to give clear colorless oil. The residue was chromatographed on a column of silica gel eluting with CH 2 Cl 2 /MeOH/NH 4 OH (14:1:0.1) to give 120 mg (59%) of the title compound as white solid.
[0588] 1 H-NMR (CDCl 3 ) δ: 3.98-3.75 (2H, m), 3.17 (2H, t, J=10.8 Hz), 2.56 (2H, s), 1.46 (9H, s), 1.60-1.25 (4H, m). Signals due to O H and N H 2 were not observed.
Step 3. tert-Butyl 4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidine-1-carboxylate
[0589] The title compound was prepared according to the procedure described in step 6 of Example 1 from 6-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (step 2 Example 15) and tert-butyl 4-(aminomethyl)-4-hydroxypiperidine-1-carboxylate (step 2 of Example 22).
[0590] MS (ESI) m/z: 336 (M+H) + .−BOC
[0591] 1 H-NMR (CDCl 3 ) δ: 8.91 (1H, t, J=6.1 Hz), 8.01 (1H, dd, J=10.2, 2.5 Hz), 7.16 (1H, dd, J=8.4, 5.6 Hz), 6.90 (1H, dt, J=8.4, 2.5 Hz), 3.95-3.74 (2H, m), 3.44 (2H, d, J=6.1 Hz), 3.28-3.12 (2H, m), 1.71-1.45 (4H, m), 1.46 (9H, s), 1.43 (6H, s). A signal due to OH was not observed.
Step 4. 6-Fluoro-N-[(4-hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide
[0592] The title compound was prepared according to the procedure described in step 2 of Example 2 from tert-butyl 4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidine-1-carboxylate (step 3 of Example 22).
[0593] MS (ESI) m/z: 336 (M+H) + .
[0594] 1 H-NMR (CDCl 3 ) δ: 8.88 (1H, t, J=5.8 Hz), 8.02 (1H, dd, J=10.5, 2.3 Hz), 7.15 (1H, dd, J=8.4, 5.6 Hz), 6.89 (1H, dt, J=8.4, 2.3 Hz), 3.45 (2H, d, J=5.8 Hz), 3.04-2.82 (4H, m), 1.69-1.57 (4H, m) 1.43 (6H, s). A signal due to O H was not observed.
Step 5. Methyl 1-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidin-1-yl]methyl}cyclobutanecarboxylate
[0595] The title compound was prepared according to the procedure described in step 3 of Example 2 from 6-fluoro-N-[(4-hydroxypiperidin-4-yl)methyl]-3,3-dimethyl-2-oxoindoline-1-carboxamide and methyl 1-formylcyclobutanecarboxylate (step 4 of Example 22) and methyl 1-formylcyclobutanecarboxylate (Davis, Charles R. et al., J. Org. Chem., 1993, 58, 6843).
[0596] MS (ESI) m/z: 462 (M+H) + .
[0597] 1 H-NMR (CDCl 3 ) δ: 8.85 (1H, t, J=5.8 Hz), 8.02 (1H, dd, J=10.4, 2.6 Hz), 7.14 (1H, dd, J=8.6, 5.3 Hz), 6.88 (1H, dt, J=8.6, 2.6 Hz), 3.70 (3H, s), 3.40 (2H, d, J=5.8 Hz), 2.73 (2H, s), 2.61-2.30 (6H, m), 2.10-1.78 (6H, m), 1.65-1.56 (2H, m) 1.42 (6H, s). A signal due to O H was not observed.
Step 6. 1-{[4-({[(6-Fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxy piperidin-1-yl]methyl}cyclobutanecarboxylic acid
[0598] The title compound was prepared according to the procedure described in step 4 of Example 2 from methyl 1-{[4-({[(6-fluoro-3,3-dimethyl-2-oxo-2,3-dihydro-1H-indol-1-yl)carbonyl]amino}methyl)-4-hydroxypiperidin-1-yl]methyl}cyclobutanecarboxylate (step 5 of Example 22).
[0599] m.p.: 159° C.
[0600] IR (KBr) ν: 3300, 2939, 1738, 1535, 1495, 1481, 1350, 1302, 1231, 1155 cm −1 .
[0601] MS (ESI) m/z: 448 (M+H) + .
[0602] 1 H-NMR (CDCl 3 ) δ: 8.94 (1H, t, J=5.9 Hz), 7.99 (1H, dd, J=10.2, 2.3 Hz), 7.16 (1H, dd, J=8.5, 5.6 Hz), 6.90 (1H, dt, J=8.5, 2.3 Hz), 3.46 (2H, d, J=5.9 Hz), 2.95-2.74 (4H, br), 2.84 (2H, s), 2.61-2.48 (2H, m), 2.41-2.24 (1H, m), 2.04-1.86 (3H, m), 1.83-1.66 (4H, m), 1.43 (6H, s). Signals due to O H and CO 2 H were not observed.
[0603] Anal. Calcd. for C 23 H 30 FN 3 O 5 .1H 2 O: C, 59.34; H, 6.93; N, 9.03. Found: C, 59.02; H, 6.57; N, 8.95.
Example 23
1-{[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID HYDROGEN CHLORIDE SALT
[0604] 1-{[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1h-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid (41.0 g, 99.2 mmol, Example 9) was dissolved with tetrahydrofuran (820 mL). The mixture was filtered and washed with tetrahydrofuran (410 mL) and the resulting solution was heated to 45° C. Aqueous concentrated hydrogen chloride (12N, 8.27 mL, 99.2 mmol) was added to the solution at 45° C. for 20 min and stirred at this temperature for 1 h. The suspension was cooled to 20° C. for 1 min, and stirred at 2 h. After filtration, the resulting solid was washed with tetrahydrofuran (205 mL), and dried in vacuo at 40° C. The titled compound was obtained as white solid (38.6 g, 86.6%) PXRD (2θ(+/−0.1): 9.2, 11.0, 16.5, 22.0)
Example 24
1-{[4-({[(3,3-DIMETHYL-2-OXO-2,3-DIHYDRO-1H-INDOL-1-YL)CARBONYL]AMINO}METHYL)PIPERIDIN-1-YL]METHYL}CYCLOBUTANECARBOXYLIC ACID HEMIFUMARATE SALT
[0605] 1-{[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1h-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid (2.09 g, 5.04 mmol, Example 9) was dissolved with THF (25 mL) at 60° C. Fumaric acid (293 mg, 2.52 mmol) was added to the solution. The mixture was concentrated until 12.5 mL. It was cooled to room temperature, and stirred for 1 h. After filtration, the obtained solid was washed with THF (3 mL), and dried in vacuo. The desired compound was obtained as a white solid (2.02 g, 85%).
[0606] 1 H NMR (DMSO, δ) 8.59 (t, 1H, J=5.9 Hz), 8.04 (d, 1H, J=8.1 Hz), 7.44 (dd, 1H, J=1.5, 7.3 Hz), 7.30 (ddd, 1H, J=1.5, 8.1, 8.1 Hz), 7.19 (dd, 1H=8.1, 7.3 Hz), 6.62 (s, 1H), 3.19 (t, 2H, J=5.9 Hz), 2.89 (br-d, 2H, J=11.8 Hz), 2.75 (s, 2H), 2.35-2.20 (m, 2H), 2.20 (br-t, 2H, J=11.8 Hz), 2.00-1.75 (m, 4H), 1.75-1.50 (m, 3H), 1.37 (s, 6H), 1.30-1.10 (m, 2H).
[0607] mp 181° C.
[0608] PXRD (2θ(+/−0.1): 5.7, 10.8, 11.4, 12.4, 16.6)
Preparation:
3,3-DIMETHYL-1,3-DIHYDRO-2H-INDOL-2-ONE
Step 1. 1-bromo-1-methyl-propananilide
[0609] Under nitrogen atmosphere, a solution of 2-bromoisobutyryl bromide (150 g, 652 mmol) in ethyl acetate (200 mL) was added to a well-stirring solution of aniline (66.8 g, 717 mmol) and Et 3 N (72.6 g, 717 mmol) in ethyl acetate (400 mL) on ice bath, maintaining reaction temperature under 30° C. The mixture was stirred at room temperature for 2 h. The cold water (600 mL) was added and stirred at room temperature for 20 min. The mixture was separated and the aqueous layer was extracted with ethyl acetate (600 mL). The combined organic layer was washed with 2N HCl (180 mL), water (180 mL) and dried over sodium sulfate. After filtration, the filtrate was concentrated. The desired compound was obtained as a pale yellow solid (153 g, 97%).
[0610] Rf 0.77 (heptane/ethyl acetate=60/40)
[0611] 1 H NMR (CDCl3, δ) 8.46 (br-s, 1H), 7.55 (d, 2H, J=8.1 Hz), 7.36 (dd, 2H, J=7.3, 8.1 Hz), 7.16 (t, 1H, J=7.3 Hz), 2.06 (s, 6H)
Step 2. 3,3-Dimethyl-1,3-dihydro-2h-indol-2-one
[0612] A mixture of AlCl 3 (16.5 g, 75.0 mmol) and 1-bromo-1-methyl-propananilide (10.0 g, 41.3 mmol, Step 1) was heated slowly to about 90° C. The mixture was maintained at 90-120° C. for 30 min. The mixture was cooled at 30-40° C. then toluene (100 mL) was added to the well-stirring mixture. The resulting slurry was added to well-stirring ice water (100 g). The mixture was separated and the aqueous layer was extracted with ethyl acetate (50 mL). The combined organic layer was washed with 1N HCl (30 mL), 10 wt % aqueous sodium carbonate (30 mL), dried over sodium sulfate, and filtered. The filtrate was evaporated affording a yellow solid. (6.94 g). The obtained solid was dissolved with ethyl acetate (14 mL) under reflux. The solution was cooled slowly to room temperature and it was stirred at room temperature for 1 h. Heptane (56 mL) was added slowly to the resulting slurry. The slurry was stirred at 20-30° C. for 1 h and cooled to 0-5° C. After stirring for 1 h, it was filtered off and the obtained solid was washed with a small amount of ethyl acetate/heptane (1/4). The desired compound was obtained as a white solid (5.4 g, 81%).
[0613] Product: Rf 0.37 (heptane/ethyl acetate=60/40)
[0614] 1 H NMR (CDCl3, δ) 7.60 (br-s, 1H), 7.23-7.18 (m, 2H), 7.05 (t, 1H, J=7.3 Hz), 6.90 (dd, 1H, J=1.5, 7.3 Hz), 1.40 (s, 6H)
[0615] All publications, including but not limited to, issued patents, patent applications, and journal articles, cited in this application are each herein incorporated by reference in their entirety.
[0616] Although the invention has been described above with reference to the disclosed embodiments, those skilled in the art will readily appreciate that the specific experiments detailed are only illustrative of the invention. It should be understood that various modifications can be made without departing from the spirit of the invention. Accordingly, the invention is limited only by the following claims.
|
This invention relates to compounds of the formula (I):
or a pharmaceutically acceptable salt thereof, wherein:
A, R 1 , R 2 , R 3 , R 4 and R 5 are each as described herein or a pharmaceutically acceptable salt, and compositions containing such compounds and the use of such compounds in the treatment of a condition mediated by 5 -HT 4 agonistic activity such as, but not limited to, as gastroesophageal reflux disease, gastrointestinal disease, gastric motility disorder, non-ulcer dyspepsia, functional dyspepsia, irritable bowel syndrome (IBS), constipation, dyspepsia, esophagitis, gastroesophageal disease, nausea, central nervous system disease, Alzheimer's disease, cognitive disorder, emesis, migraine, neurological disease, pain, cardiovascular disorders, cardiac failure, heart arrhythmia, diabetes or apnea syndrome.
| 2
|
FIELD OF THE INVENTION
[0001] This invention relates to an impeller shroud, for a propeller, the shroud allows some water to flow over the propeller. The shroud is mounted on a draft tube, which allows both a propeller shaft to rotate the propeller and air to enter the shroud. The arrangement aerates water, especially contaminated water, and speeds aerobic digestion or decomposition of the contaminants. It is believed that this is achieved by micro sized air bubbles generated by the impeller, which maximizes absorption of air into the water. The shroud has apertures allowing water to be drawn into the shroud, where the propeller is believed to cavitate the water creating a strong vacuum which draws air down the draft tube into the propeller which mixes the air and water uniformly. The propeller then propels the air water mixture into the surrounding water causing a gentle mixing action. The propeller shaft is attached by a bearing box to a motor. Preferably the device is mounted on a frame attached to a float or floats. In use it aerates water, such as but not limited to hog barn effluent and other lagoons for industrial effluents. Application of such aerators greatly reduces the smell and effluents present, to such an extent that complaints about smell vanish, the water in the lagoons is odorless and usable for industrial applications. It is conjectured that this is due to the aerator supplying air and oxygen to satisfy biological oxygen demand and prevent or reduce anaerobic digestion and decomposition. An aerator incorporating shroud and propeller is environmentally beneficial in that it reduces the effects of pollution and contamination.
PRIOR ART
[0002] Aerators are known. An aerator is known locally to applicant of which only a single example exists without printed publication, which has a shroud with a rear aperture for a shaft to rotate a propeller, parallel to the shaft are two pipes or tubes to support the shroud and two bearings for the shaft. One tube has an end bend connecting through an aperture to the shroud to supply air down the tube, water is supplied through the shaft aperture. Two transverse plates welded to the tubes have the shaft bearings bolted to them. A motor drives the shaft mounted on the longer air supplying tube, which itself is mounted on another pipe pivoted on a frame connecting two pontoons. The motor was coupled to the shaft by a rubber coupling. When tested this aerator was less effective than current invention, probably because the propeller suction was less effective down the side tube, dissolving less air. It also vibrated substantially wearing the bearings so they needed replacement every seven or eight weeks or two months. The device also seized when the temperature fell below −7 or −8° C. There was substantial room for improvement.
[0003] The problem with lagoons used to store pollutants and contaminants is that generally the initial aerobic digestion or decomposition removes the dissolved oxygen from the lagoon water and anaerobic digestion or decomposition begins, the products of anaerobic decomposition often include vapors and gasses of horrible odor. It is known that aeration both stops anaerobic digestion and decomposition and encourages and initiates aerobic digestion and decomposition. Obviously a steady supply of oxygen is required to maintain dissolved oxygen for aerobic digestion or decomposition. Typically it is provided by passing air through the water, where it dissolves. Many such devices have been patented and many are commercially available.
[0004] Applicants had a 2½ million gallon (11 million liter) lagoon which was used for waste water from a truck wash. It produced a horrible odor which was a nuisance and made applicants very unpopular with the local community. Two devices of the present invention were installed and within fourteen days, the smell had vanished and the lagoon water seemed clean, at least for washing, solving applicants' problem, and improving local community relations. Local authorities using a crude quantitative test rated the treated lagoon odor as 1, acceptable, at the edge of the lagoon, roughly 0 is no noticeable smell, 10 is the maximum detectable, hog barn lagoons rate between 7 and 8.
[0005] In a separate instance, a hog barn stage-one lagoon for liquid excrement after removal of solids from 4,000 hogs and 100 dairy cattle, flow estimated at 80,000 gallons every two weeks, was treated with three aerators of the invention. Previously there were intense odors and endless complaints from neighbours. Within seven days of installation of the aerators of the invention, there was very little noticeable odor around the lagoon, within fourteen days the odor was almost completely eliminated. Further there are now no complaints from neighbours. Not only did the odor vanish for practical purposes, but the sludge build up around the outside edge of the lagoon had disappeared and the liquid of the lagoon itself was much cleaner. Previously two other types of aerators were tried by comparison only the aerators of the invention were effective. One ½ horsepower aerator tested had no effect. The other aerator, which had the same horsepower, 5, as applicants' aerator, did far less than applicants' aerator, and used three times as much electricity.
BRIEF SUMMARY OF THE INVENTION
[0006] In view of the observed deficiencies of commercially available prior art aeration devices, the present invention provides a new impeller shroud for aeration devices for industrial waste water lagoons. The shroud has a front aperture for outward aerated water flow and rear apertures for inward water access. It is also connected to a draft tube which has an aperture for inward air access. When assembled a propeller rotates in the shroud, driven by a propeller shaft passing through the draft tube. The propeller sucks water in through the rear apertures, which cavitates in the shroud and sucks air down the draft tube to produce microbubbles of air which dissolve in the water. The absence of a shaft or propeller bearing in the shroud is significant because otherwise the suction effect of the propeller would be eliminated or at least greatly reduced. The aerated water then mixes smoothly with the water in the lagoon. The shroud draft tube has an aperture for air access, and a motor connected through a bearing box to the propeller shaft. Preferably the draft tube-motor assembly is mounted on a frame so that the propeller impeller is submerged in the water, while the draft tube aperture, bearing box and motor are in the air. Preferably the device is mounted on a frame, which may be pivotable from a horizontal position above water, to an angled position with propeller and shroud submerged. The frame may be mounted on a raft, which may include floats. Generally the motor is electric, although it is not so limited, and may be connected by an electric cable to a power supply. The cable may extend to the raft, which is typically moored in a lagoon, although not so limited.
[0007] There has thus been outlined, rather broadly, the more important features of the invention in order that the description thereof may be better understood, and in order that the present contribution to the art may be better appreciated. There are additional features of the invention that will be described hereinafter and that will form the subject matter of the claims appended thereto.
[0008] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangement of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practised and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of the description and should not be regarded as limiting.
[0009] It is a principal object of the invention to provide a shroud for a propeller that overcomes the shortcomings of prior art aerators. It is a principal object of the invention to provide a shroud with a front aperture for outward aerated water flow and rear apertures for inward water access. It also a principal object to provide a shroud with a rear draft tube allowing inward air access. It is a further principal object of the invention that the draft tube provides access for a propeller shaft to rotate a propeller within the shroud. It is a further principal object to provide that rotation of the propeller within the shroud, sucks water through the rear shroud aperture and sucks air down the draft tube and expels aerated water from the forward aperture of the shroud. It is a subsidiary object that the propeller cavitates the water in the shroud and sucks air down the draft tube into the cavitating water to produce microbubbles of air which dissolve in the water. It is a further principal object of the invention to provide no propeller bearing or shaft bearing in the shroud and draft tube, to affect, reduce or eliminate the suction effect of the propeller in the shroud. It is a further principal object of the invention to provide aerated water which mixes smoothly with the water surrounding the shroud. It is a further object of the invention to provided an air access aperture in the draft tube. It is a further subsidiary object of the invention to provide a motor to drive said propeller shaft. It is also a further subsidiary object of the invention to provide a bearing box to connect the motor to the propeller shaft. It is a subsidiary object to provide a frame to mount the draft tube-motor assembly is mounted on a frame so that the propeller impeller is submerged in the water, while the draft tube aperture, bearing box and motor are in the air. It is a further subsidiary object of the invention that the frame is pivotable from a horizontal position with propeller, shroud, shaft, draft tube, bearing box and motor above water, to an angled position with propeller and shroud submerged. It is a further subsidiary object of the invention to provide the frame mounted on a raft. It is a further subsidiary object of the invention to provide an electric motor for driving the bearing box. It is a further subsidiary object to provided a raft mounting the frame, propeller, shroud, shaft, draft tube, bearing box and motor, moored in a lagoon. Other objects and advantages of the present invention will become obvious to those skilled in the art, from the following specification, accompanying drawings and appended claims, and it is intended that these objects and advantages are within the scope of the present invention.
[0010] To accomplish the above and related objects, this invention may be embodied in the form illustrated in the accompanying drawings, attention being called to the fact, however, that the drawings are illustrative only, not limiting, and that changes may be made in the specific construction illustrated and described within the scope of the appended claims.
[0011] In one broad aspect the invention is directed to a draft tube for an impeller extending from a front end for connection to a shroud to accommodate a freely rotating propeller, to a rear end to accommodate a shaft to drive the propeller, and to pass air around the shaft. The tube is straight and has sufficient cross sectional area to permit the shaft and air to pass freely from the rear end to the front end. Generally the draft tube has a side aperture for air ingress toward its rear end. Preferably the draft tube has a rear attachment plate at right angles to the said draft tube. More preferably the side aperture has a stub tube protruding therefrom.
[0012] In an alternate broad aspect the invention is directed to a shroud for impeller to accommodate a freely rotating propeller. The shroud has a first aperture of sufficient size to receive a shaft to drive said propeller and to pass air into the shroud around the shaft, and at least one second aperture to pass water into the shroud. The shroud preferably has a front portion for a freely rotating propeller and a rear portion comprising the first aperture axially aligned with the position of the propeller, and the at least one second aperture is rearward of the propeller position. Usually the front portion is cylindrical and the rear portion is a disc which has the first aperture centrally therein. The disc usually has the at least one second aperture therein spaced radially apart from the first aperture. Often there are several second apertures. Conveniently the front portion is joined to the rear portion by a frustroconical mid portion.
[0013] In a second broad aspect the invention is directed to a shroud for impeller comprising a front portion for a freely rotating propeller and a rear portion having a first aperture axially aligned with the position of the propeller. The first aperture us of sufficient size to receive a shaft to drive the propeller and to pass air into the shroud around the shaft, and at least one second aperture in the shroud rearward of the propeller position to pass water into the shroud. A draft tube extends rearward from the rear portion and the first aperture. The draft tube is axially aligned with the position of the propeller, and of sufficient size to accommodate the shaft and to pass air into the shroud. Usually the at least one second aperture is rearward of said propeller position. Typically the tube and first aperture have the same i.d. The draft tube usually has a side aperture for air ingress toward its rear end. The draft tube usually has a rear attachment plate at right angles to the draft tube. Typically the draft tube has a stub tube protruding therefrom. The shroud typically has a front cylindrical portion and a rear disc portion, which has the first aperture centrally therein, and also the at least one second aperture therein spaced radially apart from the first aperture. Often there are several second apertures. Conveniently the front portion is joined to the rear portion by a frustroconical mid portion.
[0014] In a further broad aspect the invention is directed to an impeller for aeration comprising in combination front to rear shroud, propeller, propeller shaft, draft tube and motor. The propeller shaft is driven by the motor and passes through the draft tube to drive the propeller in the shroud. The propeller shaft is generally coupled by a socket in the propeller shaft which snugly receives the motor shaft, the motor shaft is usually secured in the socket by set screws. The shroud has a first aperture for the propeller shaft and air ingress into the shroud around the shaft, and at least one second aperture for water ingress into the shroud. The draft tube has a side aperture for air ingress toward its rear. Usually the front portion is cylindrical to accommodate ther propeller and the rear portion is a disc which has the first aperture centrally therein. The disc usually has the at least one second aperture therein spaced radially apart from the first aperture. Often there are several second apertures. Conveniently the front portion is joined to the rear portion by a frustroconical mid portion. The draft tube usually has a rear attachment plate at right angles to the draft tube. Typically the draft tube has a stub tube protruding therefrom. The impeller usually additionally comprising a bearing box between the draft tube and the motor. The bearing box contains a bearing for the shaft, which passes through the bearing box, and the bearing. Suitably the impeller is mounted by its bearing box on a swivel arm pivotally mounted on a frame, which itself is mounted on a floatable substrate, typically a raft. It can also be pivotally or fixedly mounted on a fixed substrate. Usually the front portion of the shroud is cylindrical to accommodate ther propeller and the rear portion is a disc which has the first aperture centrally therein. The disc usually has the at least one second aperture therein spaced radially apart from the first aperture. Often there are several second apertures. Conveniently the front portion is joined to the rear portion by a frustroconical mid portion. The draft tube usually has a rear attachment plate at right angles to the draft tube. Typically the draft tube has a stub tube protruding from the side aperture. The bearing box, when present, is attached at its front to ther draft tube by the attachment plate. The bearing is held within the bearing box by a retainer. The motor is mounted upon a motor mount plate attached to the bearing box at its rear. The impeller can be mounted by its bearing box on a swivel arm pivotally mounted on a frame. The frame itself is preferably mounted on paired parallel pontoons. The impeller is mounted on the frame between and parallel to the pontoons. The impeller is pivotable angularly through a right angle from horizontal to vertical through a plurality of angular positions. The swivel arm has mounted thereon an adjustment arm at right angles to the swivel arm and at right angles to the impeller. The frame has mounted thereon an adjustment plate cooperating with the adjustment arm. The adjustment arm has a single aperture. The adjustment plate has a plurality of apertures corresponding to the angular positions of the impeller, each aperture is registrable with the adjustment arm aperture. The impeller can be secured in angular position by passing a retaining pin through the adjustment arm aperture and one of the adjustment plate apertures.
[0015] Nearly all elements of shroud, shaft, draft tube bearing box, swivel arm and frame are preferably stainless steel, except the propeller which is aluminum.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 shows a longitudinal cross sectional view of a shroud and attached draft tube of an embodiment of the invention.
[0017] FIG. 2 shows a front view of a shroud of the embodiment of FIG. 1 .
[0018] FIG. 3 shows a partial cross sectional view of an assembled impeller of the invention incorporating the embodiment of FIG. 1 .
[0019] FIG. 4 shows a side elevational view of an aerator of the invention incorporating the embodiment of FIG. 3 .
[0020] FIG. 5 shows a top plan of the embodiment of FIG. 4 .
[0021] FIG. 6 shows a front elevational view of the embodiment of FIG. 4 .
[0022] FIG. 7 shows details of angle adjustment of the embodiment of FIG. 4 .
[0023] FIG. 8 shows a side cross sectional view of the shaft coupling of FIG. 4 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] Numeral 10 indicates shroud 12 with attached draft tube 14 of an embodiment of the invention. Shroud 12 has forward cylindrical portion 16 , 10″ diameter, 5″ deep, middle frusto conical portion 18 10″ forward diameter tapering to 7″ rear diameter, also 5″ deep and rear disc portion 20 with water access slots 22 and rear draft tube access aperture 24 . Water access slots 22 are made by drilling eight 1″ diameter apertures equispaced around draft tube access aperture 24 , centered on a circle 5⅛″ diameter, adjacent pairs are then joined to form slots 22 . Draft tube 14 has 3″ o.d., 2¾″ i.d., and is 2′ long excluding or including rear plate 26 , which is 5½″ or 5⅞″ square and ¼″ or ⅜″ thick, which has corner apertures for attachment to a bearing box. Centered 2¼″ or 3″ forward from the rear end of draft tube 24 is threaded pipe ferrule 28 , 1″ diameter and projecting ¾″, for air access. When assembled impeller 29 has shroud 12 , containing propeller 31 with hub 32 and blades or vanes 34 , hub 32 is mounted on threaded spindle 33 of drive shaft 30 . Propeller 31 is a Michigan Machine #012109 9X9 three-bladed propeller of diameter 9 inches. Shaft 30 extends through draft tube 14 into bearing box 36 . Shaft 30 is about 45¾″ long, including spindle 33 , 4″ long, the bulk of the shaft is 1¾″ diameter. Bearing box 36 is 6½″ square in cross section and extends about 1′3″ along shaft 30 , it is of 12 gauge steel plate and has a front or lower end plate 38 for attachment to draft tube attachment plate 26 and a rear or upper end plate 40 for attachment of motor 48 , it also has a side removable access plate, not shown. Shaft 30 is contained in bearing 42 held in place by retainer 44 , note that bearing 42 avoids the necessity of having an end bearing in shroud 12 for shaft 30 , which would virtually eliminate the suction effect of propeller 31 . Shaft 30 narrows slightly in bearing box 36 to 1 45/64″ diameter, at its upper or rear end it engages motor drive shaft 46 , 3″ long, 1⅛″ diameter, secured by set screws 94 in fitted socket 92 , of i.d. 1.127″ ( FIG. 8 ), which is conventional. Motor 48 is attached to circular motor mount plate 50 , 10″ diameter, 3/16″ thick, with circumferential flange projecting 3/16″ and ¼″ thick, forming a recess to receive attachably motor 48 . Plate 50 is itself attached to plate 40 of bearing box 36 . Motor 48 is a Siemens Model F038, electric motor, which is a 5 horsepower, 220 volt motor. A single or three phase electric motor are interchangeably usable in the impeller. Impeller 29 ( FIGS. 4 and 5 ) including shroud 12 , draft tube 14 , bearing box 36 and motor 48 is mounted on swivel arm 54 , a 2″ square, 0.1″ thick metal tube, 1′ long, attached to bearing box 36 by right triangular gusset plates 56 , of side 1½″ and thickness ¼″, a pair at each side of bearing box 36 . On one end of swivel arm 54 is end plate 58 which projects downward to accommodate pivot hole 60 , ¾″ diameter, plate 58 is 2″ across by 3½″ deep by ¼″ thick. On the other end of swivel arm 54 is adjustment arm 74 which extends 1′ 3½″ from top to bottom, is 2″ wide and either ¼″ or ½″ the bottom corresponds to plate 58 , but the rest extends upward as shown. Besides another corresponding pivot hole 60 , diameter ¾″, at the top is adjustment hole 76 , ¾″ diameter, which can correspond with any of eleven adjustment holes 80 , ¾″ diameter, spaced at about 80 apart, in adjustment plate 78 , itself of radius 1′. Swivel arm 54 engages support frame 64 by pivot pins or a pivot axle passing through pivot holes 60 and corresponding pivot hole, ⅝″ diameter, in trapezoidal support bracket 62 , 3″ long, 1½″ tall and ¼″ thick, mounted on longitudinal support bar 66 of support frame 64 , and an equivalent ⅝″ diameter hole in adjustment plate 78 . Transverse support bars 68 and 82 engage pontoon brackets 69 , and are secured to them by threaded bolts and nuts. Frame 64 consists of 2″ square tubing, 0.1″ thick, it has main transverse bar 68 , 3′10″ long, longitudinal bars 66 and 84 , stump transverse bars 82 , and cross support bar 86 (hidden in FIGS. 4 and 5 , but visible in FIG. 6 ). Trapezoidal bracket 62 is mounted on support bar 66 , and adjustment plate 78 is similarly mounted on support bar 84 . Pontoon brackets 69 , 2¼″ square, 0.1″ thick and 4″ long, which receive the ends of support bars 68 and 82 , are secured to pontoon support rings 70 , 4″ wide, ⅛″ thick, which encircle pontoons 72 , which are 7½′ long, 1½′ diameter of plastic, polyethylene preferred. Transverse support bars 68 and 82 project 1′3″ beyond longitudinal bars 66 and 84 , which are spaced 1′ apart. All elements including but not limited to support frame 64 , shroud 12 , draft tube 14 , bearing box 36 , shaft 30 , pontoon support rings 70 , etc., are stainless steel, in view of the corrosive nature of lagoons treated, an exception is propeller 31 which is aluminum. As shown in FIG. 6 , cross support bar 86 extends from support bar 66 to support bar 84 , while swivel arm 64 is parallel and above cross bar 86 . Pivot pins 88 pass through end plate 58 , which is attached to swivel arm 54 , then bracket 62 of support bar 66 , and also through adjustment arm 74 , which is attached to swivel arm 54 , then adjustment plate 78 attached to support bar 84 , thus providing a pivot for impeller 29 . Lock pin 90 passing through adjustment arm 74 by adjustment hole 76 and adjustment plate 78 by one of eleven holes 80 allows impeller 29 to be held at a predetermined angle for transport or use. FIG. 7 shows the angle adjustment in detail, as shown adjustment arm 74 is at an angle of 45° to the vertical, rotated about pivot pin 88 passing through an aperture in the bottom end of adjustment arm 74 and an equivalent aperture in adjustment plate 78 , the top end of adjustment arm 74 is secured by lock pin 90 passing through the 45° angle hole 80 in adjustment plate 78 and equivalent adjustment hole 76 in adjustment arm 74 . Swivel arm 54 is welded to adjustment arm 76 and moves with adjustment arm 76 . Bearing box 36 shown in ghost, is welded directly to swivel arm 54 and indirectly through gusset plates 56 . Thus angling adjustment arm 76 angles bearing box 36 , and hence impeller 29 . Although the floating support is described in detail, those skilled in the art would appreciate that any practical floating support can be used, and impeller 29 can be mounted on a fixed support either in the middle of the body of water, or at its edge, such as but not limited to a bank, shore, jetty and the like. All these given dimensions are intended to be taken as a general guide to those skilled in the art, and it is understood these may be varied as practice dictates or minor improvements indicate.
[0025] In use the shroud bottom is typically between 1′ and 1½′ below water level. The propeller turns at 1750 rpm, the set speed of the motor, which is not adjustable, and as a result there is essentially no water in the draft tube. As a further result the propeller does not seize, because there is no water in the draft tube to freeze, the water in the shroud being in constant motion also does not freeze. The impeller operates reliably down to at least −30° C. or −31° C. without freezing, a significant advantage in much of North America. It aerates through 5 or 6″ of ice, producing a frozen white foam in the hole through the ice. In time this frozen foam covers the entire aerator, including draft tube and motor, resembling an igloo, through which the motor can be heard humming away. It is believed that as air incoming through the draft tube is at −30° C. or −31° C., while the water in the shroud is probably between 0 and 4° C., that the turning of the drive shaft, at about 1750 rpm, in the draft tube prevents freezing and seizing of the impeller. The device was observed to seize at −38° C. In warmer weather, when there is no surface ice, the impeller generates a foam which eventually dissipates covering the entire lagoon with a white foam about ¼″ thick or deep. After prolonged use the lagoon gives positive oxygen readings using an oxygen reading device, no positive oxygen readings were noted when testing the truck wash lagoon before aeration. No competitor's aerator was observed to produce the same amount of foam as of the impeller of the invention, nor was one as effective as instant impeller to applicants' knowledge. Larger 20 or 25 horsepower aerators produced patches of foam around the aerators, but didn't cover the slough. It is believed that the smaller bubbles of instant impeller produce much better aeration than the larger bubbles observed in other aerators. It is also considered that the motor shaft-propeller shaft coupling and the bearing box coupling which greatly reduce vibration and hence bearing wear, avoids the need for a bearing in the impeller shroud, which if present would incommode aeration by the propeller. Such bearings are normally a sleeve mounted by vanes in the shroud, which obviously affects the flow around the propeller. It is also believed that the air flowing down the draft tube is evenly distributed by the propeller in the shroud, and that the absence of bearings in the propeller enhances air flow which is central around the shaft, better distributed and creates better suction. Similarly the water flows evenly into the shroud and mixes better with the air to produce a foam, some of which dissolves into and aerates the water surrounding the shroud.
[0026] As those skilled in the art would realize these preferred described details and materials and components can be subjected to substantial variation, modification, change, alteration, and substitution without affecting or modifying the function of the described embodiments.
[0027] Although embodiments of the invention have been described above, it is not limited thereto, and it will be apparent to persons skilled in the art that numerous modifications and variations form part of the present invention insofar as they do not depart from the spirit, nature and scope of the claimed and described invention.
|
A shroud for an impeller used for aeration of contaminated water, has a front portion for a propeller, behind it is a rear portion with separate apertures for water and air, the air aperture accommodates the propeller shaft. A draft tube connected to the shroud has a stub tube at the rear end for air ingress. The propeller shaft passes through the draft tube, and a bearing box to a motor. The draft tube has a rear attachment plate to which the bearing box is attached. The bearing box has a bearing for the shaft held in place by a retainer, it also is attached at its rear to a motor mounting plate, on which the motor is mounted. The impeller is mounted on a swivel arm mounted pivotally on a frame, typically on a raft. The swivel arm allows the impeller to be positioned angularly and lockably in a plurality of angular positions from horizontal to vertical.
| 1
|
FIELD OF THE INVENTION
This invention relates to improvements in air-fuel ratio control in internal combustion engines.
BACKGROUND OF THE INVENTION
In conventional automotive engine control, the extent that certain well-known engine and emission system performance goals can be achieved is largely determined by the capacity to control the engine air-fuel ratio. In general, many conventional vehicle powertrain controllers PCMs attempt to maintain the engine air-fuel ratio at the well known stoichiometric ratio (λ=1). This ratio is generally found to yield satisfactory engine performance.
Engine control systems that are capable of controlling fuel, air, and recirculated exhaust gas EGR, attempt to maintain the air-fuel ratio at stoichiometry by coordinating control of the quantity of fuel, air, and EGR admitted into the engine, based on predetermined relationships between those control parameters calibrated for the specific engine application, and based on the present engine operating condition.
Such control may not account for manufacturing variations or for disturbances to the control system, for example the inevitable system performance changes due to aging. As such, it is common in the art of engine control to sense the performance of the air-fuel ratio control itself, for example using an oxygen sensor located in the exhaust path of the engine to observe, in a conventional manner, the actual engine air-fuel ratio. The observed (sensed) air-fuel ratio may then be fed back to the engine controller, which may trim (adjust) one of the three control parameters in order to compensate for the variations or disturbances.
In many such systems, fuel is a high resolution control parameter, making it an attractive candidate when precise air-fuel ratio control is desired. However, such systems may be "fuel-lead" systems in that the driver directly sets a fuel command which is directly related to engine torque, and only indirectly sets the air and EGR commands. As such, fuel command adjustments tend to be more perceptible to the driver in these systems. Such perceptibility is generally considered to be a disadvantage, as it disturbs the torque command--particularly in transient maneuvers.
Alternatively, these fuel-lead systems may trim the quantity of air admitted into the engine in engine air-fuel ratio control. Because air, unlike fuel, is not directly controlled by the driver in these systems, air trim is less perceptible to the driver. However, air trim does not provide the resolution available with fuel trim, and air trim can only be used in certain engine operating regions.
Further, these fuel-lead systems may trim the quantity of EGR admitted into the engine for air-fuel ratio control. Like air trim, EGR trim is less likely to be perceived by the driver in many of these systems. Further, when the quantity of EGR and the ratio of fuel to air in the engine rise or fall together, such as when EGR is trimmed for air-fuel ratio control, the desired air-fuel ratio correction may be achieved while limiting the creation of oxides of nitrogen (an undesirable combustion product) in the engine. Still further, the engine spark command is less sensitive to EGR trim than to fuel or air trim. However, EGR is not available or desirable in certain engine operating regions, such as in high engine load regions, or at idle. Further, EGR control does not have the resolution available with fuel control.
In the above-described systems, there are advantages and disadvantages associated with trimming fuel, air or EGR in order to control air-fuel ratio. What is needed is a system control strategy that controls engine air-fuel ratio using all three control parameters in a manner that retains the benefits of each and minimizes their weaknesses.
SUMMARY OF THE INVENTION
The present invention comprises a comprehensive air-fuel ratio control method for an engine controller that is not limited to control of a single engine parameter, but selects and adjusts the parameter best suited to the present engine operating condition.
In general, the method senses the engine operating condition and determines, based on that condition, which control parameter is best suited for air-fuel ratio control in terms of the benefits and detriments it provides at that operating condition.
For example, at low load operating conditions, air has insufficient resolution for air-fuel ratio control. Additionally, EGR is typically not active at such operating conditions, due to concerns over control stability. Accordingly, fuel is the parameter that is trimmed in the closed loop air-fuel ratio control, as it has sufficient resolution for the delicate control in the low load operating region and, as the driver is typically not engaging the accelerator pedal in the low load region, concern that the driver will perceive the fuel trim is minimized.
Engine control systems often abandon stoichiometry at extremely high engine loads, allowing the engine to operate with a slightly "rich" air-fuel mixture. Prior to that "extremely high" engine load range, there is a high load range in which it is desirable to maintain a stoichiometric mixture. In this range, air is at or near its maximum flow capacity, providing little usefulness as a control parameter. Controlling around EGR is possible in such a region, but too much EGR can erode engine torque yield, which is generally considered a disadvantage in higher engine load operating ranges. As such, fuel is trimmed in such regions for stoichiometric control.
Finally, in the operating region between the described low and high load regions, EGR may be trimmed in air-fuel ratio control. Fuel is avoided to minimize driver perception of the control. Air trim also may be used for air-fuel ratio control in the region, but EGR trim is preferred thereover in that it is likely to be even less perceptible than air. However, if EGR trim becomes saturated (runs out of authority), the system may further refine the air-fuel ratio by holding the EGR trim steady, and by trimming either air or fuel.
This method combines the advantages of the three potential control variables to provide air-fuel ratio control over the applicable engine operating range that does not substantially compromise power when it is desired, does not compromise control precision, and minimizes driver perception.
DESCRIPTION OF THE ILLUSTRATIONS
FIG. 1 is a general diagram of an engine control system; and
FIGS. 2, 3a, 3b, 4, 5a, 5b and 5c are computer flow diagrams illustrating the operation of the system of FIG. 1 in accord with the principles of this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, an internal combustion engine 10 is provided fuel by some conventional fuel delivery system, such as by fuel injectors 12 mounted in proximity to each of the cylinders of the engine. The injectors may be controlled in a conventional manner, for example by an injection pulse width generated in the powertrain controller PCM 16, the pulse width being indicative of the amount of time an injector should be injecting fuel into the engine 10.
In the preferred embodiment, the quantity of fuel to be administered into the engine is directly related to the driver's request, such as by the driver's positioning of the vehicle accelerator pedal 24. Such systems, often called fuel-lead systems, make the fuel command directly related to the driver's request, and make air and EGR commands only indirectly related to the driver's request.
Air is drawn into the engine through a bore, wherein a throttle valve 14 is located to control the amount of air allowed into the engine according to a command generated by the PCM 16. In this embodiment, the valve consists of a flat blade 14 which rotates with respect to the air inlet according to the angular position of a rotary actuator 18 connected to the blade by a shaft in a conventional manner. The angular position of the actuator is controlled by the PCM 16.
The angular position of the blade 14 is monitored by an angular position sensor 20, such as a conventional rotary potentiometer, mounted in proximity to the blade, for example on the shaft. The position sensor 20 monitors the blade angle and transmits the measurement to the PCM 16. The inventors contemplate that other air control means may be used in the system incorporating this invention, such as engine valve control which meters the air ingested into the engine via PCM controlled valve lift actuators.
An apparatus 24 by which the vehicle operator may apprise the PCM 16 of a desired engine operating point is located in the vehicle passenger compartment. This apparatus may simply be a conventional accelerator pedal 24, with a pedal position sensor associated therewith so as to monitor the pedal position and transmit the measurement to the PCM 16.
The fuel injected into the engine 10 by means of the fuel injectors 12 is combined with air admitted into the engine by the throttle valve 14, and is distributed to the engine cylinders, where it is ignited in a conventional manner, the product of the ignition being expelled as exhaust gas through an exhaust conduit 26.
A closed conduit 28 is attached between the engine exhaust conduit 26 and the intake manifold for transporting a quantity of the exhaust gas back to be recirculated into the engine 10 with the engine intake air, according to the conventional process of exhaust gas recirculation EGR.
A valve 30 is situated in the conduit 28 to meter the quantity of exhaust gas recirculated. The valve 20 can be any conventional valve capable of controlling the flow of a gaseous substance, such as a conventional butterfly valve. The valve is controlled by a rotary actuator 32 which may be connected to the valve 30 by a common drive shaft. The actuator 32 is controlled according to a command generated in the PCM 16. The position of the valve is monitored by a conventional valve position sensor 36, such as a rotary potentiometer, located in proximity to the EGR valve. The measured EGR position is transmitted to the PCM 16.
The ignited air-fuel mixture creates a force which ultimately rotates the crankshaft of the engine in the usual manner. A conventional rotational speed sensor (not shown) is located in proximity to the crankshaft of the engine 10 to sense the rotational speed of the crankshaft. The sensed value is transmitted to the PCM 16 as a measurement of engine speed RPM.
A conventional oxygen sensor 34 is located in proximity to the engine exhaust conduit in such a manner that a substantial portion of the engine exhaust gas flows by the sensor. The sensor generally indicates the oxygen content in the exhaust gas, the indication being transmitted to the PCM 16. The PCM periodically reads and categorizes the indication as describing a "rich" engine operating condition, where the ratio of air to fuel is below the stoichiometric ratio, or a "lean" operating condition where the air to fuel ratio is above the stoichiometric ratio.
In predetermined engine operating regions, the PCM will attempt to maintain the air to fuel ratio close to the stoichiometric ratio. Necessarily, such operation will cause frequent switching of the oxygen sensor indication from a "lean" indication to a "rich" indication. The PCM, in a conventional manner, categorizes the sensor indication as either rich or lean. Once categorized, the air-fuel ratio status is stored in memory for use in accord with the principals of this invention.
The PCM 16 takes the form of a standard digital computer, such as a Motorola MC68HC11 single chip microcomputer. The principles of this invention are implemented in the form of an operating program stored in the computer's memory.
Automotive engine air-fuel ratio control methods attempt to drive the actual air-fuel ratio to a desired value when operating in predetermined operating ranges. Fuel-lead engine control systems, which are systems that directly control fuel as a function of an operator command such as the operator's positioning of the vehicle accelerator pedal, and that control air, EGR and spark corresponding to the fuel command, will adjust (trim) only one of the fuel, air, and EGR commands to correct for deviations from the desired air-fuel ratio. Often, such adjustments are stored in a memory location corresponding to a "cell" pertaining to the operating conditions at which the adjustment was deemed necessary.
The engine operating region in which closed loop air-fuel ratio control is to be carried out may be divided into a predetermined number of such cells. The values in the memory locations corresponding to these cells are initialized (or re-initialized after memory has been cleared) to values corresponding to "no correction". Later, when operating in a certain cell, any air-fuel ratio adjustments made will be recorded in some conventional fashion in the cell. The active cell value will then be used in the ultimate calculation of the desired quantity of the parameter to be admitted into the engine.
It has been shown that certain engine operating regions are better suited to say, fuel trim, while others are be better suited to either air or EGR trim. The present invention takes this information into account in that it does not limit the parameter to be trimmed to any one of the three mentioned parameters, but trims the parameter that provides the most desirable operation depending on the present engine operating point.
In this embodiment, each operating cell may be defined by engine operating conditions, such as by engine speed or engine load or both. A series of operating cells over the engine operating range is provided for in system memory in the form of a memory lookup table. In this embodiment, one lookup table is provided in non-volatile memory to store block learn values for each of the three engine control parameters of air, fuel and EGR. Individual entries in the above-described tables contain closed loop control information for the cell associated therewith.
In accord with the principles of this invention, while closed-loop air-fuel ratio control is active, only one of the three of air, fuel, or EGR will be active for air-fuel ratio control. The active parameter has a closed loop correction factor CLCF which is adjusted in a rapid manner in response to the sensed actual air-fuel ratio and a block learn table, one value within the table being adjusted more slowly than the CLCF, in response to the CLCF. In general, the CLCF value and the value in the block learn table as adjusted are used to drive the actual engine air-fuel ratio toward the stoichiometric air-fuel ratio.
For example, the CLCF value associated with the active parameter is trimmed or adjusted rapidly in accord with a short time constant in response to the rich or lean output of the oxygen sensor 34 and in direction to restore the air-fuel ratio to the stoichiometric ratio. The rapid response is primarily used to provide quick compensation for variations in the air-fuel ratio from stoichiometry. The CLCF value is a multiplier which, when increased in magnitude increases the air-fuel ratio, and when decreased in magnitude decreases the air-fuel ratio. The fuel, air, and EGR commands are multiplied by their CLCF multipliers before the commands are issued to the respective actuators. In this embodiment, a CLCF value of 128 represents no correction to the command, or a unity gain multiplier, with the value being increased or decreased therefrom as necessary. The three CLCF values are stored in volatile memory.
The value associated with the active cell in the block learn table that is operating is trimmed or adjusted more slowly than the CLCF values, but still is adjusted to drive the actual air-fuel ratio toward stoichiometry. There is one block learn value available for each cell in the tables associated with each of fuel, air and EGR. The individual block learn values, instead of being trimmed directly in response to the actual air-fuel ratio as sensed by the oxygen sensor 34, are rather adjusted according to the state of the corresponding CLCF value. However, the effect of trimming the block learn values is the same as the effect of trimming the CLCF values. For example, increasing the block learn value will increase the air-fuel ratio, and decreasing the block learn value will decrease the air-fuel ratio. Further, like the CLCF values, a block learn value of 128 represents unity gain, and the value is increased or decreased therefrom as necessary.
The active block learn value is adjusted in the same direction as the corresponding CLCF value, so as to ultimately drive that CLCF value back toward the unity gain value. For example, if the CLCF value corresponding to the one of fuel, air, and EGR that is active is increased beyond its unity value, the corresponding block learn value is, in time, increased. The effect of the block learn increase is an increased air-fuel ratio which, when sensed by the oxygen sensor 34, will force the corresponding CLCF value back toward the unity gain value.
The adjustment of the block learn value is slow in accord with a long time constant. As such, unnecessary excursions are avoided, such as from CLCF response to transient disturbances in the system, such as sensor noise. Unlike the CLCF values, the block learn values are stored in non-volatile memory to provide a long-term correction to the evolving needs of the system. They are intended to provide a more permanent, more careful adaptation to system changes than the CLCF values. By combining the CLCF values with the block learn values, the system has the capacity to quickly respond to changing system needs (via the CLCF values), while "remembering" any adjustments needed to operate at the desired air-fuel ratio in the longer term (via the block learn values).
Referring to FIG. 2, when power is first applied to the system, such as when a conventional vehicle ignition switch is turned to its "on" position, the PCM initiates the engine control program at step 50 and then proceeds to step 52 where the PCM provides for system initialization. For example, at this step data constants are transferred from read only memory locations to random access memory locations and counters, flags and pointers are initialized. Additionally at this step, a general counting variable is initialized to zero.
The routine then proceeds to step 54 where the above described three closed-loop correction factors CLCFs are initialized. The CLCF values are stored in volatile memory, such that they must be initialized at step 54 whenever memory keep-alive power is dropped. In the preferred embodiment, these values are initialized to 128, which corresponds to a unity gain factor in the closed loop control, as discussed.
The routine then proceeds to step 55, to determine whether there has been a loss of non-volatile memory since the last operation of the PCM, for example by a battery disconnect or by some system power failure. If such a memory loss has occurred, the routine proceeds to step 57, to initialize non-volatile memory to appropriate initial values. Most importantly in the context of the present invention, block learn values stored in the three block learn tables are initialized to 128 (a unity gain value in this embodiment) at this point.
Next, or if there has been no loss of non-volatile memory, the routine moves to step 56 where interrupts used in vehicle control, including engine control in accord with this invention, are enabled. The interrupt pertaining to execution of the routine incorporating the principles of this invention, called the real-time interrupt, is enabled at this step to occur approximately every 6.25 milliseconds. The PCM then proceeds to a background loop at step 60 which is continuously repeated. This loop may include system diagnostic and maintenance routines. In this embodiment, the PCM interrupts the background loop upon occurrence of the real-time interrupt to execute a general real-time interrupt service routine incorporating the principles of this invention.
This general routine is illustrated in FIG. 3, and is entered at step 70. The PCM proceeds to step 72 to execute general engine control functions well known in the art of engine control, especially those functions necessary for execution of the routine incorporating the principles of this invention. For instance, at this step a desired idle air command is generated, and the engine air-fuel ratio AFRAT is calculated.
The routine then proceeds to step 73 to determine engine load EL, and engine speed RPM. These two values are commonly used in engine control as indicative of the engine operating point. EL may be calculated as a function of the operator requested engine operating point, such as from the position of an accelerator pedal in a vehicle, and RPM may be determined in a conventional manner, such as from a sensor located in proximity to an engine output shaft that rotates at a speed proportional to the engine speed.
The routine then advances to step 74, to determine the active cell to be used in the current iteration of this routine for the purpose of trimming one of air, fuel, or EGR in accord with this invention. As discussed, the active cell is related to the engine operating point, which may be ascertained from the above-determined engine load and speed.
The routine then moves to step 75 to ascertain whether the engine operating point has changed to the extent that the present active cell as determined at step 74 differs from the cell that was active in the previous iteration of this routine. If so, the routine proceeds to step 76, where the three CLCF values may be reset to their unity gain values, as any air-fuel ratio correction information that may have been contained in the CLCF values from the previous iteration may not be in accord with the needs of the engine in its current operating state. Accordingly, that potentially obsolete information may, at the option of the system designer, be discarded, and new corrections may take place which are more likely to be in accord with the needs of the engine in its current operating state.
Next, or if the active cell did not change, the routine moves to step 77, to determine a fuel command in a conventional manner, according to the following equation
Fuel Command=(EL*BL.sub.F /128* CL.sub.F /128)/(AFRAT)
where EL is engine load, BL F is the block learn value associated with the active cell in the fuel block learn lookup table, CL F is the fuel closed loop correction factor, and AFRAT is the calculated actual engine air-fuel ratio. As discussed, the value 128 represents unity gain for both the block learn value and the closed loop correction factor. This is illustrated in the above fuel equation, where both of these values are divided by 128.
After computing the fuel command, the routine proceeds to steps 78 and 80, to compute the desired EGR command. First, at step 78, a base EGR command is calculated. The routine for computing the base EGR command may be any conventional EGR computation routine which determines a desirable quantity of exhaust gas to be recirculated into the engine intake to be combined with the engine intake air. After computing the base EGR command, the overall EGR command is calculated at step 80 in a conventional manner.
In the preferred embodiment, the overall EGR command is calculated according to the following equation
EGR Command=BL.sub.E /128*base EGR command*CL.sub.E /128
where BL E is the block learn value associated with the active cell in the EGR block learn lookup table, and CL E is the EGR closed loop correction factor. Both BL E and CL E are divided by 128 for scaling purposes, as in the case of the already discussed fuel command calculation. The calculation at step 80 merely trims the conventional base EGR command according to the previously calculated stored block learn and CLCF values, so as to drive the actual air-fuel ratio toward the desired air-fuel ratio.
Next, at steps 82 and 84, the desired quantity of air to be admitted into the engine is calculated. First, at step 82, a base air command is determined. This term is used as a general purpose calibration factor that may be determined in a conventional engine calibration process, as a desired amount of air to be admitted into the engine at the current engine operating point. In this embodiment, the base air command is determined as a function of the engine operating range as indicated by engine speed and engine load, and further is based on the ratio of the total air charge (including both the quantity of EGR admitted to the engine and the quantity of "fresh" air admitted to the engine) to the fresh air charge.
After determining the base air command, the routine advances to step 84, to determine the air command according to the following equation
Air Command=base air command/((BL.sub.A /128)*(CL.sub.A /128))
where BL A is the block learn value associated with the active cell in the air block learn lookup table, CL A is the air closed loop correction factor, and BL A and CL A are divided by 128 for scaling purposes, as discussed above for the fuel and EGR command calculations.
After computing the air command, the routine proceeds to step 88, to select an air-fuel ratio trim mode in accord with the principles of this invention. The mode select is carried out by the routine illustrated in FIG. 4, and will be discussed shortly.
The routine then proceeds to step 90, to perform any necessary adjustments of the closed loop correction factor CLCF for the active one of fuel, air, and EGR parameters, as selected in the routine illustrated in FIG. 4. The CLCF adjustment step is well known in the art of engine air-fuel ratio control, as discussed. In this embodiment, an adjustment may be made once per real-time interrupt, so as to provide quick response to the evolving needs of the system.
After adjusting the CLCF value, the routine proceeds to steps 92 through 98, to make any necessary adjustments to the block learn value associated with the active cell in the block learn lookup table corresponding to the mode selected in the routine illustrated in FIG. 4. The block learn adjustment, unlike the CLCF adjustment, is not carried out each time the real-time interrupt service routine is executed, but rather is carried out after a predetermined number of real-time interrupts occur. For instance in the preferred embodiment, it is desired that the block learn values be updated approximately every 200 milliseconds, which requires about 32 iterations of the real-time interrupt between successive iterations of the block learn adjustment routine.
Accordingly, at step 92, a general counting value i, which is reset upon system power-up at step 52 of the routine illustrated in FIG. 2, and is incremented upon every execution of the real-time interrupt service routine, is compared to a predetermined value n. If i equals n, the routine proceeds to step 96 to reset i so as to set up the next delay period. The routine then proceeds to step 98 to carry out the block learn routine, which is illustrated in FIG. 6, and will be described shortly.
Returning to step 92, in the preferred embodiment, the value of n is set to 32 so as to provide approximately a 200 millisecond delay period between successive executions of the block learn calculation routine.
After executing the block learn calculation routine at step 98, the routine moves to step 99, to issue, in any conventional manner the above determined commands to their respective actuators so as to administer the desired amount of fuel, EGR and air to the engine. Next, the routine proceeds to step 100, to re-arm the real-time interrupt in preparation for the next iteration of this routine. The routine then moves to step 102, where it returns to the background loop illustrated as step 58 in FIG. 2.
Returning to step 92, if i does not equal n, meaning that 200 milliseconds have not yet passed since the previous iteration of the block learn calculation routine, the routine proceeds to step 94, to increment the counter as an indication that the routine is one step closer to another execution of the block learn calculation routine. The routine then proceeds to step 100 to re-arm the real-time interrupt, and then returns to the background loop of FIG. 2, via step 102, as discussed.
The mode select routine, called from step 88, is illustrated in FIG. 4, and is entered at step 130. This routine generally selects the operating parameter to be adjusted so as to drive the air-fuel ratio toward a desired air-fuel ratio. As previously discussed, the engine air-fuel ratio may be "fine-tuned" by trimming or adjusting the quantity of fuel, air or EGR admitted into the engine, assuming the engine has the capacity to control each of these quantities.
Practical constraints exist in conventional engine control that make it advantageous to trim some engine parameters in certain engine operating ranges, and other parameters in other ranges. Further, certain parameters simply cannot be used in some engine operating ranges. For instance, when the engine of many conventional systems is operating at idle, air cannot be trimmed, as the air valve is near closed, and has poor resolution. Similarly, in high power modes of operation, air typically cannot be trimmed because the air valve is likely to have run out of authority.
It is well known in the art that EGR control has an undesirable effect on idle stability, and as such should not be used at idle. Further, EGR trim is generally avoided in high power modes of operation, as it can attenuate engine power. Still further, EGR trim has limited authority, such that even extreme (minimum or maximum) amounts of EGR trim may not provide sufficient air-fuel ratio compensation.
Fuel trim is generally only used in engine operating ranges where air and EGR trim cannot or should not be used, as fuel trim is typically more perceptible to the driver in any operating range, which is considered to be a disadvantage in engine control.
The routine of FIG. 4, in accord with the principles of this invention, accounts for the above described advantages and disadvantages associated with trimming the three control parameters in engine control by selecting the parameter considered to provide the most benefit at the most recent sensed engine operating conditions. The closed loop correction factor associated with the selected parameter and the block learn value for the cell corresponding to the present engine operating conditions for that selected parameter will then be trimmed as necessary for air-fuel ratio control at steps 90 and 98 of the routine of FIG. 3, as discussed.
Additionally, if EGR trim is determined not to provide sufficient compensation at its extreme values, supplemental compensation may be provided by trimming fuel or air. In this embodiment, air is selected in the routine of FIG. 4 as the parameter by which the additional compensation is provided when EGR trim is found to be inadequate for complete compensation.
Specifically, the routine starts at step 130 of the routine illustrated in FIG. 4, and proceeds to step 132 to determine if the engine is in an idle state. The idle state may be diagnosed using the most recent measurements of engine speed and engine load in a conventional manner. If the engine is in an idle state, the above discussed practical considerations make it most beneficial to use fuel trim to control air-fuel ratio. As such, the routine proceeds to step 134 to enable fuel mode, and to disable the other two modes, which may have been active from a previous iteration of this routine. The routine then proceeds to step 154 where it is directed to return to the calling routine shown as step 88 of the routine illustrated in FIG. 3.
If the engine is determined not to be in an idle mode, the routine proceeds to step 136, to determine whether the engine is operating in a high power mode. The high power mode may be determined by comparing the present engine speed and load to a predetermined speed and load range, the range corresponding to the high power mode range. The high power mode may be any mode where it is considered advantageous to continue closed loop engine air-fuel ratio control using feedback from some air-fuel ratio sensing device, such as a conventional oxygen sensor, but where high power operation is desired.
Typically, conventional engine control allows open loop engine operation in the highest power range, mainly for engine power enhancement. This invention recognizes an engine operating range just below the highest power range, where closed loop control is still desirable, due to its beneficial impact on engine efficiency and engine emissions. However, it is still considered important to provide the highest power possible within certain well recognized limits. As such, and for the above discussed practical considerations, fuel is selected as the parameter to be trimmed, if necessary. Accordingly, if it is determined at step 136 that the vehicle is operating in the high power mode, the routine proceeds to step 134, to select fuel mode. The routine then returns to its calling routine via step 154, as discussed.
If it is determined that the engine is not operating at idle or in the high power mode, the engine is classified as being in an intermediate region of operation wherein it is considered most beneficial to use EGR trim to control the engine air-fuel ratio, to the extent possible.
The advantages of using EGR for this purpose are commonly understood by those with ordinary skill in the art of engine control. For instance, it is common in fuel-lead systems, such as the system in this embodiment, that EGR trim provides the least perceptible compensation to the air-fuel ratio. Further, EGR compensation is known in such systems to be less sensitive to perturbations than either air or fuel, providing smoother compensation. However, it has been determined that, under certain engine operating conditions, EGR may run out of authority, as discussed. In such cases, compensation from another of the three parameters is necessary for adequate air-fuel ratio control.
In accord with the principles of this invention, air trim or fuel trim may be used to further compensate in cases where EGR is saturated high or low. Accordingly, steps 142, 146, 148, and 150 attempt to determine whether EGR is, in fact, saturated. If so, in the preferred embodiment, air trim is effected to provide the further compensation. However, the inventors contemplate that fuel trim may also be used to provide further compensation.
Specifically, the routine proceeds to step 142 to determine if the most recent EGR command is at the minimum possible command, zero EGR. If so, it is maintained at zero for the present iteration of the routine, and the air mode is activated at step 144, such that any further adjustments to the air-fuel ratio for the present iteration will be carried out via air trim. After enabling the air mode, the routine moves to step 154, where it is directed to return to the calling routine illustrated as step 88 of FIG. 3.
If the present EGR command is not at its minimum value, the routine proceeds to step 146, to determine if the EGR command is at the maximum possible command, or 100 per cent EGR. If so, the maximum command is maintained as such for the present iteration, and the air mode is activated at step 144, such that any further adjustments to the air-fuel ratio for the present iteration will be carried out via air trim. The routine then returns to its calling routine via step 154, as discussed.
Beyond checking the EGR command, the routine checks for a system failure that may have resulted in the EGR valve being fully open or fully closed. Such an EGR valve position would be a fault if detected at steps 148 or 150, in that the only way to execute either of these steps is if the EGR command is not at zero or 100 percent at steps 142 or 146. Accordingly, if the EGR valve is detected to be at zero or 100 per cent at steps 148 and 150, it is in disagreement with the commanded EGR position, and a fault is assumed to exist. In such a case, further EGR trim for the present loop is discontinued, and either air trim or fuel trim is substituted therefor. In the preferred embodiment, air trim is used as the substitute parameter, but the inventors envision fuel trim as also being a suitable substitute.
Specifically, the routine proceeds to step 148 to check the EGR position, via the EGR valve position sensor 36. If the EGR sensor substantially indicates zero EGR, the routine proceeds to step 144, to enable air mode and to disable EGR and fuel modes. The routine then advances to step 154, where it is directed to return to the calling routine of FIG. 3, as discussed.
Alternatively, if at step 148, the EGR position is not substantially zero, the routine proceeds to step 150, to determine whether the EGR valve is at a substantially fully open position. If the EGR valve position sensor 36 indicates that the valve is substantially fully open, which would be in disagreement with the result seen at step 146, a fault is assumed, and the routine proceeds to enable air mode and disable both EGR and fuel modes at step 144. The routine then proceeds to step 154, where it is directed to return to the calling routine of FIG. 3, as discussed.
However, if the EGR valve position sensor 36 does not indicate that the valve is substantially fully open, the routine proceeds to step 152, where EGR mode is enabled, and both air and fuel modes are disabled. As illustrated in FIG. 4, EGR is only enabled, i.e. step 152 is only executed, if the EGR valve is in such a position that it has authority to move in both a closing and an opening direction, and if it is not detected to be faulty. After enabling EGR and disabling both air and fuel, the routine proceeds to step 154, where it is directed to return to the calling routine of FIG. 3, as discussed.
FIG. 5 illustrates the routine to trim or adjust the specific block learn value for the selected active cell (corresponding to the most recent sensed engine operating state) in the block learn lookup table corresponding to the mode that is active. Generally, this routine modifies the selected block learn value so as to ultimately drive the associated closed loop correction factor (CLCF) to zero. As described earlier, for each of fuel, air and EGR, the engine operating region is divided into a series of subregions or cells, each cell having both a block learn value and a closed loop correction factor CLCF.
Accordingly, for any engine operating region in which closed loop air-fuel ratio control is desired, one of the three parameters may be trimmed to provide precise air-fuel ratio control in accord with the principles of this invention. FIG. 5 illustrates the routine where the block learn values are adjusted to accommodate for the evolving needs of the system, in an attempt to adapt the control in response to variations in the performance of the various parts of the engine control system.
Specifically, the block learn calculation routine is entered at step 170. The routine proceeds to step 172, to determine if the block learn update is enabled. The update may be enabled if there are no perceived substantial failures in the closed loop air-fuel ratio control system, or if the system is operating in an engine operating range where closed loop control is considered beneficial.
For instance, conventional engine control systems may run "open loop" or without oxygen sensor feedback while the engine is cold or while operating in a very high power range, as indicated by engine load or engine speed. In such cases, the block learn update, as checked at step 172, may be disabled in a conventional manner. Upon detecting such a disablement, the routine of FIG. 5, at step 172, will terminate by proceeding to step 264, where it is directed to return to the calling routine of FIG. 3.
If the block learn is enabled at step 172, the routine proceeds to step 174, to determine whether the fuel mode has been enabled by the most recent iteration of the routine of FIG. 5. If fuel mode is enabled, the routine then proceeds to step 178, to determine whether CL F has been increased beyond its "unity gain" value (which is 128 in this embodiment), indicating that step 90 attempted to increase the magnitude of the fuel command so as to drive the actual air-fuel ratio toward the desired air-fuel ratio. If such an increase has taken place, the routine proceeds to step 180, to set the enrich flag, for example by setting it to a digital one, as an indication that the fuel block learn value corresponding to CLF must itself be increased so as to drive the CLCF value back toward its "unity gain" value, per the discussed role of the block learn value.
Alternatively, if CL F has not been increased to a value beyond its "unity gain" value, the routine proceeds to step 184 to ascertain whether CL F has been decreased below its "unity gain" value, indicating that step 90 attempted to decrease the magnitude of the fuel command so as to drive the actual air-fuel ratio toward the desired air-fuel ratio. If, at step 184, such a decrease is found, the routine proceeds to step 186, to clear the enrich flag, for example by setting it to a digital zero, as an indication that the quantity of fuel delivered to the engine must be decreased in order to drive the corresponding CL F value toward its "unity gain" value.
If CL F has not been decreased below its "unity gain" value, the routine terminates, by proceeding to step 264, where it directed to return to the calling routine illustrated in FIG. 3. Termination of the routine is proper, as no adjustment of the block learn value is assumed to be necessary when the corresponding CLCF value has not been adjusted in either direction.
After setting the enrich flag at step 180, or clearing it at step 186, the routine proceeds to steps 182 through 202 to trim the corresponding fuel block learn value so as to drive CL F back toward its "unity gain" value.
Specifically, at step 182, the routine looks up the specific block learn value BL F for the selected cell in the block learn lookup table corresponding to the mode that is active (fuel mode is active at this point in the routine). The found value BL F will be adjusted during the remaining steps of this iteration of the routine illustrated in FIG. 5.
The routine next proceeds to "trim" BL F , in accord with principles of this invention in steps 188 through 202. First, the routine checks the status of the fuel enrich flag to determine whether BL F must be increased (enrich flag set), which will increase the amount of fuel per unit air into the engine, or whether BL F should be decreased (enrich flag clear) which will decrease the amount of fuel per unit air into the engine.
If the fuel enrich flag is set, the routine proceeds to step 190, to increase BL F by an amount K 2 . Generally, K 2 is an offset or gain, which may be predetermined in a conventional manner, in accord with the desired rate at which the fuel block learn should be adjusted. For instance, in this embodiment, the block learn calculation occurs every 200 milliseconds, such that when fuel mode is active, and when enriching, the fuel block learn will be increased at a rate of K 2 points per 200 milliseconds. K 2 may be stored in read only memory in the powertrain control module 16.
Enrichment gains, such as K 2 , are common in the art of engine air-fuel ratio control to provide the necessary block learn response to the engine's evolving air-fuel ratio compensation needs. In this embodiment, different gains are provided for the enrichment and enleanment of all three control parameters, which allows various responses for fuel, air, and EGR trim, according to the needs and goals of the system.
After adding the offset K 2 to the fuel block learn value, the routine proceeds to steps 192 and 194 to limit the block learn value, if necessary, to a predetermined maximum value. Such limits are used in conventional systems due to a variety of limitations on the capacity of the system to trim the fuel command. For instance, the value may be limited to prevent an memory overflow, such as what may occur if the value was incremented beyond 255. Additionally, the value may be limited to minimize the potential for disruption when the control moves between cells, for example when the control switches from a cell that has been heavily adjusted to one that has undergone very little adjustment. The limits may be predetermined during engine calibration, in a manner common in the art of engine control.
Specifically, if at step 192 it is determined that BL F has been incremented to its upper limit, the routine proceeds to limit BL F to the high limit value at step 194. After limiting BL F , or if no limitation is deemed necessary, the routine proceeds to step 202, to store the trimmed block learn value back in the memory location in the lookup table from which it was referenced above at step 182. After storing the trimmed value, the routine returns to the calling routine of FIG. 3, via step 264.
Returning to step 188, if the enrich flag is clear, indicating that the fuel block learn value must be reduced so as to properly provide air-fuel ratio compensation, the routine proceeds to step 196, Where BL F is decreased by a predetermined amount K 3 . K 3 is a fuel enleanment gain determined in a conventional manner, so as to provide a desirable response to a need to drive CL F back to its reset value, as discussed. K3 should be determined in a manner and for reasons analogous to those used in the calculation of the constant K 2 . K 3 may be stored in read only memory in the powertrain control module 16.
After reducing CL F by the amount K 3 , the routine proceeds to steps 198 and 200 to check BL F against a predetermined lower limit, for the reasons set forth above for providing an upper limit on BL F . Specifically, at step 198, if CL F has been reduced below the lower limit, the routine proceeds to step 200, to limit CL F to the lower limit. Next, or if CL F is not below the lower limit, the routine proceeds to step 202, to store the trimmed BL F in the memory location from which it was originally referenced at the discussed step 182. After storing the trimmed CL F value, the routine proceeds to step 264, where it returns to the calling routine set out as step 98 of FIG. 3.
Returning to step 174 of FIG. 5, if the fuel mode has not been enabled, the routine proceeds to step 204 to determine if air mode is enabled, per the most recent execution of the routine of FIG. 4. If the air mode has been enabled, the routine executes steps 208 through 232, to trim the block learn value for the selected cell in the air block learn lookup table, in the same manner as was described for trimming the fuel block learn value. If air mode is not enabled, the routine proceeds to step 234 to determine of EGR mode is enabled. If the EGR mode is enabled, the executes steps 238 through 262 to to trim the block learn value for the selected cell in the EGR block learn lookup table corresponding to the mode that is active.
Specifically, if at step 204, air mode is enabled, the routine proceeds to step 208 to determine if CL A has been increased beyond its "unity gain" value, which is 128 in this embodiment. As discussed, an increase in CL A indicates that the conventional closed loop correction routine determined, while air mode was enabled, that the air-fuel ratio was too rich, and more air was needed per unit fuel.
If, at step 208, it is determined that CL A has been increased, the routine proceeds to step 210, to set the enrich flag. Alternatively, if it is determined that CL A has not been increased, the routine proceeds to step 212, to determine whether CL A has been decreased below its "unity gain" value, for instance when the CLCF correction routine attempted to enrich the air-fuel ratio while air mode was active. If CL A has been decreased below 128, the routine proceeds to step 212, to clear the enrich flag.
After setting the enrich flag at step 210, or after clearing the enrich flag at step 214, the routine proceeds to step 216, to select the air block learn value BL A for the selected cell in the air block learn lookup table corresponding to the mode that is active. The routine then proceeds to step 218, to determine the status of the enrich flag. If the enrich flag is set, the routine proceeds to step 226, to increase the air block learn value by a predetermined amount K5, which is predetermined as the rate at which it is deemed most desirable to increase the air block learn value.
The routine then proceeds to step 228 to limit BL A to a predetermined upper limit value, in a manner common in the art, for the reasons set forth for limiting the fuel block learn value at step 192. Specifically, at step 228, if BLA has been increased beyond the upper limit value, the routine proceeds to step 230 to limit BL A to the upper limit value.
After limiting BL A , or if no limit is necessary at step 228, the routine advances to step 232, to store the adjusted BL A value in the memory location from which it was referenced at step 216.
Returning to step 218, if the enrich flag has not been set, the routine moves to step 220, to reduce BL A by a predetermined amount, K 4 . As was discussed for the predetermined constants K 2 , K 3 and K 5 , the constant K 4 is predetermined based on the desired rate of reduction of the air block learn value BL A .
After reducing BL A at step 220, the routine proceeds to step 222 to limit BL A to a predetermined lower limit value, if necessary. Specifically, at step 222, if BL A is less than a predetermined lower limit value, the routine proceeds to step 224, to set BL A to that lower limit value.
Whether BL A is limited at step 224 or not, the routine next proceeds to step 232, to store the adjusted BL A value in the cell from which it was referenced at step 216, the adjusted value replacing the value previously stored in the cell. After storing BL A , the routine proceeds to step 264, to return to the calling routine, shown as step 98 of FIG. 3.
Returning to 204, if the air mode is not enabled, the routine proceeds to step 234, to determine if the EGR mode is enabled, as discussed. If the EGR mode is enabled, an adjustment will be made for the EGR block learn value for the active cell in a manner analogous to that described for the adjustment of the block learn value for both fuel and air. If not, the routine returns to the calling routine via step 264, and no block learn adjustment is made for this iteration of the routine.
However if, at step 234, the EGR mode is enabled, the routine proceeds to step 238, to determine if CL E has been increased beyond its "unity gain", which is 128 in this embodiment. If, at step 238, it is determined that CL E has been increased above 128, the routine proceeds to step 244, to set the enrich flag to 1. Alternatively, if at step 238, CL E has not been increased beyond 128, the routine proceeds to step 240, to make a determination as to whether CL E has been decreased below its "unity gain" value. If so, the routine proceeds to step 242, to clear the enrich flag. If, at step 240, it is determined that CL E has not been decreased below 128, the routine proceeds to step 264, where it is directed to return to the calling routine of FIG. 3.
If the enrich flag is set at step 244, or is cleared at step 242, the routine proceeds to step 246, to select the EGR block learn value BL E from the active cell, i.e. the cell associated with the present engine operating condition, as indicated by the most recent sensed engine speed and load.
Next, the routine advances to step 248 to determine the status of the enrich flag. If the enrich flag is set, the routine proceeds to step 256 to increase the EGR block learn value by a predetermined amount K 7 . The value K 7 is predetermined in a manner common in the art of engine air-fuel ratio control according to the desired rate of increase of BL E .
After increasing BL E , the routine proceeds to step 258, to limit BL E according to a predetermined upper limit value. As discussed for both fuel and air trim limiting, the limit value is set as the highest tolerable EGR block learn value, as dictated by system performance goals and constraints. If, at step 258, BL E exceeds the upper limit, the routine proceeds to step 260, to set BL E to the upper limit. Whether BL E is limited to the upper limit or not, the routine then proceeds to step 262, to store the adjusted EGR block learn value in the cell that was selected at step 242, the adjusted value supplanting the value previously stored in the cell. The routine then advances to step 264, where it is directed to return to the calling routine in FIG. 3, as discussed.
Returning to step 248, if the enrich flag is not set, the routine proceeds to step 250, to decrease BL E by an amount K 6 which is predetermined according to a desirable rate of decrease of the EGR block learn value. After decreasing BL E at step 250, the routine proceeds to step 252 to limit BL E to a predetermined lower limit value, if necessary. Specifically, at step 252, if it is determined that BL E has been decreased below the lower limit value, the routine proceeds to step 254, to set BL E to the lower limit value.
Whether BL E has been limited at step 254 or not, the routine proceeds to step 262, to store the updated BL E in the cell selected at step 242, the adjusted value supplanting the previous stored value in the cell. Next, the routine advances to step 264, to return to the calling routine shown as step 98 of FIG. 3, as discussed.
The foregoing description of a preferred embodiment for the purpose of describing the invention is not to be considered as limiting or restricting the invention since many modifications may be made by the exercise of skill in the art without departing from the scope of the invention.
|
An internal combustion engine air-fuel ratio control method and apparatus wherein a most favorable parameter selected from the group consisting of air, fuel, and recirculated exhaust gas is adjusted in response to detected deviation of the air-fuel ratio away from the desired ratio. Supplemental control is provided by means of the remaining parameters in the event that the most favorable parameter runs out of authority.
| 5
|
This is a divisional of U.S. application Ser. No. 251,153 filed Sep. 29, 1988 now U.S. Pat. 4,971,859, which is a divisional of U.S. application Ser. No. 022,467 filed Mar. 6, 1987, now U.S. Pat. 4,806,642 which is a continuation of U.S. application Ser. No. 657,211 filed Oct. 5, 1984 now abandoned, which is a continuation-in-part of U.S. application Ser. No. 547,297 filed Oct. 31, 1983 now abandoned.
SUMMARY OF THE INVENTION
The present invention relates to a compound of the formula ##STR1## wherein R 1 is OH or SH; R 2 is hydrogen, NHR in which R is hydrogen or COR 6 where R 6 is alkyl of 1-4 carbon atoms, aryl or arylalkyl; R 3 is bromine or NHR where R is hydrogen or COR 6 ; X is O or S; R 4 is hydrogen or CH 2 OR 5 in which R 5 is hydrogen, alkyl of 1-8 carbon atoms, aryl arylalkyl, ##STR2## or COR 6 , or a pharmaceutically acceptable acid or base addition salt thereof.
In a second generic aspect, the present invention relates to a compound of the formula 1, wherein R 1 is OH or SH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is alkyl of one to four carbon atoms, aryl or arylalkyl; R 3 is hydrogen; X is O or S; R 4 is alkyl of one to eight carbon atoms, aryl or arylalkyl, and R 5 is hydrogen, or a pharmaceutically acceptable acid or base addition salt thereof.
In a third generic aspect, the present invention relates to a compound of the formula 1, wherein R 1 is OH or SH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is alkyl of one to four carbon atoms, aryl or arylalkyl; R 3 is hydrogen; X is O or S; R 4 is CH 2 OR 7 in which R 7 is alkyl of one to eight carbon atoms, cycloalkyl of five to seven ring members, cycloalkylalkyl, aryl or arylalkyl, and R 5 is hydrogen, or a pharmaceutically acceptable acid or base addition salt thereof.
The present invention includes a method of manufacture, pharmaceutical composition comprising an effective amount of a compound of the formula 1 in all three generic aspects with a pharmaceutically acceptable carrier, as well as a method of treatment of autoimmune diseases such as arthritis, systemic lupus erythematosus, inflammatory bowel diseases, transplantation, juvenile diabetes, myasthenia gravis, multiple sclerosis as well as viral infections and cancer by administering an effective amount of a compound of the formula 1 in all three generic aspects in unit dosage form.
DETAILED DESCRIPTION
The term "alkyl of 1-8 carbon atoms" means a straight or branched hydrocarbon chain up to 8 carbon atoms such as, for example, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tertiary-butyl, or octyl.
The term "cycloalkyl of five to seven ring members" means cyclopentyl, cyclohexyl, or cycloheptyl.
The term "cycloalkylalkyl" means a cyclopentyl, cyclohexyl, or cycloheptyl radical attached to an alkyl chain of up to four carbon atoms, straight or branched, such as for example, cyclohexylmethyl or cyclohexylethyl.
The term "aryl" includes unsubstituted and substituted aromatic ring such as, phenyl or phenyl substituted by halo, e.g., fluoro, chloro, bromo, or alkyl of 1-4 carbon atoms, such as methyl or ethyl, hydroxy, alkoxy of 1-8 carbon atoms, such as methoxy or ethoxy, or trifluoromethyl.
The term "arylalkyl" means an aromatic ring attached to an alkyl chain of up to 4 carbon atoms, such as unsubstituted or substituted phenylethyl or benzyl where the substituents on the aromatic ring may be the same as defined above.
Pharmaceutically acceptable base salts of the phosphate ester, where R 5 is ##STR3## are the alkali metals, ammonium or substituted ammonium salts, such as sodium, potassium, and ammonium salts. The base salts may be prepared by standard methods known in the art.
Pharmaceutically acceptable acid addition salts are those derived from inorganic acids such as hydrochloric, sulfuric and the like, as well as organic acids such as methanesulfonic, toluenesulfonic, tartaric acid, and the like. These salts may also be prepared by standard methods known in the art.
Other pharmaceutically acceptable salts are those derived from inorganic bases such as sodium hydroxide, potassium hydroxide or ammonium hydroxide or organic bases such as arginine, N-methyl glucamine, and the like. These salts may also be prepared by standard methods known in the art.
A preferred embodiment of the present invention in its first generic aspect is a compound of formula 1 wherein R 1 is OH or SH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is alkyl of 1-4 carbon atoms or phenyl; R 3 is bromine or NH 2 ; X is O or S; R 4 is hydrogen or CH 2 OR 5 in which R 5 is hydrogen, alkyl of 1-8 carbon atoms, benzyl or phenyl, or a pharmaceutically acceptable acid addition or base salt.
Another preferred embodiment of the present invention in its first generic aspect is a compound of formula 1 wherein R 1 is OH; R 2 is hydrogen or NH 2 ; R 3 is bromine or NH 2 ; X is O; R 4 is hydrogen or CH 2 OR 5 in which R 5 is hydrogen or a pharmaceutically acceptable acid addition or base salt.
Particular embodiments of the present invention in its first generic aspect include 2,8-diamino-9-[(2-hydroxyethoxy) methyl]-9H-purin-6-ol, 2-[(2,8-diamino-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol, 2,8-diamino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-phenoxyethoxy)methyl]-6H-purin-6-one and 2-[(2-amino-8-bromo-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol. The latter compound is not only useful pharmacologically but is also useful as an intermediate for preparing certain compounds of the present invention.
A preferred embodiment of the present invention in its second generic aspect is a compound of formula 1, wherein R 1 is OH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is alkyl of one to four carbon atoms, phenyl or benzyl; R 3 is hydrogen; X is O; R 4 is alkyl of one to eight carbon atoms, phenyl or benzyl, and R 5 is hydrogen, or a pharmaceutically acceptable acid addition or base salt.
Another preferred embodiment of the present invention in its second generic aspect is a compound of formula 1, wherein R 1 is OH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is methyl; R 3 is hydrogen; X is O; R 4 is alkyl of four to eight carbon atoms, phenyl or benzyl, and R 5 is hydrogen or a pharmaceutically acceptable acid addition or base salt.
Particular embodiments of the present invention in its second generic aspect include 2-amino-1,9-dihydro-9-[[[1-(hydroxymethyl)hexyl]oxy]methyl]-6H-purin-6-one and 2-amino-1,9-dihydro-9[[[1-(hydroxymethyl)nonyl]oxy]methyl-6H--purin-6-one. The above compounds are not only useful pharmacologically but are also useful as intermediates for preparing certain compounds of formula 1 of the present invention in its first generic aspect.
A preferred embodiment of the present invention in its third generic aspect is a compound of formula 1, wherein R 1 is OH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is alkyl of one to four carbon atoms, phenyl or benzyl; R 3 is hydrogen; X is O; R 4 is CH 2 OR 7 in which R 7 is alkyl of one to eight carbon atoms, cycloalkyl of five to seven ring members, cycloalkylalkyl, phenyl or benzyl, and R 5 is hydrogen, or a pharmaceutically acceptable acid addition or base salt.
Another preferred embodiment of the present invention in its third generic aspect is a compound of formula 1, wherein R 1 is OH; R 2 is hydrogen or NHR in which R is hydrogen or COR 6 where R 6 is methyl; R 3 is hydrogen; X is O; R 4 is CH 2 OR 7 in which R 7 is alkyl of two to eight carbon atoms, cyclopentyl, cyclohexyl, cyclopentylmethyl, cyclohexylmethyl, phenyl or benzyl, and R 5 is hydrogen, or a pharmaceutically acceptable acid addition or base salt.
Particular embodiments of the present invention in its third generic aspect include 2-amino-9[[2-(cyclohexylmethoxy)-1-(hydroxymethyl)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one; 2-amino-9-[[2-(hexyloxy)-1-(hydroxymethyl)ethoxy] methy]-1,9-dihydro-6H-purin-6-one; 2-amino-9-[[2-heptyloxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one; 2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(pentyloxy)ethoxy]methyl]-6H-purin-6-one; 2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(oxyloxy) ethoxy]methyl]-6H-purin-6-one, and 2-amino-1,9-dihydro-9-[[1-hydroxymethyl)-b 2-(phenoxy) ethoxylmethyl]-6H-purin-6-one.
The compounds of formula 1 may prepared according to the following scheme: ##STR4##
The compounds of formula 2 above where R 1 =OH, R 2 =NH 2 , X=O, R 4 =H or CH 2 OH may be prepared according to British Patent Specification 1,567,671 or J. C. Martin, et al, in J Med Chem 26, 759 (1983). The remainder of the compounds of formula 2 above used as starting materials and final products are prepared according to the schemes 1 and 2. Treatment of a compound of formula 2 with N-bromosuccinimide in acetic acid, DMF or methanol produces a compound of formula 3 which when treated with hydrazine hydrate gives the hydrazine of formula 4 or directly the 8-amino derivative of formula 5. The reaction of the 8-bromo compound with hydrazine may or may not proceed entirely to the 8-amino compound. Thus when the 8-hydrazine compound is obtained, it may be further reacted with Raney nickel to allow the reduction to go to completion and afford the desired 8-amino compound. Compounds of formula 5 wherein R 1 , R 2 , and R 4 have been defined according to compounds of formula 1 may be further converted by known methods to provide R 5 substituents of formula 1 or, for example, where R 1 is OH, converting said compound to a compound of formula 1 where R 1 is SH by known means.
The compounds of the present invention and of the formulae 1, 2, 3, 4, and 5, shown above, may also be prepared by the following schematic sequences of reaction steps as illustrated in Schemes 1 and 2. The numbers in parentheses toward the end of each reaction scheme correspond to the compounds of the present invention as defined above. A more detailed description of the reaction steps is provided in the Examples.
In the preparation of compounds of the present invention and of the formulae 1 and 5, there are employed novel intermediates which are part of the present invention. These are compounds of the formula ##STR5## wherein Y is acetyloxy or chloro and R 7 is alkyl of one to eight carbon atoms, cycloalkyl of five to seven ring members, cycloalkylalkyl, aryl or arylalkyl. Preferably, R 7 is alkyl of two to eight carbon atoms, cyclopentyl, cyclohexyl, cyclopentylmethyl, cyclohexylmethyl, phenyl or benzyl. ##STR6##
The compounds of the present invention have shown to exhibit significant enzyme inhibition activity and cytotoxic activity. In the purine nucleoside phosphorylase (PNP-4) enzyme assay, total inhibition was achieved at a concentration less than about 300 micromoles on certain compounds. The same compounds also were found by a standard test (Science, 214, 1137, 1981) to be selectively cytotoxic for T-cells in the presence of 2'-deoxyguanosine at a similar concentration range. For example, 2,8- diamino-9-[(2-hydroxyethoxy)methyl)]-9H-purine-6-ol is selectively cytotoxic to T-cell at a concentration of about 30 micromoles in the presence of 10 micromoles of 2'-deoxyguanosine. Similarly, 2-[(2,8-diamino-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol is selectively cytotoxic to T-cell at a concentration of about 7 micromoles in the presence of 10 micromoles of 2'-deoxyguanosine. Both compounds were nontoxic to B-cell in the presence of the same amount of 2'-deoxyguanosine. Since T-cells play a central role in immune response, use of the compounds of the invention is contemplated for the immunoregulation of autoimmune disease such as rheumatoid arthritis, systemic lupus erythematosus, inflammatory bowel disease, cancer, and viral diseases, transplantation, juvenile diabetes, myasthenia gravis, and multiple sclerosis. The present invention thus includes compositions containing a compound of formula 1 in treating disease such as autoimmune disease characterized by abnormal immune response in warmblooded animals. According to this aspect of the invention, the properties of the compounds of the invention are utilized by administering to a warm-blooded animal an effective amount of a pharmaceutical composition containing as the active ingredient at least about 0.1 percent by weight, based on the total weight of the composition of at least one such compound of the invention.
Pharmaceutical compositions of the invention can be formulated in any suitable way, preferably with an inert carrier for administration orally, parenterally, ophthalmically, topically, or by suppository.
For example, the compounds of the present invention are formulated into dosage forms such as tablets or syrups by blending with an inert pharmaceutical carrier such as lactose or simple syrup by methods well known in the art. For injectionable dosage forms, they are formulated with vehicles such as water, peanut oil, sesame oil, and the like. In these dosage forms, the active ingredient is from about 0.05 grams to 0.5 grams per dosage unit.
The present invention is further illustrated by way of the following examples.
EXAMPLE 1
2-Amino-8-bromo-9-[(2-hydroxyethoxy)methyl]-9H-purin6-ol a
N-bromosuccinimide (0.415 g; 2.3 mmol) is added to a solution of acycloguanosine (0.5 g; 2.2 mmole) (prepared according to British Patent 1,567,671) in acetic acid (7 ml) and the mixture stirred at room temperature for 20 hours. The solution is then diluted with water (20 ml) and the precipitated product is filtered, washed, and triturated with hot water to give 0.25 g of white solid, mp>300° C.
EXAMPLE 1A
The procedure described in Example 1 is repeated to prepare the following 8-bromo-9-substituted guanines starting from appropriate 9-substituted guanines in each case using acetic acid, methanol or DMF as solvent:
2-amino-8-bromo-9-[[2-(heptyloxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp>250° C., dec;
2-amino-8-bromo-9-[[2-(hexyloxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp>250° C., dec;
2-amino-8-bromo-9-[[2-butoxy-1-(hydroxymethyl) ethoxy]methyl]-9H-purin-6-ol, mp>200° C.;
2-amino-8-bromo-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(octyloxy)ethoxy]methyl]-6H-purin-6-one, mp 223°-226° C., dec;
2-amino-8-bromo-9-[[2-(hexyloxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp 212°-214° C.;
2-amino-8-bromo-9[[2-ethoxy-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one, mp 217°-219° C., dec;
2-amino-8-bromo-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(pentyloxy)ethoxy]methyl]-6H-purin-6-one, mp>250° C., dec;
2-amino-8-bromo-9-[[2-(cyclohexylmethoxy)-1-(hydroxymethyl)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp 210°-212° C. (dec);
2-amino-8-bromo-1,9-dihydro-9-[[1-(hydroxymethyl)-2-phenoxyethoxy]methyl]-6H-purin-6-one, mp 218°-219° C., dec;
2-amino-8-bromo-1,9-dihydro-9-[[2-hydroxy)-1-[(4-methoxyphenoxy)methyl]ethoxy]methyl]-6H-purin-6-one; mp 205°-210° C., dec;
2-amino-8-bromo-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(4-methylphenoxy)ethoxy]methyl]-6H-purin-6-one, mp 207°-208° C., dec;
2-amino-8-bromo-1,9-dihydro-9-[[2-(4-chlorophenoxy)-2-(hydroxmethyl)ethoxy]methyl]-6H-purin-6-one, and 2-amino-8-bromo-1,9-dihydro-9-[[[1-(hydroxymethyl) nonyl]oxy]methyl]-6H-purin-6-one, mp 211°-212° C., dec.
EXAMPLE 2
2,8-Diamino-9-[(2-hydroxyethoxy)methyl-9-9H-purin-6-ol
The crude 2-amino-8-bromo-9-[(2-hydroxy-ethoxy)methyl]-9H-purin-6-ol from acycloguanosine (3.17 g; 0.14 mol) is suspended in water (10 ml) and 97% hydrazine (4 ml) is added to the mixture. The mixture is refluxed for 48 hours, cooled and filtered to give a white solid (1.6 g) which is triturated with hot water (75 ml) to give the analytical sample (1.5 g), mp>300° dec.
EXAMPLE 3
2-[(2-Amino-8-bromo-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol
N-bromosuccinimide (0.375 g; 2.1 mmol) is added to a solution of 9'-[(1,3-dihydroxy-2-propoxy) methyl]guanine (0.5 g; 1.9 mmole) [prepared according to J. C. Martin; C. A. Dvorak, D. F. Smee, T. R. Matthews, and J. P. H. Verheyden, J Med Chem 26, 759-761 (1983)] in acetic acid (7 ml). The suspension is stirred for 1.5 hours at room temperature and then diluted with water (60 ml). The aqueous solution is concentrated and the residue is recrystallized from water to give 0.44 g of the product; mp>300° dec.
EXAMPLE 4
2-[(2,8-Diamino-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol
A mixture of 2-[(2-amino-8-bromo-6-hydroxy-9H-purin-9-yl)methoxy]-1,3-propanediol (13.7 g; 41 mmole) and 97% hydrazine (6.07 ml) in water (300 ml) is heated to reflux for 48 hours. At the end of this time, the solution is cooled and filtered to give 9.15 g of crude solid. The crude product is suspended in water (120 ml) and Raney nickel (9 g) is added. The mixture is heated at reflux for 6 hours, filtered hot and cooled. The crystals are collected and dried to give 7.15 g of the product, mp>280° dec.
EXAMPLE 4A
The procedure described in Example 4 is repeated to prepare the following 8-amino-9-substituted guanines starting from appropriate 8-bromo-9-substituted guanines in each case using methoxyethanol as a cosolvent as necessary to make a homogeneous reaction mixture:
2,8-diamino-9-[[2-ethoxy-1-(hydroxymethyl)ethoxy] methyl]-9H-purin-6-ol, mp>220° C., dec;
2,8-diamino-9-[[2-(hexyloxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one, mp>265° C., dec;
2,8-diamino-9-[[2-butoxy-1-(hydroxymethyl)ethoxy] methyl]-9H-purin-6-ol, mp>240° C., dec;
2,8-diamino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(pentyloxy)ethoxy]methyl]-6H-purin-6-one, mp 274°-277° C., dec;
2,8-diamino-9-[[2-(heptyloxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp>260° C., dec;
2,8-diamino-9-[[2-(hexyloxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one, mp 260°-265° C., dec; 2,8-diamino-9-[[2-(cyclohexylmethoxy)-1-(hydroxymethyl)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp 242°-247° C., dec;
2,8-diamino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(octyloxy)ethoxy]methyl]-6H-purin-6-one, mp>265°-271° C., (dec);
2,8-diamino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-phenoxyethoxy]methyl]-6H-purin-6-one, mp 265°-271° C., dec;
2,8-diamino-1,9-dihydro-9-[[2-hydroxy-1-[(4-methoxyphenoxy)methyl]ethoxy]methyl]-6H-purin-6-one;
2,8-diamino-1,9-dihydro-9-[[1-hydroxymethyl)-2-(4-methylphenoxy)ethoxy]methyl]-6H-purin-6 one; mp>250° C., dec;
2,8-diamino-1,9-dihydro-9-[[2-(4-chlorophenoxy)-1-hydroxymethyl)ethoxy]methyl]-6H-purin-6-one, and
2,8-diamino-1,9-dihydro-9-[[[1-(hydroxymethyl)nonyl] oxy]methyl]-6H-purin-6-one.
EXAMPLE 5
9-[[2-Benzyloxy-1-(benzyloxymethyl)-ethoxy]methyl]-8-hydrazine-guanine
A mixture of 9-[[2-benzyloxy-1-(benzyl oxymethyl)-ethoxy]methyl]guanine (2.1 g) [prepared according to K. K. Ogilvie, V. O. Cheriyan, B. K. Radatus, K. O. Smith, K. S. Galloway, and W. L. Kennell, Can J Chem, 60, 3005 (1982)] and N-bromosuccinimide (0.94 g) in acetic acid (21 ml) is stirred overnight and then is diluted with water and extracted with chloroform. The chloroform extract is dried and concentrated to give 2.3 g of yellow oil. The crude oil is suspended in ethanol (100 ml) and treated with 95% hydrazine. The solution is heated to reflux for 24 hours. The reaction mixture is then cooled and the product (0.75 g) filtered and dried, mp>210° dec.
EXAMPLE 6
8-Amino-9-[[2-benzyloxy-1-(benzyloxymethyl)-ethoxy]-methyl]-guanine
A mixture of 9-[[2-benzyloxy-1-(benzyloxymethyl)-ethoxy)methyl]-8-hydrazine-guanine (0.45 g; 0.98 mmol), water (40 ml), ethanol (40 ml), ammonium hydroxide (20 ml) and Raney nickel (1 g) is heated to reflux for 24 hours. The catalyst is filtered off and the filtrate concentrated to a solid which is recrystallized from ethanol to give 0.16 g of analytical sample, mp 255°-260° dec.
EXAMPLE 7
N-[9-[[1-(Butoxymethyl)-2-(phenylmethoxy)ethoxy] methyl]-6-hydroxy-9H-purin-2-yl]acetamide
Dry HCl (g) is bubbled into a stirred mixture of paraformaldehyde (1.45 g, 0.048 mol) and 1-butoxy-3-(phenylmethoxy)-2-propanol (5.0 g, 0.021 mol) in methylene chloride (57 ml) at 0° C. until all the solid is dissolved. The resulting solution is stored at 0° C. for 16 hours, dried over MgSO 4 , and then evaporated to give chloromethyl glycerol ether as a very unstable clear oil. The clear oil is then added dropwise to a stirred mixture of potassium acetate (5.0 g, 0.051 mol) in acetone (60 ml). The mixture is stirred for 16 hours at room temperature and then filtered and evaporated. The residual oil is dissolved in toluene, washed with saturated NaHCO 3 and water, dried, and evaporated to give the acetoxy derivative as an oil (5.6 g) which is immediately used for condensation with diacetylguanine.
A mixture of diacetylguanine (4.6 g, 0.0195 mol) and crude acetoxy derivative from above (5.6 g), p-toluene sulfonic acid (43 mg) and sulfolane (5 ml) is heated to 95° C. under nitrogen atmosphere for 72 hours. At 24 hours and 48 hours, additional amounts of p-toluene sulfonic acid (20 mg each) are added. After 72 hours, the mixture is cooled, diluted with toluene and filtered. The filtrate is concentrated, chromatographed, and recrystallized from toluene to provide the desired product (1.33 g), mp 139°-141° C.
EXAMPLE 8
The procedure described in Example 7 is repeated to prepare the following guanine-2-acetamide derivatives, starting from diacetylguanine and appropriate 1-(alkoxy or alkyl or substituted phenoxy)-3-(phenylmethoxy)-2-propanols in each case.
N-[6,9-dihydro-9-[[1-[(octyloxy)methyl]-2-(phenylmethoxy)ethoxy]methyl]-6-oxo-1H-purin-2-yl]acetamide, mp 127°-132° C.;
N-[6,9-dihydro-6-oxo-9-[[1-(phenoxymethyl)-2-(phenylmethoxy)ethoxy]methyl]-1H-purin-2-yl]-acetamide, mp 144°-146° C., and
N-[9-[[1-(ethoxymethyl)-2-(phenylmethoxy)ethoxy] methyl]-6,9-dihydro-6-oxo-1H-purin-2-yl]acetamide, mp 131°-133° C., dec.
EXAMPLE 9
2-Amino-9-[[2-butoxy-1-(hydroxymethyl)ethoxy]methyl]-9H-purin-6-ol
A mixture of N-[9-[[1-(butoxymethyl)-2-(phenylmethoxy)ethoxy]methyl]-6-hydroxy-9H-purin-2-yl]acetamide (1.15 g, 25.9 mmol), 20% palladium on carbon (0.2 g), cyclohexene (20 ml), and ethanol (10 ml) is heated at reflux under N 2 . After 8 and 2O hours, additional amounts of catalyst (0.1 g) are added. After 36 hours, the solution is cooled, filtered through celite, and the filter cake is washed with DMF/ethanol. The filtrates are combined, refiltered and concentrated. The residue is mixed with aq. methyl amine (20 ml) and the mixture is heated at reflux for two hours, filtered and concentrated. The residue is recrystallized from water to give the desired product (0.7 g), mp 208°-211° C.
EXAMPLE 10
The procedure described in Example 9 is repeated to prepare the following 9-substituted guanine derivatives, starting from N-[9-substituted-6-hydroxy-9H-purin-2-yl]acetamides in each case. Cyclohexene and cyclohexadiene can either be used in the transfer hydrogenation reaction 2-amino-9-[[2-ethoxy-1-(hydroxymethyl)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp 206°-209° C.; 2-amino-1,9-dihydro-9[[1-(hydroxymethyl)-2-phenoxyethoxy]methyl]-6H-purin-6-one, mp 195°-198° C., and 2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(octyloxy) ethoxy]methyl]-6H-purin-6-one, mp 227°-230° C.
EXAMPLE 11
2-Amino-9-[[1-[(heptyloxy)methyl]-2-[phenylmethoxy) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one
A mixture of 2-amino-6-chloropurine (Aldrich Chemical Co.) 11.2 g, 0.066 mol) hexamethyldisilazane (160 ml), and ammonium sulfate (1.09 g) is refluxed for 2.5 hours and then cooled, concentrated and pumped to dryness. The residue is dissolved in dry toluene (210 ml) and is treated with Hg(CN) 2 . The mixture is heated to 80° C. and a solution of 2-(chloromethoxy)-1-(heptyloxy-3-(phenylmethoxy) propane (prepared from 1-(heptyloxy)-3-(phenylmethoxy)-2-propanol (19 g, 0.068 mol), paraformaldehyde (4 g) and dry HCl (g) in CH 2 Cl 2 (160 ml) as described in the first part of Example 7, in toluene (210 ml) is added to the solution and heated to 80°-85° C. for 2.5 hours. The mixture is cooled, concentrated, and diluted with CH 2 Cl 2 (1.0 L) and is allowed to stand overnight. The CH 2 Cl 2 solution is filtered, washed with 30% KI, 10% potassium carbonate solution and water. The organic layer is dried and concentrated. The residue is chromatographed over silica gel column using a high pressure liquid chromatographic instrument (Waters Prep 500). The column is eluted with ethyl acetate and hexane (1:1) to give the condensation product (i.e., chloropurine derivative) (6.45 g) which is hydrolysed as follows.
A mixture of the above chloropurine derivative (6.42 g, 0.0139 mol) methanol (150 ml) and sodium methoxide (3 g, 0.056 mol) is treated with mercaptoethanol (4.4 ml) and water (0.26 ml). The mixture is then heated to reflux under nitrogen for two hours and then an additional amount of sodium methoxide (1.9 g) is added. The reaction mixture is heated to reflux for an additional 4.0 hours, cooled, and concentrated to about 50 ml. The concentrate is diluted with water (120 ml) and the solution is acidified to pH 6.0. The solid precipitate is filtered, washed with water, and dried. The crude product is then recrystallized from methanol/water to give an analytical sample (4.25 g), mp 185°-187° C.
EXAMPLE 12
The procedure described in Example 11 is repeated to prepare the following 9-substituted guanines starting from 2-amino-6-chloropurine and appropriate 1-(alkoxy or substituted phenoxy or alkyl)-3-(phenylmethoxy)-2-propanols in each case:
2-amino-9-[1-(cylcohexylmethoxy)methyl]-2-(phenylmethoxy)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one, mp 198°-201° C;
2-amino-9-[1-[(hexyloxy)methyl]-2-(phenylmethoxy) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one; mp 192°-194° C.
2-amino-1,9-dihydro-9-[1-[(pentyloxy)methyl]-2-(phenylmethoxy)ethoxy]methyl]-6H-purin-6-one, mp 192°-194° C.;
2-amino-1,9-dihydro-9-[-1-[(octyloxy)methyl]-2-(phenylmethoxy)ethoxy]methyl]-6H-purin-6 one, mp 184°-186° C.;
2-amino-1,9-dihydro-9-[1-(phenoxy)methyl)-2-(phenylmethoxy)ethoxy]methyl]-6H-purin-6-one;
2-amino-1,9-dihydro-9-[[[1-[(phenylmethoxy)methyl]hexyl]oxy]methyl-6H-purin-6-one, mp 206°-208° C.;
2-amino-1,9-dihydro-9[[[1-[(phenylmethoxy)methyl] nonyl]oxy]methyl-6H-purin-6-one, mp 205°-207° C.;
2-amino-9-[1-[(4-chlorophenoxy)methyl]-2-[phenylmethoxy]ethoxy]methyl]-1,9-dihydro-6H-purin-6one, mp>210° C.;
2-amino-1,9-dihydro-9-[1-[(4-methoxyphenoxy)methyl]-2-[phenylmethoxy]ethoxy]methyl]-6H-purin-6-one, mp 150°-156° C., and
2-amino-1,9-dihydro-9-[1-[(4-methylphenoxy)methyl]-[phenylmethoxy]ethoxy]methyl]-6H-purin-6-one, mp 198°-200° C.
EXAMPLE 13
2-Amino-9-[[2-(heptyloxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one
A mixture of 2-amino-9-[1-[(heptyloxy)methyl]-2-(phenylmethoxy)ethoxy]methyl]-1,9-dihydro-6H-purin-6-one (3.9 g, 8.97 mmol), ethanol (200 ml), cyclohexadiene (87 ml, 92.3 mmol), and 20% palladium on charcoal (1.5 g) is heated to reflux under nitrogen atmosphere. After seven hours an additional amount of 20% palladium on charcoal (0.5 g) is added and the mixture is heated to reflux for a total of 18 hours. The mixture is filtered hot and then allowed to cool. The solid formed is collected and dried to give the desired purine (1.95 g), mp 224°-225° C.
EXAMPLE 14
The procedure described in Example 13 is repeated to prepare the following 9-substituted guanines starting from appropriate phenylmethoxy derivatives described in Example 11 and 12.
2-amino-1,9-dihydro-9-[[[1-(hydroxymethyl)hexyl] oxy]methyl]-6H-purin-6-one, mp 228°-229° C.;
2-amino-1,9-dihydro-9-[[[1-(hydroxymethyl)nonyl] oxy]methyl]-6H-purin-6-one, mp>250° C., dec;
2-amino-9-[[2-(ethoxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6H-purin-6-one, mp 206°-209° C.;
2-amino-9-[[2-(butoxy)-1-(hydroxymethyl)ethoxy] methyl]-9H-purin-6-ol, mp 208°-211° C.;
2-amino-]-[[2-(hexyloxy)-1-(hydroxymethyl)ethoxy] methyl]-1,9-dihydro-6-H-purin-6-one;
2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(penyloxy)ethoxy]methyl]-6H-purin-6-one, mp 218°-220° C.;
2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(octyl-oxy)ethoxy]methyl]-6H-purin-6-one, mp 227°-230° C.;
2-amino-9-[[2-(cyclohexylmethoxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purine-6-one, mp>260° C., dec;
2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-phenoxyethoxy]methyl]-6H-purin-6-one, mp 195°-198° C.;
2-amino-1,9-dihydro-9-[[1-(hydroxymethyl)-2-(4-methylphenoxy)ethoxy]methyl]-6H-purin-6one, mp 206°-208° C.;
2-amino-1,9-dihydro-9-[[2-(hydroxy-1-(4-methoxyphenoxy)methyl]ethoxy]methyl]-6H-purin-6-one, mp 210°-217° C., dec, and
2-amino-9-[[2-(4-chlorophenoxy)-1-(hydroxymethyl) ethoxy]methyl]-1,9-dihydro-6H-purin-6-one,
SYNTHESIS OF STARTING MATERIALS
EXAMPLE A
1-Butoxy-3-(phenylmethoxy)-2-propanol
n-Butanol (2.5 ml, 27 mmol) is added to a suspension of sodium hydride (50% in mineral oil; 1.3 g, 27 mmol) in DMF (5 ml) and the mixture is then heated to 80° C. for 1.0 hours when all the sodium hydride is consumed. A solution of 2,3-epoxypropyl benzyl ether (benzyl glycidylether*) (4.52 g, 27 mmol) in DMF (5 ml) is added slowly to the n-butoxide solution. The mixture is then heated to 80° C. for 16 hours, diluted with water and extracted with ether. The ether layer is dried and concentrated to give an oil which is distilled to provide the desired product (3.1 g), bp 125°-130°/0.8-0.5 mm.
EXAMPLE B
The procedure described in Example A is repeated to prepare the following 1-alkoxy or aryloxy-3-(phenylmethoxy)-2-propanols, starting from appropriate alkanols or phenols in each case.
1-(ethoxy)-3-(phenylmethoxy)-2-propanol, bp 92°-99° C./0.25-0.3 mm;
1-(pentyloxy)-3-(phenylmethoxy)-2-propanol, bp 115°-118° C/0.3 mm;
1-(hexyloxy)-3-(phenylmethoxy)-2-propanol, bp 123°-125° C./0.12 mm;
1-(heptyloxy)-3-(phenylmethoxy)-2-propanol, bp 141° C./0.36 mm, and
1-(octyloxy)-3-(phenylmethoxy)-2-propanol, bp 150°-155° C./0.7 mm.
EXAMPLE C
1-(Phenylmethoxy)-2-decanol
Benzyl alcohol (108 g, 1.0 mol) is added to a suspension of 50% sodium hydride-mineral oil (48 g, 1.0 mol) in DMF (200 ml) at room temperature. The mixture is then heated to 80° C. for two hours. A solution of 1,2-epoxydecane* (85 ml) in DMF (50 ml) is added slowly to the sodium salt over 30 minutes and the mixture is then heated at 80° C. for 20 hours. The reaction mixture is cooled, diluted with water, neutralized with acetic acid, and extracted with ether. The ether extract is concentrated to give an oil which is distilled to give the desired product (131 g), bp 178°-180° C./4 mm.
EXAMPLE D
The procedure described in Example C is repeated to prepare the following 1-(phenylmethoxy)alkanols, starting from appropriate 1,2-epoxides in each case.
1-(cyclohexylmethoxy)-3-(phenylmethoxy)-2-propanol, bp 136°-139° C./0.24-0.22 mm;
1-(phenylmethoxy)-2-heptanol, bp 125°-130° C./3-5 mm;
1-(phenoxy)-3-(phenylmethoxy)-2-propanol, bp 148°-157° C./0.32 mm;
1-(4-methylphenoxy)-3-(phenylmethoxy)-2-propanol, bp 194° C./2 mm;
1-(4-methoxyphenoxy)-3-(phenylmethoxy)-2-propanol, bp 175°-184° C./0.4 mm, and
1-(4-chlorophenoxy)-3-(phenylmethoxy)-2-propanol, bp 188°-190° C./1.2-1.3 mm.
|
Novel purine derivatives are described as agents for treating autoimmune diseases as well as a method of manufacture and pharmaceutical compositions as well as novel intermediates in the manufacture thereof.
| 2
|
FIELD OF THE INVENTION
[0001] The present invention concerns orodispersible self supporting films having quick dissolution times for therapeutic and food use.
STATE OF THE ART
[0002] Orodispersible self supporting films for releasing active ingredients for therapeutic or food use have been known for a long time and are available on the market.
[0003] These films disintegrate quickly in the mouth releasing the active ingredient.
[0004] Many of the films known at the state of the art use pullulan as the film forming component which is, however, an ingredient that is expensive and difficult to find.
[0005] It has thus been attempted to replace pullulan with less expensive ingredients that are, in any case, capable of maintaining the properties like their quick dissolution times, mouth freshness, marked aroma, and simplicity of preparation.
[0006] US2003011259 describes a film having quick dissolution times containing maltodextrin and hydrocolloids, in quantities that are greater than 10%, as film forming component. Hydrocolloids are necessary in order to facilitate the disgregation of the film but do not give the sensation of having a clean mouth since they tend to gel in contact with saliva.
[0007] EP1689374 by the same applicant describes self-supporting films for releasing active ingredients for therapeutic or food use based on maltodextrin and a plasticizer, totally without hydrocolloids. These films quickly disgregate in the mouth and release the active ingredient in the oral cavity keeping the sensation of having a clean mouth that is indeed of pullulan-based films.
[0008] These films however have a drawback concerning their physical stability as they tend to harden over time.
SUMMARY OF THE INVENTION
[0009] It has now been surprisingly found that it is possible to avoid hardening of the films based on maltodextrin and plasticizer by incorporating, in the composition, a homopolymer or copolymer of vinyl acetate.
[0010] The polymers in general of vinyl acetate and in particular polyvinyl acetate are insoluble in water, the latter being used in many medicinal products, for example in pharmaceutical formulations with a prolonged release over time, or as a base in chewing gum.
[0011] The present invention concerns orodispersible self-supporting films without hydrocolloids comprising:
a) a film-forming substance consisting of a maltodextrin in a quantity comprised between 40 and 80% by weight; b) a plasticizer in a quantity comprised between 15 and 55% by weight; e) a surfactant system in a percentage comprised between 0.5 and 6% by weight; d) an active ingredient for food or therapeutic use in a quantity comprised between 0.05 and 30% by weight,
characterised in that it contains a homopolymer or copolymer of vinyl acetate, in a quantity comprised between 2 and 10% by weight where the percentages are calculated on the total weight of said film.
DETAILED DESCRIPTION OF THE INVENTION
[0016] The orodispersible films of the invention have disgregation times evaluated in vitro that are lower than 3 minutes, they do not stick, they do not expand and are stable over time as far as the mechanical properties of elasticity and tensile strength are concerned.
[0017] The copolymer of vinyl acetate is preferably selected from the group consisting of polyvinylpyrrolidone vinyl acetate, ethylene vinyl acetate. More preferably the homopolymer of vinyl acetate, namely polyvinyl acetate, is used.
[0018] In particular the polyvinyl acetate used in the invention has an weight average molecular weight of between 5000 and 500000, preferably between 250000 and 450000. A polyvinyl acetate that can be used in the invention is that sold with trademark Kollicoat® SR 30D commercialised by BASF.
[0019] Preferably the content of polyvinyl acetate in the film according to the present invention is between 2.5 and 10%, more preferably between 3 and 10%, even more preferably between 3 and 6% and according to a particularly preferred solution between 3 and 5.5% by weight on the total weight of the film.
[0020] The maltodextrin used in the self-supporting film of the present invention has a dextrose content, expressed in equivalents, that is less than 50, and preferably is between 11 and 40.
[0021] The plasticizer used in the film of the present invention is preferably selected from the group consisting of polyalcohols, esters of citric acid, sebacic acid esters or mixtures thereof.
[0022] Particularly preferred are propylene glycol, glycerine, sorbitol, maltitol and mixtures thereof
[0023] The surfactant system used in the film of the present invention consists of one or more surfactants, preferably selected from the group consisting of sorbitan derivatives, sorbitol derivatives, esters of sucrose, fatty acid esters and their mixtures.
[0024] The active ingredient for food use is preferably an active ingredient with a breath freshening action and/or indicated for oral hygiene, preferably eugenol or menthol or a vegetal extract or an active ingredient of natural origin, suitable for nutritional supplementation, preferably mineral salts among those normally used for such a purpose or one or more vitamins. According to a particularly preferred solution the vitamin is ascorbic acid.
[0025] The active ingredient for therapeutic use can be an ingredient with essentially topical action of the oral cavity selected from antibacterial, antifungal, antiviral agents or disinfectants of the oral cavity, or it can be an ingredient with an essentially systemic action selected from the group consisting of anti-inflammatory, analgesic, antipsychotic, hypnotic, anxiolytic, muscle relaxant, antimigraine, antiparkinsonian, antiemetic, antihistaminic, beta blocker, anti-asthmatic anti-hypertensive, antitussive, laxative agents, inhibitors of type V phosphodiesterase, antikinetosis agents.
[0026] Active ingredients contained in such films are preferably selected from the group consisting of: Piroxicam, Ketoprofen, Diclofenac, Tramadol, Morphine, Nifedipine, Diazepam, Lorazepam, Alprazoiam, Bromazepam, Triazolam, Lormetazolam, Zolpidem, Paracetamol, Selegiline; Atenolol, Salbutamol, Sumatriptan, Clozapine, Ceterizine and their pharmaceutically acceptable salts.
[0027] Moreover, the films according to the invention can possibly contain other excipients selected in the class of non-stick substances like for example colloidal silica or talc, sweeteners, flavourings, colorants, preservatives, buffer systems or mixtures thereof.
[0028] The films object of the invention can be produced with known processes, like those described in EP 1689374.
[0029] In particular a process can be used comprising the steps of:
i) dispersing the maltodextrin, the plasticizer, the surfactant system, the homopolymer or copolymer of vinyl acetate, preferably polyvinyl acetate and the active ingredient for therapeutic or food use in a polar solvent, ii) laminating the mixture obtained in the previous step on a silicone paper, iii) drying, iv) removing the silicone paper from the film obtained in the preceding step.
[0034] The polar solvent used in step (i) is preferably selected from water, water-mixable solvents or relative mixtures. According to a particularly preferred solution it consists of water. The temperature of the step itself, when the mixture of the aforementioned solvents is used, is preferably comprised between 60 and 105° C.
Example 1
Preparation of Placebo Orodispersible Films
[0035] The polymer mixture used for preparing the films was obtained by solubilizing maltodextrin DE 6 in a suitable amount of water kept at T=80° C.
[0036] The mixture was subsequently gradually cooled and glycerine, the surfactants, the homopolymer or copolymer of vinyl acetate and the other components were added in the ratios indicated in Table 1. The system obtained is kept under stirring until all the components were dissolved.
[0037] The composition of the polymer mixtures used for preparing the film is shown in Table 1.
[0000]
TABLE 1
Composition %(w/w)
Components
1
2
3
4
5
6
7
8
9
10
11
maltodextrin
78.99
80.72
76.50
74.87
70.78
62.68
76.50
76.00
77.00
76.50
75.00
DE6
glycerine
18.05
14.57
17.48
17.11
16.17
14.32
17.50
17.00
16.50
17.50
17.00
Span80
2.96
3.71
3.01
3.01
3.05
2.99
3.00
3.00
3.00
3.00
PVAc
1.00
3.01
5.01
10.00
20.00
Capryol 90
3.00
EVA
3.00
4.00
3.50
PVP/VA
3.00
5.00
[0038] The preparation of the film was carried out using the Mathis Labcoater-Labdryer model LTE —S (M) (CH) according to a method that foresees coating the mixture on a protective silicone sheet. The operation conditions used are as follows:
Coating speed: 1 m/min Drying time: 15 min Drying temperature: 60° C. Rotation speed of the fan: 1800 rpm (revs/minute) Coating thickness: 380 um
[0044] The films thus prepared were separated by the protective sheet, cut with the desired dimensions and preserved in waterproof and lightproof packets.
Example 2
Determination of the Tensile Properties
[0045] The analysis of the tensile properties was carried out in accordance with ASTM standards (International Test Method for Thin Plastic Sheeting) (D 8 82-02) using an Acquati electronic dynamometer mod. AG/MC1 (I) on which a load cell of 5 N was assembled. The result of the tests is expressed as an average of the analysis on 5 samples for each formulation. The film was preliminarily cut into strips with a length of 100 mm and width of 12.5 mm. Once it was verified that there were no breaks or a lack of homogeneity in the matrix, the samples were positioned longitudinally between two pneumatic clamps spaced at 60 mm from one another. The separation velocity of the clamps was set at 500 mm/min. The test was considered finished once the film broke. Variations in the rigidity of the material were measured by determining the elastic modulus (Y) after the preparation of the films and after three months of preservation at 40° C.
[0046] The addition of PVAc was considered positive if the value Y increased at the moment of the preparation with respect to the formulation free from this component and if the variation of this value (V) after 3 months from the preparation did not vary more than 25%
Results
[0047] The elastic modulus values Y are shown in Table 2
[0000]
TABLE 2
films 1-6 elastic modulus values after preparation thereof
and after being preserved for three months at 40°
C. and variation percentage (V) thereof over time.
Preservation (months)
Formulation
0
3
(V)
1
26
61
135%
2
59
78
32%
3
113
119
5%
4
55
69
25%
5
35
40
14%
6
14
23
64%
[0048] The results show how the addition of PVAc in the range 3-10% makes it possible to improve the mechanical properties of the film. Indeed, with respect to the reference formulation 1, the films containing PVAc in the selected range make it possible to increase the values of Y and at the same time reduce the variation (V) of such a parameter Y over time.
Example 3
Preparation of Orodispersible Films Containing Diclofenac
Preparation of the Film
[0049] The films, the composition of which is shown in Table 3 were prepared according to what is described in example 1
Determination of the Mechanical Properties
[0050] The elastic modulus was determined according to what is described in Example 1.
Disgregation Test
[0051] The disgregation test was carried out according to, the specifications for orodispersible tablets shown in Eur. Ph. Ed. 7.0, setting the time T<3 min and using samples of 6 cm 2 .
[0052] For every formulation, three tests were carried out and the results were expressed as an average±standard deviation.
Dissolution Test
[0053] The dissolution test in vitro was carried out on samples of 6 cm 2 using “Basket Dissolution Apparatus” (Eur. Ph. 7.0, Section 2.9.3).
[0054] The following parameters characterise the method used for evaluating the % drug dissolved:
Equipment: Sotax AT7 Smart Dissolution system with Basket Temperature: 37±0.5° C. Dissolution medium: phosphate buffer pH 6.8 Volume of dissolution: 500 mL Rotation speed: 100 rpm (revs/minute) Sampling time: 5 minutes
[0061] The buffer volume described was inserted in the 7 vessels of the dissolution system and the system was left to settle at the set temperature of 37° C. A film was introduced in each of the first 6 baskets, the 7 th vessel was used as the control and therefore the relative basket was kept empty.
[0062] Once the set temperature was reached, the baskets were lowered into the dissolution medium. After 5 minutes an aliquot was taken from each vessel. The samples obtained were analysed in HPLC by using the following method.
[0063] HPLC Agilent 1100, with Grace Alitima HP C 18 column with dimensions 100×4.6 mm and 3 μm. An isocratic elution was carried out comprising mixing a mobile phase A and a mobile phase B. Phase A consisted in 90% of a 20 mM phosphate buffer at pH 2.0 prepared dissolving 3.12 g of sodium dihydrogen phosphate in 1 litre of Milli-Q water and regulating the pH to 2.0 with conc. phosphoric acid (H 3 PO 4 ) and 10% of tetrahydrofuran for HPLC. Phase B consisted of grade HPLC Methanol. The two phases were mixed in the proportions indicated here: Phase A: 40%, Phase B: 60%. The column temperature was set at 40° C., flow 1.3 ml/min, selected wavelength 254 nm, injection volume 2 μl.
Results
[0064] The results shown in table 3 indicate that the addition of PVAc makes it possible to obtain films having mechanical properties and tensile strength that are considerably higher than reference films, while maintaining unaltered disgregation and release characteristics.
[0000]
TABLE 3
Composition and technological characteristics of the films
Formulation
Components
D1
D2
Maltodextrin IT6
57.11
60.73
Glycerine
3.80
4.04
Span 80
1.44
1.53
PVAc 5,00
5.00
—
sorbitol
6.66
7.08
Peach aroma
3.42
3.64
Betaine
2.78
2.95
Mint aroma in PG
1.90
2.02
Sucralose
1.14
1.21
Tween 20
0.72
0.77
Titanium dioxide
0.23
0.24
Diclofenac epolamina
15.80
15.78
Mechanical properties
160
118
Y(kPa)
Dissolution test
98.6
104.5
% dissolved (limit >80%)
Disaggregation test
passed
passed
T < 3 min
Example 4
Preparation of Orodispersibile Films Containing Diclofenac Preparation of the Films
[0065] The films D1 and D2 of the example 3 were preserved at 25° C. for 9 months and thus characterised according to the methods shown in the previous examples. In particular the elastic modulus was determined according to what is described in Example 1, whereas the disgregation time was verified according to what is described in Example 3.
Results
[0066] The results are shown in Table 4.
[0000]
TABLE 4
Composition and technological characteristics of the films
Formulation
D1
D2
Mechanical properties
172
173
Y (kPa)
Disaggregation test
Passed
Passed
T < 3 min
[0067] From the results shown above it is possible to highlight that the formulation D1 has a variation V % of Y after 9 months equal to 7.5%. On the other hand, the formulation without polyvinyl acetate has a variation % of Y of 46.6% much greater than the threshold limit of 25%.
|
The present invention concerns an orodispersible self-supporting film free from hydrocolloids comprising: a) a film-forming substance consisting of a maltodextrin in an amount comprised between 40 and 80% by weight; b) a plasticizer in an amount comprised between 15 and 55% by weight; e) a surfactant System in an amount comprised between 0.5 and 6% by weight; d) an active ingredient for food or therapeutic use in an amount between 0.05 and 30% by weight, characterised in that it contains a homopolymer or a copolymer of vinyl acetate in a quantity comprised between 2 and 10% by weight where the percentages are calculated on the total weight of said film
| 0
|
CROSS REFERENCE TO RELATED APPLICATIONS
This Application is a division of and claims the benefit of the earlier filing date of co-pending U.S. patent application Ser. No. 12/767,784, filed Apr. 26, 2010,which is a continuation of U.S. patent application Ser. No. 11/213,218, Aug. 25, 2005,which issued on Apr. 27, 2010, as U.S. Pat. No.: 7,704,907, the entire contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
The following invention is generally directed to synthetic hybrid rock compositions of matter, articles of manufacture and related processes employing as starting material mine tailings, mine development rock, ash, slag, quarry fines, slimes, and similar mineral waste materials.
DESCRIPTION OF RELATED ART
Mine reclamation and waste mineral processing are not, by far, new industries. Numerous systems, processes and methods exist to affect environmental mine clean-up, and manufacture useful products from raw materials comprised primarily of waste minerals constituents.
U.S. Pat. No. 3,870,535 discloses a method of treating coal mining refuse to produce a cementitious material, which is self-hardening at atmospheric pressure, and may be used as structural fill, road base material, or alternatively as an aggregate consolidated barrier to prevent penetrating percolation and resulting surface water contamination. The method involves treating coal mining tailings from coal extraction processes with lime (to neutralize sulfuric acid), or lime and a pozzolanic material, such as fly ash, to react at atmospheric pressure for at least several days, in the presence of moisture with sulfate ions that have been released from the tailings, and in some cases also to react with soluble iron products in the tailings. The claimed products are admixtures of coal mining refuse and stoichiometrically distinct concentrations of lime, water and fly ash. The products of the invention are generally of the variety 3CaO, Al 2 O3, 3CaSO 4, 30 -32H 2 O or 3CaO, Al 2 O 3 , CaSO 4 , and 10-12H 2 O. Permeability testing data for product samples indicated that permeability diminished after completion of a seven day curing period at 100° F. Likewise, compressive strength data indicated that the material's compressive strength, measured in PSI, increased as the curing period progressed. Detailed information regarding the composition's density and plasticity is not disclosed. However, the composition is cementitious in nature, and therefore limited in application and potential utility. Well known disadvantages associated with cement based products include high porosity and structural instability as a result of temperature and climate fluctuations.
U.S. Pat. No. 5,286,427 discloses a method of effecting environmental cleanup by producing structural building materials using mine tailings waste material. The method involves providing facilities for producing the structural building material; providing raw materials for producing the building material, the raw materials comprising unprocessed mine tailings (with a material gradation suitable for immediate use) as a substitute for processed silica sand, plus cement and aluminum powder; analyzing the mine tailings to determine composition and weight percentage amounts of other raw materials present; preparing a slurry from the mine tailings and combining the slurry with other raw materials to form a batch slurry; adjusting amounts of other raw materials in accordance with determined weight percentage amounts in the mine tailings; and processing the batch slurry through the provided facility, including a final curing step that produces the building structural material. Due to the chemical reaction that takes place in the casting stage, the production slurry changes from a fluid form to a quasi-solid form of the building material. The quasi-solid form expands and conforms to a mold shape and facilitates being cut into smaller units prior to curing. The autoclaved aerated cement, as produced and claimed, is of limited utility because the composition lacks plasticity and is therefore incapable of efficient subsequent reformation. Information regarding the material's permeability, porosity, and required curing time period are not disclosed. As previously stated, well known disadvantages associated with cement include high porosity and structural instability as a result of temperature and climate fluctuations.
U.S. Pat. No. 6,825,139 discloses a crystalline composition, a poly-crystalline product, an article of manufacture, and a related process utilizing coal ash as starting material. The process involves mixing coal ash particles with at least one glass forming agent and at least one crystallization catalyst, melting this combination to form a mixture, and cooling the resulting mixture to ambient temperature to form a homogenous, non-porous poly-crystalline product comprising SiO 2 , Al 2 O, CaO, Fe 2 O 3 , TiO 2 , MgO, Na 2 O, Li 2 O, CeO 2 , ZrO 2 , K 2 O, P 2 O 5 , Cr 2 O 3 , ZnO and MnO 2 . The poly-crystalline products are poly-crystalline materials obtained from glass compositions by means of catalysis crystallization and consisting from one to several crystalline mineralogical phases uniformly distributed in the remaining glass phase. Microstructure assessment, as revealed by electron microscopy, showed a dense glass-ceramic structure with crystal dimensions approximately 1 μm. The composition's mineralogical composition, as demonstrated by X-ray diffraction, revealed that the predominant crystalline phase is anorthite, whereas additional crystalline phases include albite and lithium disilicate. The glass density was found to be up to 2720 kg/m 3 ; the porosity less than 0.02%; and bending strength was up to 150 MPa. However, the composition is heated to temperatures that require addition of at least one crystallization catalyst to effect the various crystalline phases, and to that extent the composition, article and corresponding process are relatively cumbersome and prone to inaccuracy should mistakes occur during catalyst addition.
Bulk processing of relatively homogeneous mined mineral material has also resulted in the creation of numerous ceramic tile products of varying quality and durability. For instance, conventional ceramics produced by processing mixtures of natural mineral constituents and admixtures can be classified according to their glass content as non-vitreous, semi-vitreous, and vitreous. Non-vitreous ceramic, of which Dal-Tile is an example, is generally manufactured from clay, talc, and carbonate minerals, and has water absorption greater than about 7%. No fluxing minerals such as feldspar are used in these compositions. Non-vitreous Dal-Tile of this type has a water absorption of 13-14%, as measured by ASTM C373. This type of tile has virtually no glass content, and gets its structural integrity from solid-state reactions and sintering. Semi-vitreous ceramic, of which Balmor is an example, generally has some glass content and corresponding water absorption between about 4% and about 7%. This is a red body product, its color due to its natural iron content. Such bodies are often made of natural clay-containing earth mixtures which contain natural quartz and feldspar. The latter acts as a fluxing agent to produce a liquid phase during firing, said liquid phase converting to glass during cooling. Vitreous ceramic, including porcelain tile, of which Granitifiandre. Kashmir White is an example, has less than 4% water absorption. True porcelain products typically have water absorption values less than about 0.5%. These materials are primarily produced from the raw materials kaolinite clay, quartz, and feldspar. They have a high glass content (typically 20-30%), and are also characterized by a lack of crystalline phases that have precipitated from the melt during cooling. They often contain the mineral mullite (3Al 2 O 3 -2SiO 2 ) formed at elevated firing temperatures from solid state decomposition of the kaolinite raw material.
Commercially available ceramic-tile materials—non-vitreous
FIG. 1 is the scanning electron microprobe back-scattered electron (BSE) image of the non-vitreous commercial ceramic tile manufactured by Dal-Tile™. This BSE image illustrates the typical microfabric of this non-vitreous ceramic tile dominated by discrete flaky particles ( 1 and 2 ) that are cemented (sintered) with no apparent glass matrix. The Energy Dispersive X-ray (EDX) microchemical analysis spectra of the dominant flaky particles show a magnesium-silicate chemistry. This composition corresponds with the mineral “enstatite” (MgO—SiO 2 ) identified in the X-ray diffraction analysis (XRD) performed on this ceramic tile sample. The enstatite mineral phase did not “grow” or crystallize out of a melt, since none exists, but instead was formed as a high temperature pseudo-morphous solid state replacement mineral for an original largely talc feedstock material. Talc is a hydrated magnesium silicate mineral Mg 3 Si 4 O 10 (OH) 2 ).
Light colored (white) reaction rims ( 3 ) surround voids (black), some of which contain partially dissolved particles ( 4 ). EDX analysis indicates that the rims ( 3 ) possess a magnesium aluminum silicate chemistry that corresponds with the mineral cordierite (MgO—Al 2 O 3 —SiO 2 ) detected by XRD analysis. The partially dissolved particles in the center of some of the voids have a magnesium oxide chemistry typical of periclase. The abundance of this MgO material was too low to be detectable in XRD analysis.
Minor angular particles ( 5 ) with a silica chemistry corresponds to the composition of quartz (SiO 2 ) detected as a minor component in this ceramic tile by XRD analysis.
The abundant void space (black) illustrates the high porosity of this non-vitreous ceramic tile material ( 6 ). The absence of significant glassy matrix in this material causes poor grain-to-matrix bonding contact ( 7 ). Both of these physical properties contribute to greater water absorption, lower hardness and lower modulus of rupture (MOR—a measure of mechanical strength) determined for this ceramic tile.
Commercially Available Ceramic-Tile Materials—Semi-Vitreous
FIG. 2 is the scanning electron microprobe back-scattered electron (BSE) image of the Balmor™ semi-vitreous commercial ceramic tile. FIG. 2 illustrates the typical microfabric of this semi-vitreous ceramic tile comprised of partially to completely dissolved primary mineral grains. EDX analyses of these mineral grains revealed the chemical compositions, which correlate to the specific minerals identified by XRD analysis as being constituents of this tile material. These include potassium-feldspar ( 10 ), plagioclase feldspar ( 11 ), quartz ( 12 ) and goethite (Fe(OH) 2 ) ( 13 ).
These primary mineral grains are cemented by a semi-continuous amorphous glass matrix. The EDX microchemical analysis of two glassy matrix areas ( 14 and 15 ) shows that the particular ratios of the cations K, Na, and Ca in the two glassy areas appear to be similar to the two adjacent feldspar compositions (compare 10 with 14 and 11 with 15 ). This similarity indicates that glass compositions may vary with respect to the cation composition, and are influenced by the specific cation constituents within the adjacent mineral grains that melt or dissolve to form the glass matrix material.
FIG. 2 reveals that the glassy matrix of this semi-vitreous ceramic tile is semi-continuous resulting in a moderate degree of retained porosity 16 . This porosity is largely, but not completely, unconnected resulting in lower water absorption properties. The primary grains are not entirely bonded ( 17 ) to the glassy matrix which causes a reduction in the durability and hardness of the material.
FIG. 2 also shows no secondary crystallite minerals within the glassy matrix. No evidence is indicated that new crystalline mineral phases have precipitated from the melt during the cooling process.
Commercially available ceramic-tile materials—vitreous
FIG. 3 is the scanning electron microprobe back-scattered electron (BSE) image of the Granitifiandre Kashmir White vitreous porcelain ceramic tile. This BSE image illustrates the typical microfabric of this vitreous ceramic tile comprised of remnants of partially dissolved primary grains. The EDX microchemical analysis of some of these grains correlates with the XRD analysis to confirm that the mineralogy of this ceramic tile is dominated by quartz ( 20 ), plagioclase feldspar ( 21 ) and zircon ( 22 ).
FIG. 3 reveals that the quartz grain boundaries show evidence of significant dissolution ( 20 ) while the feldspar grains are severely to completely melted or dissolved ( 21 ). The minor zircon grains were evidently an admixture to achieve a mottled texture in the porcelain tile body (surface 22 ). The glassy matrix appears to be continuous, leaving only a few isolated voids or pores and producing low water absorption properties ( 23 ).
FIG. 3 also shows no apparent secondary crystallite minerals within the glassy matrix and suggests that no such secondary minerals formed from the melt. However, mullite—a mineral formed through solid state transformation from kaolinite—was identified in XRD analysis. Because of its typical needle-shaped crystal shape and very small particle size, its presence in this ceramic was not positively identified in the BSE analysis. The total atomic weight (density) of mullite may be too similar to the glass matrix rendering it indistinguishable from the glass.
As discussed above, inefficiencies involving conventional methods of processing waste minerals such as mine tailings, and the structural and compositional limitations inherent in conventional ceramic products—particularly with respect to porosity and corresponding water absorption, diminished hardness and low modulus of rupture—demonstrate that a dual need exists for: (1) an effective and efficient strategy to reclaim mineral wastes such as mine tailings at low cost and high safety; and (2) a low cost and easily manufactured non-clay vitreous synthetic rock material with superior, and heretofore collectively unavailable, characteristics including low porosity; impermeability without glazing; high-plasticity for subsequent reformation; and high strength and durability. The disclosed invention addresses these dual needs simultaneously.
BACKGROUND OF THE INVENTION
Mine tailings and mine reclamation efforts have evoked enormous environmental concerns in the United States and abroad. Tailings are waste products remaining in containment areas or discharged to receiving waters after metals are extracted from a particular site, and consist primarily of waste rock containing a variety of rock forming minerals, including as major constituent groups crystalline silica, feldspars and clay minerals; with minor constituent groups including carbonates, sulfates, sulfides and micas. Pollution issues associated with mine tailings relate to the structural integrity and stability of tailings containment areas and the potential for pollution impacts should containment failure occur. At the heart of these concerns is the pollution potential of mine tailings on ground and surface water, and correspondingly how such potential pollution affects people living in the immediate vicinity of tailings containment areas.
The need for effective mine reclamation strategies, and safe disposition of potentially hazardous mine tailings, is widely recognized in the mining and environmental industries alike. There is no legitimate doubt that disposing of mine tailings in a safe manner, as opposed to continually attempting their containment, is desirable from both an environmental safety and economic point of view. Likewise, other mineral waste materials raise similar environmental contamination concerns, and the need for their safe and effective disposition is also well acknowledged.
As far back as ancient Mesopotamia, researchers have located what they believe to be basalt rock slabs formed from silt. It is believed that inhabitants used the basalt rock as a main staple in the region for a variety of purposes, including pottery, architecture, writing materials, art objects and tools. In simulation studies to recreate the basalt rock from silt, researchers were able to approximate the composition and texture of the basalt rock using local alluvial silt as raw starting material, and heating the material within a defined temperature range over a sustained time period. The resulting basalt rock was characterized by matted clinopyroxene crystals embedded in a glassy matrix, with starting material remnants either rarely appearing in, or completely absent from, the final basalt rock. The basalt rock was most likely of limited strength, as it lacked an aggregate microstructure. Due to the observed presence of many large pores, some as big as 3 mm, the basalt had high water absorption, likely well in excess of 7%.
In more recent examples of waste materials, fly ash and bottom ash from burning coal for electric power are largely incombustible residuals formed from inorganic minerals in coal. Roughly hundreds of million tons is produced every year in the USA alone. Fly ash and bottom ash are also produced in waste incinerators and biomass-fueled power plants. Slag mineral waste materials result from metal processing operations. Quarry and dredging operations often produce silicate waste materials such as fines or slimes that must be disposed of in a safe manner.
Relatively pure mineral materials (kaolinite clay, feldspar, quartz, talc, etc.) have conventionally been used to manufacture a variety of ceramic materials with varying compositions and degrees of quality. As previously described, non-vitreous Dal-Tile, semi-vitreous Balmor Tile and vitreous Granitifiandre Kashmir White tile represent a very few. However, these and a vast array of other conventional ceramic products (ceramic tile, dinnerware, sanitaryware, etc.) are typically manufactured by methods that rely on the plasticity and bonding (in the unfired state) of clay—largely kaolinite—and generally use relatively pure raw materials. As previously stated, conventional ceramics also demonstrate a number of undesirable characteristics, including—moderate to high porosity and water absorption, low hardness and strength, and the absence of secondary crystallite formation upon cooling, which contributes to product durability. Also, in the manufacture of conventional ceramics, considerable concern is placed on the quality and purity of the raw material ingredients. Further, contaminants in the raw materials can cause considerable damage to the quality of the conventional product in terms of structural integrity and defects in the cosmetic properties. Surprisingly, Applicant's process and composition are tolerant of higher concentrations of many materials that are considered contamination in conventional ceramics manufacture. Such materials include iron, magnesium, manganese, sulfur, and their compounds.
The need exists in the environmental clean-up industry to develop an effective and efficient strategy for reclaiming mines, disposing of mine tailings after mineral extraction at the mine is complete, disposing of mine development rock, disposing of fly ash and bottom ash from power plants or incinerators, disposing of slag, and disposing of fines or slimes. An equally significant need exists in the synthetic rock industry to produce a low porosity, easily manufactured, low absorption vitreous tile in a cost effective and relatively fast manner.
SUMMARY OF THE INVENTION
The applicant's invention provides a crystalline and glass composition derived from processing raw mine tailings and similar waste materials, which can be used to create valuable articles of manufacture and products for a wide variety of uses, particularly, but without limitation, in the commercial and residential construction industry, for example floor, wall, and roof tile, brick, blocks, siding, panels, pavers, countertops, aggregates for road base, and other building materials. The unique composition comprises a clast phase, a glass phase, and a crystalline phase. Said clast phase is further comprised of mineral grains, mineraloid grains, glass spherules, or rock fragments, any of which may have been partially melted, or partially dissolved, or partially transformed by chemical reaction. Said glass phase provides a matrix that cements together the clasts. Said crystalline phase is fully enveloped by the glass phase, having formed by growth from the melt. The unique composition of clasts fused together by a unique glass phase, which further comprises a newly formed crystalline phase, is characterized by a microscopic aggregate breccia (synthetic rock/glass matrix) structure with superior physical and structural characteristics, including low porosity, low absorption, increased strength and durability, retained plasticity to facilitate reformation subsequent to initial processing, and readily distinguishable chemical attributes in comparison to conventional synthetic rock materials, as demonstrated by scanning-electron-microprobe analysis.
The glass phase (glass matrix) is created as a result of partially melting a suite of original raw mineral constituents, which may include feldspar, quartz and mineral materials found in a wide variety of rock types, and which further may be present as individual mineral grains (monomineralic) or as rock fragments (polymineralic). After an optimal melting period, the resulting glass matrix is cooled over an optimal cooling period, and during the cooling period unique silicate and non-silicate minerals with varying proportions of iron, magnesium, calcium and sulfur crystallize from the melt to form small crystallites distributed throughout the glass matrix. Importantly, the newly formed secondary crystallites include specific inosilicate, tectosilicate and sulfate compounds that are not present in the starting raw material, and are not found in commercially-available ceramics in the same fashion. Occasionally, some of these minerals may be found in commercially-available ceramics; however those minerals are not secondary crystallites formed from a melt phase, but rather are remnants of the raw starting material. The specific minerals formed in applicants ceramic materials are influenced by the unique chemistry of the waste mineral feedstock materials such as tailings, ash, etc.
Inosilicates are single-chain and double-chain silicate minerals. The Pyroxene Group of inosilicates comprises single-chain, non-hydrated ferromagnesian chain silicates. The Amphibole Group of inosilicates comprises double-chain, hydrated ferromagnesian chain silicates. Wollastonite is a calcium silicate mineral in the inosilicate group.
Tectosilicates are framework silicate minerals, including minerals such as quartz and the Feldspar Group. Plagioclase feldspar is a solid solution series of feldspar minerals with varying amounts of sodium and calcium.
Sulfate minerals are a group of minerals containing sulfur. Gypsum and anhydrite are calcium sulfates, with anhydrite forming the dehydrated form and gypsum the hydrated form.
Pyroxenes, particularly enstatite and hypersthene (the iron containing version of enstatite), as well as augite, diopside, bronzite, and pigeonite, are not conventionally present in raw starting materials, and have not been detected in vitreous, semi-vitreous or porcelain ceramics. Rather, pyroxenes have been detected, via X-Ray Diffraction analysis (XRD) and Scanning Electron Microprobe analysis (microprobe) using an Energy Dispersive X-ray Spectrometer (EDS), only in high porosity ceramics, such as the non-vitreous ceramic Dal-Tile discussed above. However, microprobe analysis reveals that those pyroxenes in the non-vitreous ceramic have a morphology that indicates to one skilled in the art that they are the result of solid-state chemical reactions rather than crystallization from a melt phase. Conversely, amphiboles, particularly in the form of hornblende, have been detected in raw mine rock materials, but not in processed material, because these compounds do not survive high temperature processing as a result of dehydration and bond degradation during the heating process.
Wollastonite and plagioclase are common ingredients of some non-vitreous conventional ceramics to achieve specific ceramic types and properties. However, wollastonite and plagioclase have not been detected using microprobe analysis and EDS techniques as a newly crystallized phase in conventional ceramics, rather they appear as sintered primary mineral grains.
Anhydrite and/or gypsum are not conventionally present in raw starting materials, and have not been detected in conventional non-vitreous, semi-vitreous or vitreous ceramics.
Applicant's compositions and articles of manufacture comprise both original tailings fragments as well as newly formed mineral phases, which renders them compositionally distinct not only from the raw mine tailings starting material, but—more importantly—from conventional synthetic rock compositions and corresponding articles of manufacture. A key compositional distinction between the raw starting material, applicant's compositions and articles, and conventional synthetic rock compositions is the presence or absence of inosilicate minerals, specifically pyroxenes, wollastonite, tectosilicates, specifically plagioclase feldspar, and sulfates, specifically anhydrite. As more fully set forth below, applicant's compositions and articles contain pyroxene inosilicates, newly formed plagioclase, wollastonite and anhydrite, which heretofore have not been detected in low porosity, vitreous synthetic rock materials. Specific pyroxene minerals that may form in this synthetic rock may include, but are not limited to, one or more of the following: augite, diopside, hypersthene, pigeonite, bronzite and enstatite.
In addition, applicant's invention employs a unique heating and cooling strategy, which completely obviates the need for the addition of crystallization catalysts. That is, heating of the raw material to a temperature at which some, but not all, of the components of the raw material begin to at least partially melt. At these temperatures, a liquid phase is created that can flow to coat individual aggregate particles, bind them together, and fill in void spaces. The liquid phase can also begin to dissolve additional solid material. Upon cooling at reasonable unquenched rates, this liquid phase can partially crystallize without the need for addition of nucleation additives because, due to partial melting, there are already present solid surfaces to initiate crystallization. Mechanical pressure to squeeze the material at temperature can help to distribute the liquid phase among the various solid surfaces and increase binding. Vacuum to remove gas from void spaces can help to eliminate resistance to filling in the voids with the liquid phase.
Typically the first components of the raw material to liquefy are glass particles or feldspars, many of which liquefy at temperatures of approximately 1050 to 1300 degrees C. Preferably, the raw material comprises glass or feldspar that becomes liquid at temperatures in the range of 1100 to 1200 degrees C. Cooling from these temperatures preferably takes place at a rate slow enough to allow crystallization to occur, preferably about 1 to 50 degrees C. per minute, more preferably about 5 to 20 degrees C. per minute, and most preferably about 10 degrees C. per minute when cooling is initiated from the peak temperature for the first few hundred degrees of cooling. Cooling at a maximum rate of 10 degrees C. per minute is also especially preferred as the material passes through the temperature range of 600 to 500 degrees C., to avoid fracture due to the associated volume change of the beta-to-alpha phase transition of any quartz that may be present in the material.
In the embodiments and examples of the present invention that follow, an amount of mine tailings, for example Historic Idaho-Maryland Mine Tailings (“HIMT”), containing both rock fragments and individual mineral grains, is heated in a forming chamber to an optimal temperature, preferably in the range of 1100 to 1200 degrees C., and thereby partially melted over an optimal period of time, preferably about 0.5 to 6 hours. During the partial melting process, the HIMT raw material is simultaneously exposed to pressure modification, which preferably is the application of mechanical force to the material in the range of 1 to 200 psi, and which further may also be the application of vacuum to reduce the absolute pressure to within the range of about 1 to 600 mbar in order to remove interstitial gas phase.
Heating the HIMT raw material with pressure modification results in a partially melted matrix, which is then allowed to cool over an optimal period of time. During the cooling period, newly formed mineral crystallites with varying proportions of silicon, aluminum, iron, magnesium, calcium, and sulfur crystallize from the initial raw material melt to form small crystallites distributed throughout a glass matrix. As previously stated, the invention does not employ added crystallization catalysts or nucleating agents to facilitate the crystallization process.
The newly formed crystallized minerals occurring in the glass matrix comprise a combination of minerals from the Pyroxene Group, Plagioclase Feldspar Group and Sulfate Group. Morphological characteristics of the newly crystallized minerals indicate their secondary growth from the initial raw material melt, as opposed to from a solid state glass reaction. Most notably, these secondary growth indicators include the newly formed minerals' generally uniform size, crystalline morphology and uniform composition throughout the glass matrix.
In one embodiment, the invention provides a vitreous, non-porous, impermeable polycrystalline composition comprising an amount of clasts, an amount of glass matrix, and an amount of at least one secondary crystalline phase. Said clasts comprise grains of single minerals, such as quartz, or rock fragments, or unmelted glass fragments, or mineraloid grains. Said glass matrix is distributed between the clasts, bonding to them and filling in the nearly all of the interstitial space. Said at least one secondary crystalline phase is contained within the glass matrix, and is comprised of crystals formed from a melt with a mineral composition selected from the group consisting of ferromagnesian minerals, pyroxenes (for example, clinopyroxene, orthopyroxene, augite, diopside, hypersthene, pigeonite, bronzite, enstatite), illmanite, rutile, wollastonite, cordierite, and anhydrite.
In one embodiment, the invention provides a method for processing mine tailings resulting in a vitreous, non-porous, impermeable polycrystalline composition. Said method comprises air drying a sampling of mine tailings to less than 3% moisture; screening the mine tailings to remove material larger than 516 microns; and calcining the mine tailings in air at approximately 900 degrees C. The mine tailings are then mechanically compacted in a tube with an approximate pressure of 350 psi at an approximate temperature of 1130 degrees C. for approximately 60 hours, and subsequently cooled at a rate of approximately 1 to 3 degrees C. per minute, forming said composition, comprising a clast phase, a glass phase, and at least one crystalline phase. Said clast phase comprises grains of single minerals, such as quartz, or rock fragments. Said glass phase is distributed between said clast phase, bonding to clast particles and filling in nearly all surrounding interstitial space. Said at least one crystalline phase is contained within said glass phase, and comprises crystals formed from a melt with a mineral composition consistent with minerals selected from the group consisting of bronzite, augite and pigeonite.
In another embodiment, the invention provides a method for processing mine tailings resulting in a vitreous, non-porous, impermeable polycrystalline composition. Said method comprises drying a sampling of mine tailings to less than 3% moisture; screening the mine tailings to remove material larger than 516 microns; and calcining the mine tailings in air at approximately 900 degrees C. The mine tailings are then mechanically compacted in a tube with an approximate pressure of 300 psi at an approximate temperature of 1140 degrees C. for approximately 6 hours, and subsequently cooled at a rate of approximately 10 to 20 degrees C. per minute, forming said composition, comprising a clast phase, a glass phase, and at least one crystalline phase. Said clast phase comprises grains of single minerals, such as quartz, or rock fragments. Said glass phase is distributed between said clast phase, bonding to clast particles and filling in nearly all surrounding interstitial space. Said at least one crystalline phase is contained in said glass phase and comprises crystals formed from a melt with a mineral composition consistent with minerals selected from the group consisting of bronzite, augite, pigeonite, anhydrite and ilmanite.
In another embodiment, the invention provides a method for processing metavolcanic mine development rock resulting in a vitreous, non-porous, impermeable polycrystalline composition. Said method comprises air drying a sampling of the development rock to less than 3% moisture; and screening the development rock through a 516 micron screen. Development rock powder is then processed through the apparatus described in U.S. Pat. No. 6,547,550 (Guenther) at a temperature of approximately 1160 degrees C., with mechanical pressure oscillating between approximately 30 psi and 160 psi for a defined time period, in a partial vacuum atmosphere for approximately 60 minutes, and subsequently cooled at an approximate rate of 5 to 15 degrees C. per minute, forming said composition, comprising a clast phase, a glass phase and at least one crystalline phase. Said clast phase comprises polymineralic and monomineralic clasts. Said glass phase is distributed between said clast phase, bonding to clast particles and filling in nearly all surrounding interstitial space. Said at least one crystalline phase is contained in said glass phase and comprises crystals formed from a melt with a mineral composition consistent with minerals selected from the group consisting of augite, pigeonite, maghemite and ilmanite.
In another embodiment, the invention provides a method for processing coal fly ash resulting in a vitreous, non-porous, impermeable polycrystalline composition. Said method comprises air drying a sampling of the coal fly ash to less than 3% moisture; screening the coal fly ash with a 516 micron screen; and thereafter calcining the coal fly ash. The coal fly ash is then mechanically compacted at an approximate pressure of 300 psi in a tube at an approximate temperature of 1115 degrees C. for approximately 10 hours, and subsequently cooled at an approximate rate of 10 to 20 degrees C. per minute, forming said composition, comprising a clast phase, a glass phase, and at least one crystalline phase. Said clast phase comprises remnant clasts from the original feedstock constituents. Said glass phase is distributed between said clast phase, bonding to clast particles and filling in nearly all surrounding interstitial space. Said at least one crystalline phase is contained in said glass phase and comprises crystals formed from a melt with a mineral composition consistent with minerals selected from the group consisting of wollastonite, plagioclase feldspar, anhydrite, and calcium sulfate.
In another embodiment, the invention provides a method of processing waste materials selected from the group consisting of mine tailings, waste rock, quarry waste, slimes, fly ash, bottom ash, coal ash, incinerator ash, wood ash, and slag, resulting in a vitreous, non-porous, impermeable polycrystalline composition. Said method comprises subjecting the waste materials to a screening apparatus; conveying the waste materials from said screening apparatus to a heated rotating chamber for chemical transformation; conveying the waste materials from said heated rotating chamber to a second heated chamber optionally fixed with a vacuum; conveying the waste materials from said second heated chamber to a third heated chamber positioned within a heating element; applying pressure to the waste materials in said third heated chamber forming a hybrid rock; extruding said hybrid rock through a die device and removing said hybrid rock from said third heated chamber for subsequent use or further modification.
The benefits, advantages and surprising discoveries resulting from the present invention are, in a word, remarkable. First and foremost, a surprising discovery regarding applicant's invention is the presence of pyroxene inosilicates in the final composition and corresponding articles. Heretofore, pyroxene mineral compounds have not been detected in vitreous, low-porosity, low absorption synthetic rock materials such as applicant's present invention. Rather, pyroxenes have only been conventionally detected in highly porous, non-vitreous materials.
Also surprising is the fact that applicant's invention achieves maximum crystallization without the addition of crystallization catalysts or other nucleating agents. The raw material in applicant's invention is not heated beyond its melting point, but rather is only partially melted, which preserves crystallization nuclei sites already present in the glass matrix. Conversely, conventional synthetic rock compositions must employ crystallization catalysts to facilitate crystal formation because corresponding raw materials are heated to above their melting point and completely melted to a homogenous state during processing, which destroys potential crystallization sites. Conventional crystallization catalysis is required to provide a site for crystallization.
Yet another surprising discovery regarding applicant's invention is that the invention's glass matrix can comprise various amounts of glass, but that with less than approximately 20% glass the composition achieves impermeability. Conventional low or non-permeable synthetic rock materials require a high glass content to achieve impermeability.
The invention also has the advantage of providing compositions of matter comprising crystalline particles within a glass-binding liquid matrix, which allows the compositions to maintain a significant amount of plasticity at high temperature, unlike conventional clay tile. With this heightened plasticity level the compositions can, while initially heated or re-heated, be pressed, rolled or injected into other shapes and a variety of useful products after initial preparation. For instance, fine grained versions of the solid compositions can be pressed into aggregates and cobbles for a variety of construction uses, including for use in cement, road base and cobblestones. Alternatively, commonly known abrasives, such as silica carbide, quartz and garnet, can be added to the composition for subsequent use in sanding blocks and grinding wheels.
Another advantage of the present invention is that the solid compositions and corresponding articles of manufacture are impermeable without the need for glazing. The invention's impermeability is directly related to the fact that, unlike conventional synthetic rock materials, the composition and articles contain essentially zero open porosity, due to the continuous glass matrix structure surrounding crystallites distributed throughout therein. With the exception of certain rare vitreous expensive clay products, such as porcelain, conventional synthetic rock and ceramic products require glazing to achieve impermeability.
As previously stated, applicant's invention contains virtually zero open porosity, which results in less porous and more impermeable articles as compared to conventional ceramic materials. Surprisingly, voids (closed pores) may be induced in applicant's invention to result in a lighter weight construction-type material, without compromising the invention's impermeable characteristics.
Other aspects and alternatives or preferred embodiments of the invention exist. They will become apparent as the specification proceeds.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a micrograph obtained from scanning electron microprobe analysis of commercially available (Dal-Tile) non-vitreous ceramic tile.
FIG. 2 is a micrograph obtained from scanning electron microprobe analysis of commercially available (Balmor) semi-vitreous ceramic tile.
FIG. 3 is a micrograph obtained from scanning electron microprobe analysis of commercially available (Granitifiandre, Kashmir White) vitreous ceramic tile.
FIG. 4 is a micrograph obtained from scanning electron microprobe analysis of an article of manufacture resulting from Applicant's method of processing mine tailings, including an illustration of the article's composition.
FIG. 5 is a micrograph obtained from scanning electron microprobe analysis of an article of manufacture resulting from Applicant's method of processing mine tailings, including an illustration of the article's composition.
FIG. 6 is a micrograph obtained from scanning electron microprobe analysis of an article of manufacture resulting from Applicant's method of processing mine development rock, including an illustration of the article's composition.
FIG. 7 is a micrograph obtained from scanning electron microprobe analysis of an article of manufacture resulting from Applicant's method of processing coal fly ash, including an illustration of the article's composition.
FIG. 8 is a schematic flowchart depicting an apparatus and method of processing waste mineral materials.
DETAILED DESCRIPTION OF THE INVENTION
The First Embodiment
This embodiment is an apparatus and process for processing mine tailings employing a slow cooling schedule, which results in Applicant's composition and corresponding articles of manufacture.
TABLE 1
Composition of some feed materials
Idaho-Maryland
Idaho-Maryland
mine tailings
development rock
coal fly ash
mass %
mass %
mass %
loss on ignition
11.29
4.19
19.1
SiO 2
55.6
48.7
39.84
Al 2 O 3
9.89
14.8
13.23
Na 2 O
1.99
3.40
1.77
MgO
5.01
8.17
1.66
K 2 O
1.52
0.33
0.67
CaO
7.03
9.23
19.52
Fe 2 O 3
5.12
9.72
2.62
MnO
0.11
0.15
0.02
P 2 O 5
0.18
0.12
0.42
TiO 2
0.67
0.93
0.62
C (inorganic)
0.23
0.55
5.16
C (organic)
2.33
0.02
1.65
C (total)
2.56
0.57
6.81
S
0.41
0.16
3.86
EXAMPLE 1
A sample of tailings from the Idaho-Maryland gold mine, having the general composition shown in Table 1, was air-dried to less than 3% moisture and screened to remove material larger than 516 microns (30 mesh). The raw tailings material was calcined in air at 900 degrees C. Following calcining, the material, without additives, was mechanically compacted using a ram at a pressure of approximately 350 psi within a nitride-bonded-silicon-carbide process tube at a temperature of 1130 degrees C. for an extended period of time, approximately 60 hours at temperature. The material was then slowly cooled, at a rate of 1 to 3 degrees C. per minute, forming a synthetic rock hybrid material, which was then removed from the process tube. Test specimens of the resulting synthetic rock hybrid material had an average modulus of rupture of about 85 MPa (12320 psi), and an average water absorption of about 0.3% as determined by method ASTM C373. Other resulting data are shown in Table 2.
TABLE 2
Physical properties of example synthetic rock hybrid materials.
Ex. 1
Ex. 2
Ex. 3
Ex. 4
modulus of rupture (psi)
12320
6060
9280
8230
apparent porosity (%) ASTM
0.7%
6.8%
2.3%
1.8%
C373
water absorption (%) ASTM
0.3%
3.2%
0.8%
0.7%
C373
apparent specific gravity ASTM
2.67
2.32
2.83
2.53
C373
bulk density (g/cm3) ASTM
2.65
2.16
2.76
2.49
C373
FIG. 4 is the scanning electron microprobe back-scattered electron (BSE) image of this synthetic rock hybrid material of Idaho Maryland mine tailings feedstock. FIG. 4 illustrates the three characteristic phases typical of the unique microfabric of this synthetic rock material. These three phases include clasts (partially dissolved remnant primary grains of the tailings feedstock); a glass phase derived from the partial melting of primary mineral grains; and a secondary crystalline phase comprised of similarly sized crystallites that occur in the glass phase. The latter secondary minerals crystallized from the melt prior to cooling and formation of the glass phase. FIG. 4 shows a remnant primary quartz grain with rounded edges indicating dissolution of its formerly angular grain boundaries ( 31 ). The nearly complete melting of most other primary mineral constituents of the original feedstock components such as feldspar leaves little evidence of their existence in this synthetic rock other than mottled areas that retain the chemical signature of the parent mineralogy ( 32 ).
The glass phase ( 33 ) with an aluminosilicate composition contains trace amounts of cations such as potassium, calcium, sodium, magnesium, and iron ( 33 ). EDS microchemical analysis of the glass throughout the ceramic indicates that the glass composition is heterogeneous and varies with respect to the aluminum:silicon ratio as well as the trace cation content ( 34 ).
The newly formed (secondary) crystallite comprises the crystalline phase of this synthetic rock. The longer processing time resulted in secondary crystallites comprising 40-50% of the volume of this material. The crystallites appear in two recognizable morphologies each with distinct chemistries as determined by EDS. Some crystallites appear in narrow lath and skeletal shapes and occur singly and in clusters ( 35 ). Crystallites of this morphology uniformly possess a chemistry most similar to the bronzite species of pyroxene having high magnesium but low calcium and iron contents ( 35 ). The size of the lath shaped crystallites ranges from 1 to 3 μm in width and from 5 to 25 μm in length.
The other common morphology of crystallites is an equant blocky shape similarly occurring singly and in clusters ( 36 ). This latter crystallite morphology is associated with calcium to iron ratios similar to augite or pigeonite varieties of pyroxene having high calcium but low iron contents. The size of these blocky crystallites ranges from 4 to 15 μm.
The continuous glass phase in this synthetic rock material leaves widely spaced isolated voids with little or no communication between them resulting in very low absorption values ( 37 ).
The Second Embodiment
This embodiment is a method of processing mine tailings employing a fast cooling schedule, which results in Applicant's composition and corresponding articles of manufacture.
EXAMPLE 2
A sample of tailings from the Idaho-Maryland gold mine, having the general composition shown in Table 1, was air-dried to less than 3% moisture and screened to remove material larger than 516 microns (30 mesh). The raw tailings material was calcined in air at 900 degrees C. Following calcining, the material, without additives, was mechanically compacted using a ram at a pressure of approximately 300 psi within a nitride-bonded-silicon-carbide process tube at a temperature of 1140 degrees C., with a residence time of approximately 6 hours at temperature. The material was then extruded through a rectangular die (15.2 by 1.3 cm) with a land length of 3.5 cm, and subsequently cooled at a rate of about 10 to 20 degrees C. per minute, forming a synthetic rock hybrid material. Test specimens of the resulting synthetic rock hybrid material had an average modulus of rupture of about 42 MPa (6060 psi), and an average water absorption of about 3.2% as determined by method ASTM C373. Other resulting data are shown in Table 2.
FIG. 5 shows the scanning electron microprobe back-scattered electron (BSE) image of the resulting synthetic rock hybrid material. FIG. 5 illustrates the three characteristic phases typical of the unique microfabric of this synthetic rock material. These three phases include clasts (partially dissolved remnant primary grains of the tailings feedstock); a glass phase derived from the partial melting of primary mineral grains; and a secondary crystalline phase comprised of similarly sized crystallites enveloped in the glass phase. The latter secondary minerals crystallized from the melt during cooling, likely prior to the formation of the glass phase. FIG. 5 shows a remnant primary quartz grain with rounded edges indicating dissolution of its formerly angular grain boundaries ( 41 ). The nearly complete melting of most other primary mineral constituents of the original feedstock components leaves little evidence of their existence in this synthetic rock.
The glass phase ( 42 ) with an aluminosilicate composition contains trace amounts of cations such as potassium, calcium, sodium, magnesium, and iron ( 42 ). EDS microchemical analysis of the glass throughout the ceramic indicates that the glass composition is heterogeneous and varies with respect to the aluminum:silicon ratio as well as the trace cation content ( 43 ).
Four newly formed secondary crystalline phases are apparent in this synthetic rock material including two distinct pyroxene types, anhydrite and ilmanite. Pyroxene crystallites appear in two morphologies each with distinct chemistries as determined by EDS. One pyroxene crystallite morphology is a narrow lath shape ( 44 ). The lath type pyroxenes uniformly possess a chemistry most similar to the bronzite species having high magnesium but low calcium and iron contents ( 44 ). The crystallite sizes range from 1.5 to 3 μm in width and from 5 to 50 μm in length. The faster processing time to produce this material (relative to Example 1) prevented complex cluster development of the crystallites. Other pyroxene crystallites occur with an equant blocky shaped morphology ( 45 ). This latter type pyroxene occurs singly and in simple clusters. This latter pyroxene crystallite morphology is associated with calcium to iron ratios similar to augite or pigeonite varieties with high calcium but low iron contents. The blocky crystallites range from 1 to 5 μm.
Sulfur in this synthetic rock has combined with calcium to form crystallite clusters of anhydrite ( 46 ). Individual crystallites within the clusters range from 2 to 7 μm in size.
Small similarly sized crystallites of ilmanite (iron titanium oxide) of 1 to 5 μm in size appear randomly arranged in the glassy matrix ( 47 ).
The continuous glass phase in this synthetic rock material leaves few and widely spaced isolated voids ( 48 ) with little or no communication between them, resulting in very low absorption values.
The Third Embodiment
This embodiment is a method of processing metavolcanic mine development rock employing a fast cooling schedule, which results in Applicant's composition and corresponding articles of manufacture.
EXAMPLE 3
A composite of drill-core samples taken from metavolcanic (andesite, dacite, diabase, and others) rock from the Idaho-Maryland mine (“development rock”) was air-dried to less than 3% moisture, and ground to a size fine enough to pass 100% through a 516-micron (30-mesh) screen. The development rock powder had a composition as shown in Table 1. The development rock powder, without additives, was processed through the apparatus described in U.S. Pat. No. 6,547,550 (Guenther) at a temperature of 1160 degrees C., with a mechanical pressure oscillating between about 160 psi and 30 psi with a period of oscillation of 10 minutes, in a partial vacuum atmosphere (about 170 mbar absolute pressure), with a residence time of about 60 minutes before extruding the consolidated plug of synthetic rock hybrid material. Following the extrusion, the plug was cooled at a rate of about 5 to 15 degrees C. per minute. Test specimens of the resulting synthetic rock hybrid material had an average modulus of rupture of about 64 MPa (9280 psi), and an average water absorption of about 0.8% as determined by method ASTM C373. Other resulting data are shown in Table 2.
FIG. 6 is the scanning electron microprobe back-scattered electron (BSE) image of the resulting synthetic rock material from composite Idaho Maryland development rock feedstock. FIG. 6 illustrates the three characteristic phases typical of the unique microfabric of this synthetic rock material that collectively comprise an aggregate (or breccia) arrangement. These three phases include partially dissolved remnant primary grains of the original metavolcanic feedstock constituents; a glass phase derived from the partial melting of primary mineral grains; and secondary crystalline phases comprised of similarly sized crystallites enveloped in the glass phase. The latter secondary minerals crystallized from the melt during cooling, likely prior to the formation of the glass phase. FIG. 6 shows numerous remnant grains of a variety of primary constituents forming a relatively coarse clasts fraction. These primary lithic grains include polymineralic metavolcanic rock fragments ( 51 ) and monomineralic mineral grains ( 52 ). Specific minerals that occur either in monomineralic grains comprised of a single mineral or polymineralic rock fragments comprised of multiple minerals include plagioclase feldspar ( 53 ); pyroxene ( 54 ); and remnants of degraded chlorite ( 55 ). Other primary minerals inherited from the feedstock constituents that also occur but not illustrated in FIG. 6 include sphene, quartz and hematite.
The partial melting of feldspar ( 53 ) occurring in the metavolcanic feedstock contributes to the formation of a melt phase that created a glass matrix upon cooling ( 56 ). The rounded feldspar grain margins indicate dissolution or melting of its formerly angular grain boundaries. The glass phase ( 56 ) with an aluminosilicate composition contains trace amounts of cations such as potassium, calcium, sodium, magnesium, and iron. EDS microchemical analysis of the glass throughout the ceramic indicates that the glass composition is heterogeneous and varies with respect to the aluminum:silicon ratio as well as the trace cation content ( 57 ).
FIG. 6 illustrates the formation of the dominant secondary crystalline phase that crystallized from the melt. Clusters of pyroxene crystallites appear in various locations enveloped by the glass phase ( 58 ). The individual pyroxene crystallites within the clusters possess an equant blocky morphology with calcium to iron ratios similar to augite or pigeonite varieties. Other secondary minerals that crystallized from the melt but not illustrated in FIG. 6 include maghemite (spinel group) and ilmanite (iron titanium oxide).
The continuous glass phase of this synthetic rock material envelops nearly the entire grain margin of the clasts resulting in widely spaced isolated voids ( 59 ). There is little or no communication between the isolated voids resulting in the very low absorption values determined for this synthetic rock hybrid material.
The unique structural attribute of this synthetic rock material is the aggregate breccia microfabric created by the three important components that includes 1) the primary remnant clasts, 2) the glass phase, and 3) the secondary crystallite phase. This aggregate breccia structural arrangement of components (or constituents) creates a strong aggregate microfabric with superior strength and durability properties unique to this synthetic rock material.
The Fourth Embodiment
This embodiment is a method of processing coal fly ash employing a fast cooling schedule, which results in Applicant's composition and corresponding articles of manufacture.
EXAMPLE 4
Coal fly ash material was obtained from a coal power plant, specifically Valmy train 2 in Winnemucca, Nev. The composition of the raw material is shown in Table 1. The material was air-dried to less than 3% moisture, and screened to pass 100% through a 516-micron (30-mesh) screen. Following calcining, the calcined coal fly ash material, without additives, was mechanically compacted using a ram at a pressure of approximately 300 psi within a nitride-bonded-silicon-carbide process tube at a temperature of 1115 degrees C., with a residence time of approximately 10 hours at temperature. The material was then extruded through a cylindrical die, and subsequently cooled at a rate of about 10 to 20 degrees C. per minute, forming a synthetic rock hybrid material. Test, specimens of the resulting synthetic rock hybrid material had an average modulus of rupture of about 57 MPa (8230 psi), and an average water absorption of about 0.7% as determined by method ASTM C373. Other resulting data are shown in Table 2.
FIG. 7 is the scanning electron microprobe back-scattered electron (BSE) image of the synthetic rock material fabricated from coal fly ash waste material feedstock. FIG. 7 illustrates the three characteristic phases typical of the unique microfabric of this synthetic rock material that collectively comprise an aggregate structural arrangement. These three phases include clasts of partially dissolved remnant primary grains of the original fly-ash feedstock constituents; a glass phase derived from the partial melting of primary mineral and fly-ash grains; and secondary crystalline phases comprised of similarly sized crystallites enveloped in the glass phase. The latter secondary minerals crystallized from the melt during cooling, likely prior to the formation of the glass phase. FIG. 7 shows remnant grains of primary constituents that remain in this synthetic rock including quartz ( 61 ) and fly-ash glass spherules ( 62 ).
The partial melting of fly-ash glass spherules—the dominant feedstock constituent—created a melt phase that formed a continuous glass matrix upon cooling ( 63 ). The glass phase ( 63 ) with an aluminosilicate composition contains trace amounts of cations such as potassium, calcium, sodium, magnesium, and iron. EDS microchemical analysis of the glass throughout the ceramic indicates that the glass composition is heterogeneous and varies with respect to the aluminum:silicon ratio as well as the trace cation content ( 64 ).
FIG. 7 illustrates the formation of up to four secondary crystalline phases that crystallized from the melt during the cooling process. These secondary crystalline phases include: clusters of wollastonite crystallites ( 65 ) some of which nucleated on remnant primary quartz grains ( 61 ); lath-shaped plagioclase feldspar ( 66 ) and pyroxene ( 67 ) crystallites randomly distributed in the glass phase; and blocky anhydrite crystallites (calcium sulfate) not shown in FIG. 7 . The anhydrite phase is a major component of this synthetic rock material and serves as a major receptacle for the sulfur that was a dominant constituent of the coal fly-ash waste material.
Individual wollastonite crystallites range in size from 1 to 6 μm. The lath shaped plagioclase and pyroxene crystallites range from 1 to 5 μm in width and 2 to 15 μm in length. The larger blocky anhydrite phenocrysts are a size that can be resolved with the polarized light microscope with typical sizes ranging from 10 to 70 μm.
The continuous glass phase of this synthetic rock material envelops the entire grain margin of the primary and secondary mineral grains resulting in few if any isolated voids ( 68 ). The predominant void space in this synthetic rock was inherited and associated with the primary fly-ash spherules ( 69 ). There is little or no communication between any of the isolated voids resulting in the very low absorption values determined for this synthetic rock material.
The unique structural attribute of this synthetic rock material is the aggregate breccia microfabric created by the three important components that includes 1) the primary remnant clasts, which in this example include mineral grains and mineraloid grains such as glassy fly-ash spherules, 2) the glass phase, and 3) the secondary crystallite phase. The cluster development of the large wollastonite crystallites the crystallized around primary quartz grains contributes to the coarse aggregate fraction ( 65 ). This aggregate breccia structural arrangement of components (or constituents) creates a strong aggregate microfabric with superior strength and durability properties unique to this synthetic rock material.
The Fifth Embodiment
This embodiment is a method of processing waste mineral materials such as mine tailings, ash, slag, slimes, and the like, which results in Applicant's composition and corresponding articles of manufacture.
Referring to FIG. 8 , raw material for synthetic hybrid rock manufacture 100 , may be for example mine tailings, waste rock, quarry fines, slimes, fly ash, bottom ash, coal ash, incinerator ash, wood ash, slag, or blends of these materials with each other or with pure ceramic feed materials such as clay, feldspar, quartz, talc, and the like. Silicate waste materials are particularly well-suited for use as raw material. Raw material 100 is delivered to screening apparatus 120 , which has an outlet 121 for oversize particles 122 with a size larger than a predetermined screen opening size, and which further has an outlet 123 for undersize particles 124 with a size smaller than a predetermined screen opening size. Oversize particles 122 may be recycled to screening apparatus 120 via a grinding process (not shown), or disposed of.
Undersize particles of raw material 124 are conveyed to a hopper 131 of rotary calciner 130 . Feed auger 137 is driven, for example by motor 136 , and particulate raw material is thereby conveyed to a heated rotating barrel 132 . Barrel 132 is heated by any of various means including but not limited to electric resistance heaters, gas burners, and exhaust or waste heat from other processes. Drive 139 rotates barrel 132 , which may have a smooth interior surface, or alternatively may have a surface that is corrugated or otherwise roughened, for example with lifters, to provide a means for the material to be repeatedly lifted and dropped as it moves through the barrel. Barrel 132 is inclined at a shallow angle from horizontal in order to slowly drive the powder toward the discharge assembly 133 . Calciner 130 optionally has gas inlet 135 for the addition of air or other gases and vent 134 for the removal of combustion products or other gaseous decomposition products. Calciner 130 is operated at temperatures below the point where the material begins to soften and sinter, but at elevated temperatures such that the material is preheated and dried. Other useful chemical transformations can be carried out in the calciner, including but not limited to combustion of organic materials, conversion of hydrated minerals to dehydrated oxides, desulphurization, decomposition of carbonates, and the like. The process temperature for each of these operations varies, but is generally in the range of 100 to 1000 degrees Celsius.
Calcined particulate material 139 exits at a temperature within this range, preferably about 800 to 1000 degrees Celsius, and passes through valve 140 to hopper 150 . Valve 140 can be closed to provide a vacuum-tight seal between hopper 150 and calciner 130 . Preferably valve 140 is a high-temperature rotary valve that can continuously flow material through while maintaining a pressure differential.
Hopper 150 is preferably thermally insulated, or alternatively provide with a source of heat to maintain the temperature of particulate material. Vacuum outlet 151 may be provided for connection to vacuum 152 . Vacuum removes entrained and interstitial gas from particulate material and contributes to the production of void-free synthetic hybrid rock material from a subsequent extrusion step. Vacuum can also reduce the oxidation of minerals and can increase the variety or level of crystallization in the resulting product.
Outlet 61 of hopper 150 is connected to feeder 160 at inlet flange 161 . Feeder 160 may function as a reciprocating ram, or as an auger, or as both. Auger 162 is rotated by shall 163 and drive 164 , thereby conveying particulate synthetic hybrid rock material forward into extruder barrel 180 . The entire auger/drive assembly may be moved axially, for example by means of hydraulic ram 165 moving axially in hydraulic cylinder 166 due to pressure created by pump or hydraulic power unit 167 . The axial motion of auger 162 also conveys particulate material into extruder barrel 180 .
A typical operation cycle for using both auger and ram aspects of the invention together is as follows. Under little, or none, or perhaps backward force from the hydraulic ram 165 , drive 164 rotates auger 162 , which conveys particulate material into extruder barrel 180 . When the available space in extruder barrel 180 is filled with newly conveyed particulate material, drive 164 is shut down and auger 162 stops rotating. Ram 165 is then energized by power unit 167 to provide an axial force on auger 162 , which in turn pushes on material in extruder barrel 180 . Material is conveyed axially down extruder barrel 180 in this manner for a predetermined distance. Once said predetermined distance has been reached, the force applied by hydraulic ram is reduced, and the cycle may be repeated.
Extruder barrel 180 may be constructed from a material with excellent resistance to high temperatures, good thermal conductivity, acceptable strength, and excellent resistance to wetting by or reaction with materials to be processed in the extruder. Preferably, extruder barrel 180 is constructed from silicon carbide (SiC). Most preferably, extruder barrel 180 is constructed from nitride-bonded silicon carbide (SIN—SiC), for example Advancer™ material available from St. Gobain Industrial Ceramics.
Extruder barrel 180 is compressed between feeder 160 and spider 190 and supported within furnace 170 . Furnace 170 provides heat, for example by electrical resistance heaters or by gas combustion, and is preferably a split-tube design for ease of maintenance, and also preferably has multiple zones of temperature control along its length. Furnace 170 provides heat to increase the temperature of extruder barrel 180 high enough to fuse, sinter, partially melt, or otherwise accomplish the desired vitrification of the material within.
Within extruder barrel 180 , particulate material fed by feeder 160 is conveyed axially toward reducer die 181 and heated, thereby consolidating and vitrifying particulate material into at least partially molten synthetic hybrid rock material.
Reducer die 181 connected to the end of extruder barrel 180 provides a resistance to the flow of said at least partially molten synthetic hybrid rock material and thereby increases the necessary pressure applied by ram 165 to convey the material, providing a mechanism for consolidation of the material. Optional land die 182 connected to the end of reducer die 181 may further increase the resistance to flow. In the absence of land die 182 , a spacer may be used, for example an additional short length of barrel similar to extruder barrel 180 . At the discharge end of the extruder, that is where the land die or spacer exits furnace 170 , an insulator ring 183 made of strong, thermally insulating material, preferably zirconia, is placed. Insulator ring 183 minimizes heat conduction from the furnace to spider 190 , and is captured in a recessed opening within spider 190 .
Spider 190 is a stiff plate that allows passage of extruded synthetic hybrid rock product 130 through a hole in the center while providing mechanical compression to insulator ring 183 , land die 182 , reducer die 181 and extruder barrel 180 . Spider 190 is supported by a plurality of stiff springs 191 , each reacting against a load cell 192 mounted on a fixed rigid support.
Extruded synthetic hybrid rock product 130 exits land die 182 , proceeds through insulator ring 183 and spider 190 , and is supported and conveyed by a plurality of rollers 201 within heated chambers 200 and 220 . The temperature in heated chambers 200 and 220 is maintained such that extruded synthetic hybrid rock material 230 remains deformable enough to be cut by cutters 210 attached to actuators 212 . After cutting, extruded synthetic hybrid rock material 230 may be removed from heated chamber 220 and cooled by various means to produce useful products. Alternatively, extruded synthetic hybrid rock material 230 may be conveyed to subsequent operations such as pressing, forming, rolling, molding, or glazing at a high temperature, thereby efficiently using the heat in the material.
|
The invention relates to synthetic hybrid rock compositions, articles of manufacture and related processes employing mineral waste starting materials such as mine tailings, mine development rock, ash, slag, quarry fines, and slimes, to produce valuable articles of manufacture and products, which are characterized by superior physical and structural characteristics, including low porosity, low absorption, increased strength and durability, and retained plasticity. The resulting materials are compositionally and chemically distinct from conventional synthetic rock materials as demonstrated by scanning electron microprobe analysis, and are useful in a wide variety of applications, particularly with respect to commercial and residential construction.
| 1
|
RELATED APPLICATIONS
This application is a continuation, of application Ser. No. 08/555,440, filed Nov. 9, 1995, now abandoned, which is a continuation-in-part of Ser. No. 08/157,719 fled on Nov. 26, 1993, now U.S. Pat. No. 5,465,339 in turn a continuation-in-part of Ser. No. 07/826,838, filed on Jan. 27, 1992, now U.S. Pat. No. 5,319,818.
FIELD OF THE INVENTION
This invention relates to accessibility means allowing wheelchair challenged persons improved access to recreational opportunities at beaches, lawns and fields having sand and grass surfaces that are otherwise barriers to wheelchairs.
BACKGROUND OF THE INVENTION
Wheelchair locomotion on sand, a beach, or grassy lawn or field is difficult. Sand and grass, normally considered pleasing and desirable to an able bodied person, present an obstruction to wheelchair transit and often immobilize a wheelchair user, preventing the wheelchair challenged person from participating in recreational and social activities conducted at sand and grass venues, such as for example, simple activities of sunbathing at a beach in Florida, going to a barbecue in an Arizona desert, or getting to a picnic table on the backyard lawn. Often, the wheelchair challenged person is an occasional visitor to such sites, and questions of appropriate access are forgotten or ignored. Alternatively, the installation of a permanent wheelchair access path over sand and grass is expensive and intrudes on the natural environment ambience. Prior art mechanisms for beach access include installations such as boardwalk extensions and concrete piers that support platforms extending to the beach, and/or into the ocean or body of water. Paved paths likewise allow passage and provide a hard smooth surf ace for wheelchairs. These mechanisms require the wheelchair challenged person to follow where the path leads, not necessarily where the person desires to go. At beaches, sand is a notorious barrier to wheelchair traction; the narrow wheels and the relationship of large diameter rear wheels and small diameter front wheels results in an inability to turn and maneuver the wheelchair in sand, Lawns and fields present a similar barrier; although the upper surface of a lawn may look smooth, the ground beneath is likely cratered and uneven on a scale that inhibits wheelchair locomotion . Sand and grass surfaces are uneven; sand grains and grass blades are relatively "slippery" to the rolling traction of a wheelchair. Prior art access paths are immobile and permanent installations, predetermining a fixed path. There is thus a need for a simple and conveniently deployed access pathway that is useful with wheelchairs that will provide a passage means from Point A to distant Point B over sand and grass recreational terrain surfaces.
It is an object of this invention to provide a means for the transit of a wheelchair (including a person in the wheelchair) over sandy beaches and uneven grassy surfaces such as lawns and fields. It is a further object to provide such means in an optionally temporarily deployable system (to be put in place on an as needed basis), so that the presenting environment is not significantly disturbed, and conventional maintenance, such as the periodic raking of a beach, or mowing of a lawn, is not appreciably interfered with. The pathway of the invention can be easily removed and replaced.
It is also an object of the invention to provide a retractable, and inexpensive, mechanism that allows the transit of wheelchairs at recreational venues located at beaches and lawns. The mechanism may be permanent, temporary, or temporarily and removably installed, to allow removal when not needed or when maintenance needs require. The mechanism may also be adapted to be adjustable in direction and/or length and provides a greater degree of freedom for the wheelchair user to predetermine a location at a distant desired site on the terrain involved to which the chair may be guided or taken.
These and other objects of the invention are more readily understood considered with the accompanying drawings:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows in perspective a pathway of the invention extending from a walkway over a lawn and sandy beach to a distant destination pod.
FIG. 2 is a top view of a wheelchair on a pathway of the invention.
FIG. 3 is a cross-section of a pathway through section 3A→←3A of FIG. 2.
FIGS. 4A and 4B are, respectively, a top view and cross-section of an alternatively configured pathway combining a pattern of small holes such as circles and downward projecting conical ribs in a mat useful in the invention.
FIG. 5 is a relationship chart of the size of openings in the pathway with regard to the relative size of an opening in comparison with the diameter of the small wheels of a wheelchair.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The invention provides a pathway for the transit of a wheelchair (with a person therein) over a sand or grass barrier that otherwise inhibits or obstructs wheelchair access. With reference to FIG. 1, boardwalk 1 abuts a lawn 2 leading to sandy beach 3 at a lake, ocean or other body of water 4. The pathway 5 allows conventional rolling transport of wheelchair 6 over the grass and sand surfaces. For purposes of clarity, a person in the wheelchair is not shown, but is assumed to be present. Reference to a "wheelchair" in the context herein generally includes the chair and a person seated therein. For most wheelchair challenged persons, the wheelchair is a constant necessity, intrinsically associated with the person.
The wheelchair is a conventional chair having rear side wheels 10 and 11, front side wheels 12 (not shown in the view of FIG. 1) and 13, seat 14 and back 15.
The pathway 5 is longitudinally extended and is formed by a mat having a width sufficient to accommodate the wheelchair width. The mat allows a human assistant accompanying the wheelchair user to walk thereon. Preferably, an end section 24 of the pathway mat is anchored, such as to a boardwalk or other secure fixture, or to the ground, for example, by spikes or pegs.
Depending on size considerations required by wheelchair designs (typically wheel spacing), the path is about 30 to 36 inches (about 1 meter) wide, although width is not per se a critical dimension. For example, a double width pathway (about 2 yards or 2 meters wide), allows simultaneous bi-directional movement of two chairs. A wide path may also be more aesthetically pleasing or comfort generating.
Usually, in a recreational context, the distance from departure Point A to destination Point B when the pathway is installed will be measured in the order of tens of feet or multiple meters. The path may be temporarily deployed. Preferred materials for construction of the path include flexible fiber reinforced plastic or rubber type polymer mat material, having a high UV (ultraviolet ray) resistance (recognizing the outdoor use of the path), a flexible cross-linked polymer mat or other equivalent material. Depending on the availability of local materials, or beach or lawn aesthetic preference, a woven natural fiber such as hemp, or a flexible wood slat/grid construction, is also suitable. Likewise a laminate or composite of fiber and polymer comparable to conventional indoor/outdoor carpet is a suitable construction material. An appropriate thickness for a mat path would approximate that of a typical household "indoor/outdoor" carpet, about 0.2 to 0.4 inches (approximately 1 centimeter) or more, although thickness is a variable of construction material, desired durability, use environment and other factors. Metal media flexibly configured in accordance with the teachings herein, such as in a mesh or link type design may also be useful, but have a weight and flexibility disadvantage when compared with polymer, composite or fiber materials.
As shown in greater detail in FIG. 2, the path includes a pattern of openings, 30a, 30b, 30c, 30x, etc., formed therein. Optional, upward extending "curb" sections, 31 and 32, at the side edges of the paths (approximately 0.55 to 1.0 inches (1.5 to 3 centimeters) or more above the path surface) provide a degree of guidance and/or assurance that the wheelchair does not deviate from the pathway. One or two such curbs, on one or both pathways may be provided.
The openings in the paths allow the presenting sand or grass terrain surface to penetrate up from the beach or lawn and anchor the path thereon. After a brief time and/or use, the path will "sink" slightly into the surface and become anchored. A benefit of this occurrence is that, as a result, the presence of the pathway will not greatly disturb the aesthetics of the environment. Similarly, grass from a lawn will migrate through the openings and cause anchoring. Usually, an equilibrium of the mat with the weight of the wheelchair on the sand or grass is achieved. In this regard, the path is "porous" with respect to the presenting sand or grass terrain. And the migration of the grass or sand through the openings blends the pathway visually with the environment. As used herein, "porous" refers to a holed material having openings that allow the surface material underneath to migrate upwardly through the openings. The openings also allow the pathway mat material to flexibly conform to the unevenness inherent in lawn and beach surfaces. In a path having a cross-section as characterized in FIGS. 3 and 4, the terrain material migrates upward toward the bottom surface of the mat to anchor the mat on the terrain surface. In FIGS. 4A and 4B, a section of a mat 40 (across the width thereof) is shown having downward projecting nibs 41, 42, 43, etc., extending from the bottom surface of the mat. The nibs may be conical, cylindrically-sectioned, cubical, or formed in any other three-dimensional shape, such that they have the characteristic with respect to upward migration of the terrain surface described above. A combination of openings and nibs is appropriate. Because a path configured according to FIGS. 4A and 4B requires a greater volume or mass of material, it is likely to have a greater weight and higher cost, and is consequently less preferred.
The openings may be circular or curvilinear cutouts, a square, triangle, polygon or other multisided grid or random pattern. Although not critical, the dimension and relationship of opening area may vary with terrain, wheelchair weight, wheel size and other factors. The openings should typically open approximately 20%-80% of the approximately rectangular surface area otherwise covered by the path sections on the terrain surface; openings of about 1 to 3 square inches (about 5 to 45 square centimeters) appear appropriate. Because the pathway is either regularly removed when maintenance of the beach or lawn surface is required, temporarily deployed when needed, or periodically replaced as a matter of maintenance, the pathway does not become "buried" in the terrain.
In the view shown in FIG. 1, the grass and/or beach surface, is shown to protrude or extend upward through the path "openings." The rationale of operation of the pathway mechanism is that a wheelchair supporting path is provided, which, because it is porous as defined herein, settles firmly on the presenting, uneven surface. In contrast, if, for example, a solid carpet or mat were placed over sand or grass, the solid covering, about a yard or meter wide extending 10, 20, 30 or more feet (3 to 10 or more meters), because of the uneven nature of the terrain, would not anchor itself and would not conform to the uneven surface of the lawn or beach. In addition, the appearance of a solid surface would also disturb the natural appearance and environment defeating the visually pleasing impression of a beach or lawn. In contrast, the paths herein are porous; and the openings that allow the porosity also create a pliability in the mat so that it conforms readily to the unevenness inherent in a beach or lawn surface. The openings further reduce the weight of the pathway, enabling it to be easily rolled up and removed. A pathway formed from a solid, rigid bridge material similarly contrasts with the principles of operation of the invention. The relationship of the opening size of the holes in the pattern in the pathway to the diameter of the small wheels of the wheelchair is instinctively determined first in that the openings should not be larger than the wheel diameter dimension traversing the openings. FIG. 5 shows a chart relating selected opening sizes "A", "B", "C" and "D" to wheel diameter "W." In most wheelchairs the diameter of the small wheels, usually the front wheels, is about 6.0 to 8.0 inches (2.5 to 3.5 cm.) "T" indicates pathway thickness. A useful relationship of opening size to wheel size seems to be about 1/4 to 1/3 or 5/12 (denominator=wheel diameter) with openings in the range of larger than about 1/3 to 1/2 appearing to exceed a useful limit. Sand grain size and grass coarseness are also factors for opening size within these limits. Another factor in opening configuration is that the openings should not be so wide such that the wheels become lodged therein. Hence, diameter and length and width of the openings in the pathway are related to wheel diameter in the determination of the opening size and a pattern for the openings. Openings approaching circles and squares with diameters and sides less than about 1/3 to 1/4 wheel diameter are satisfactory. Elongated rectangular shaped openings oriented transverse to the length of the pathway with a similar width, less than about 1/3 to 1/4 wheel diameter, are also satisfactory as the pathway shown in FIG. 1 is so configured.
Depending on material selection, a pathway may be formed of a sufficiently lightweight material to provide a portable mechanism to be carried with the wheelchair challenged person (or an assistant) and rolled out on site. At an attended beach, however, such as at a hotel or park, the pathway could be anchored to a boardwalk (i.e., a preexisting accessibility path) or elsewhere, and deployed by lifeguards or beach or park attendants when needed. A ground fault protected, electrically (or otherwise) powered system may also be adapted for unrolling and rolling up the pathway. To a degree, because of its flexible and porous, pliable nature and its intrinsic weight, the pathway may also be considered self-anchoring.
The pathways may be directed to, equipped with, or joined to "pod" like sections at an end thereof (e.g., sections about 30×30 inches (75×75 centimeters) square or rounded or other shaped extended surface areas capable of supporting a wheelchair and allowing limited movement thereon) to provide a positional destination and/or to allow turning movement of the wheelchair thereon, and from these sections, other pathway sections in turn may lead to other pods. Such a pod is shown in FIGS. 1 and 2 at 20. Similarly, pods for wheelchair locations may be fixed, or may be independently positioned on the terrain to provide a destination location for the wheelchair, and interconnected with other access pathways.
The size and shape of a pod is optional, however, a pod about 42-48 inches (1.0-1.2 meter) square or in diameter is a sufficiently comfortable size for a standard size adult wheelchair. At a beach, this will allow turning to different directions to avoid sunburn. A roomy "island" pod, for example, may likely be six feet (two meters) or more square to allow positional movement of the wheelchair at the destination pod and permit other persons to be seated thereon. A pod size guideline is the area defined by conventional beach umbrellas or the seating area at a side of a picnic table. The deployment of location pods and pathways leading to the pods, at an attended public or commercial beach, for example, is an activity no more difficult for beach attendants than is a conventional placement and set up of a beach lounge chair.
Depending on the material of construction and design preference, the pathway and/or pod may be colored in whole or in part, for example, by safety yellow, to highlight its presence, or camouflaged in an appropriate pattern to blend in with the natural environment.
The dimensions and proportions herein and the materials of fabrication depend on design considerations of durability, weight, public or institutional use considerations, aesthetics, ambient temperature, and other factors, provided however, that good design criteria for the wheelchair application, given the foregoing disclosure, are satisfied.
|
A pathway for providing the transit of a wheelchair, including a person therein, over an uneven terrain surface that resists the rolling traction of a wheelchair, comprising a longitudinally extended flexible mat-like pathway configured such that the surface of the pathway is relatively porous with respect to the terrain surface, such as by providing therein a plurality of openings, and is capable of receiving thereon, at opposite side sections thereof, the front and side wheels of each side of a wheelchair. The pathways may be interconnected to pod-like landing sites at recreational locations.
| 4
|
This application claims priority to U.S. Provisional Patent Application 61/315,662, filed Mar. 19, 2010, herein incorporated by reference in its entirety.
BACKGROUND
1. Field
The present invention relates generally to coupling of optical elements, and more particularly to alignment and coupling of an optical element with an optical fiber end.
2. Background
Various applications are known that involve the fusion of a silica disk or rod onto the end of an optical fiber. In general, devices of this type are made using a fusion splicing technique that relies on heating using a laser or arc source. In this approach, the silica disk and the optical fiber are heated simultaneously to create a fused region and generally the silica disk is of similar diameter to the optical fiber, or larger. In addition, such a method would involve fusing of an optically flat silica disk or a solid cylinder, with no other optical or mechanical features.
SUMMARY
An aspect of an embodiment of the present invention includes an optical element fused with an optical fiber in mechanical alignment.
An aspect of an embodiment of the present invention includes a method of manufacturing an optical element fused with an optical fiber in mechanical alignment.
DESCRIPTION OF THE DRAWINGS
Other features described herein will be more readily apparent to those skilled in the art when reading the following detailed description in connection with the accompanying drawings, wherein:
FIGS. 1A and 1B are illustrations of a fiber fused with a disk-shaped optical element in accordance with an embodiment of the present invention;
FIGS. 2A and 2B are illustrations of a fiber fused with a convex optical element in accordance with an embodiment of the present invention;
FIGS. 3A and 3B are illustrations of a fiber fused with a concave optical element in accordance with an embodiment of the present invention;
FIGS. 4A and 4B are illustrations of a fiber fused with a spherical optical element in accordance with an embodiment of the present invention;
FIGS. 5A and 5B are illustrations of a fiber fused with a side firing optical element in accordance with an embodiment of the present invention; and
FIGS. 6A-6E are illustrations of steps in a method of fusing an optical fiber with a ferrule to form a spherical optical element.
DETAILED DESCRIPTION
In an embodiment of the present invention, an optical fiber is fused to a silica ferrule or tube of varying inner diameter (ID) and outer diameter (OD). The ferrule ID is sized to match the optical fiber OD or an intermediate spacing silica sleeve with an ID that is sized to match the OD of the fiber. The ferrule OD is typically significantly larger than the optical fiber OD. The fusion is performed by heating the ferrule (typically by a laser such as a CO 2 laser, but including, for example, a fusion splicer, an electric arc resistance element, and/or a plasma) and then inserting the fiber into the hole of the ferrule. This minimizes the heating of the optical fiber which reduces damage to the optical fiber coatings and fiber doping profile. Furthermore, the ferrule can be configured with other mechanical or optical features which become useful in the finished device. Such features can be optical in nature, such as an incorporated lens or angled face, or mechanical, such as a flat or slot, which can be used as an alignment key in the finished device. In the case where the ferrule OD is significantly larger than the optical fiber OD, the finished device will generally provide greater ease of handling as compared to other approaches. In an embodiment, use of a ferrule having a relatively large OD may simply eliminate the step of separately mounting a silica disk into a ferrule. The larger OD ferrule can also be set at an industry standard OD thereby becoming the finished device ferrule with no further processing. The ID of the ferrule also serves as an “auto-aligning” feature which holds the fiber in the proper position with respect to the ferrule, with or without the intermediate spacing sleeve, and the ferrule's optical and mechanical features. In this regard, the ID may be varied from a diameter slightly larger than the fiber OD down to a diameter equal to or slightly less than the fiber OD thereby precisely locating the fiber end with respect to the ferrule end, both distance and angle, and with respect to the ferrule center.
As will be understood, the fiber to be fused may be a single mode, multimode, step index, graded index, photonic bandgap, rare earth doped, active, polarization maintaining and/or high birefringent fiber.
In an embodiment, the ferrule is made from a material having a refractive index equal to or substantially similar to the refractive index of the optical fiber to which it is to be fused. In this regard, materials of primary interest are synthetic fused silica and quartz glass. In addition to providing good refractive index matching to optical fiber, these materials generally match the thermal expansion properties of optical fiber as well. The optical element can consist of varying geometries that are shaped either by common or proprietary laser machining techniques or mechanical polishing techniques or a combination of both. It is expected that the optical element can be used with or without optical coatings, such as an anti-reflective coating for specific applications using narrow wavelength bandwidths.
In various end-use applications, the presence of the optical element tends to reduce power density on the optical fiber end face thus reducing laser induced damage. This reduction relative to a damage threshold may allow the usage of higher laser powers launched directly from the laser source into the optical element to be fused onto the optical fiber. The optical element can also function as an optical lens such as those currently sculpted onto optical fibers. In a particular embodiment the optical element may be of the disk type, for example a 2 mm disk type optical element. In an alternate particular embodiment, the element may be a 300 μm semi-spherical element. In an alternate particular embodiment, the element may be a 500 μm spherical element.
FIG. 1A illustrates an example of an optical element 10 in accordance with an embodiment of the invention. An optical fiber 12 is held within an intermediate spacing sleeve 14 and within a ferrule 16 . A flat end optical element 18 is formed at the distal end of the optical element 10 . An adhesive 20 is optionally used to seal the proximal end of the element. FIG. 1B illustrates a similar optical element 10 , lacking only the intermediate spacing sleeve 14 .
FIG. 2A illustrates an example of an optical element 10 similar to the optical element of FIG. 1A , but having a convex optical element 22 formed at the distal end. The optical element of FIG. 2B is similar to the optical element of FIG. 2A , but lacks the intermediate spacing sleeve 14 .
FIG. 3A illustrates an example of an optical element 10 similar to the optical element of FIG. 1A , but having a concave optical element 24 formed at the distal end. The optical element of FIG. 3B is similar to the optical element of FIG. 3A , but lacks the intermediate spacing sleeve 14 .
FIG. 4A illustrates an example of an optical element 10 similar to the optical element of FIG. 1A , but having a spherical optical element 26 formed at the distal end. The optical element of FIG. 4B is similar to the optical element of FIG. 4A , but lacks the intermediate spacing sleeve 14 .
FIG. 5A illustrates an example of an optical element 10 similar to the optical element of FIG. 1A , but having a side firing optical element 28 formed at the distal end. The optical element of FIG. 5B is similar to the optical element of FIG. 5A , but lacks the intermediate spacing sleeve 14 .
In an embodiment, the optical element is made from capillary tubing, also known as a ferrule, consisting of a tube having one or more inside diameters. The mechanical alignment of the optical element is also provided by the same ferrule. By way of example, a ferrule for use in an embodiment of the invention may have an outside diameter (OD) from 200 um to more than 3500 um and the inside diameter (ID) may typically be from 50 um to more than 2500 um so long as the wall thickness between the ID and OD is sufficient for forming a mass that will become the optical element. The overall length of the ferrule can typically be as short as 3 mm and as long as 100 mm. The length or thickness of the optical element formed from the ferrule can typically be as thin as 5 um and as thick as 10 mm.
The process of forming the optical element uses a methodology which allows for varying geometries and may provide the ability to achieve high production volumes, as illustrated in FIGS. 6A-6E . A ferrule 40 is cleaved to a desired length, commonly up to a few centimeters, and then positioned into a laser machining station. An optical fiber 42 or a group of optical fibers, which may be, for example, single mode or multimode fiber, prepared for fusing, are inserted into the ferrule and fixed at a predetermined location with respect to the estimated optical element location.
To form the optical element from the capillary tubing (ferrule) a sufficient amount of mass must be manipulated to form the desired shape. This mass from the ferrule is heated to achieve a molten state via laser energy typically by a CO 2 laser 44 operating at a wavelength of 10.6 um in continuous wave mode; however other types of lasers such as Nd:YAG operating at a wavelength of 1064 nm, or a CO 2 laser operating at a wavelength of 9.6 um, among others may also be used. In the illustrated embodiment, a focusing lens 46 may be used to focus the laser beam 48 onto a target region as necessary or desirable. In an embodiment, the focus spot size may be a few hundred microns, for example, 350-450 μm, or more particularly, about 380 μm. As shown in FIG. 6B , the ferrule 40 collapses as it is heated. FIG. 6C illustrates the condition when the ferrule 40 has completely collapsed, and FIG. 6D illustrates the mass at the end as it is formed into a spherical optical element. In an embodiment, the fiber and ferrule may still not have been fused together. In this approach, the fiber/ferrule assembly is then repositioned with respect to the focused beam as illustrated in FIG. 6E . Once so positioned, the fusion step may proceed.
In order to provide uniform heating, controlled laser heating may be performed while rotating (arrow) the fiber relative to the laser (or alternately, by rotating the laser beam around the fiber). As will be appreciated, the laser manipulation of the mass may produce, for example, semispherical, spherical or flat geometries. Likewise, a selected radius of curvature may be achieved in accordance with the desired final application. As described above, other heat sources aside from lasers may alternately be employed in this and other embodiments.
Once the optical element is formed from molten material of the ferrule, the fusion of the optical element to the optical fiber(s) is performed while the ferrule mass is in the molten state. Radiant energy from the molten mass will have heated the end face of the optical fiber(s) that is to be fused to the optical element. The optical fiber(s) and the molten mass should be close together to allow for heat transfer and fusion success, for example a distance on the order of a few microns up to about 20 μm. By further heating, the molten mass is grown until contact of the mass to the optical fiber(s) is made and fusion between the optical element and the fiber is accomplished. Likewise, laser machining techniques may be used to collapse the ferrule's ID onto the optical fiber to fuse the two together along the length of the ferrule. This collapse may, in principle, be partially or completely performed prior to the formation of the optical element.
While the molten ferrule mass remains soft, and with the fusion completed, the ferrule mass can be formed into a desired geometry using varying techniques such as stamp-mold forming, or other techniques commonly used to sculpt optical fiber. Alternately, or in addition, once the optical element has been cooled to room temperature it may be reformed to a desired geometry via mechanical polishing or further laser machining.
In a process in accordance with an embodiment of the invention, a first step involves cleaving a capillary tubing (ferrule) to a predetermined length. Next, the ferrule is positioned into a laser machining station. Next, the optical fiber or fibers to be fused are inserted into the ferrule. Next, the optical element mass is formed using a heating process. Once the optical element mass is formed, the optical fiber or fibers are fused to the mass. Finally, the optical element mass is sculpted to produce a final geometry using mechanical and/or laser machining.
In an embodiment, the ferrule has a large ID compared with the fiber OD. In general, such an arrangement may allow for an improved optical index mismatch at the air interface, meaning that an increased amount of the machining laser light would be delivered to the ferrule without heating the fiber. In this case, an intermediate sleeve may be positioned between the ferrule and the fiber in order to physically position the fiber.
In an embodiment, the optical element is manufactured to produce a side-fire configuration. For example, it may be machined to have an angled end-face such that light exiting the fiber is transmitted at an angle to its length.
In an embodiment, the ferrule is doped such that a portion of the ferrule to be fused has a relatively lower softening temperature compared with the bulk of the ferrule. Ferrules having this structure are described in U.S. Pat. No. 6,883,975, herein incorporated by reference in its entirety.
In an embodiment, the ferrule may be doped such that it contributes optical properties to the finished optical element. For example, the ferrule may be doped such that in the finished product, it acts as a portion of the waveguide design for the finished element. In an example, the ferrule is doped with fluorine such that it acts as a cladding or outer waveguide to contain light in the fiber/optical element system.
In an embodiment, the ferrule includes a flattened or notched internal portion that is configured to cooperate with a complementary flattened or protruding (or vice versa) external portion of the fiber to be inserted and aligned.
Those skilled in the art will appreciate that the disclosed embodiments described herein are by way of example only, and that numerous variations will exist. For example, as will be appreciated by one of ordinary skill in the art, the dimensions described herein are by way of example, but are not limits as to sizes that may be used. The invention is limited only by the claims, which encompass the embodiments described herein as well as variants apparent to those skilled in the art.
|
A product and process for fabricating an optical element from a capillary ferrule includes fusing the optical element onto an optical fiber. The optical element starts with a capillary ferrule that is sculpted on one end to form an optical property such as a flat window, ball lens, angled endface or other sculpted shape. The ferrule is fused onto an optical fiber that has been inserted into the ID of the capillary ferrule. As a result, the ferrule serves as a mechanical aligner for the optical element to fiber fusion process.
| 6
|
RELATED APPLICATIONS
[0001] This Application is related to application Ser. No. ______ filed on ______.
FIELD OF THE INVENTION
[0002] The present invention relates to the field of integrated circuits; more specifically, it relates to structures of and methods for fabricating ultra-deep vias in integrated circuits and structures of and methods for fabricating three-dimensional integrated circuits.
BACKGROUND OF THE INVENTION
[0003] In order to reduce the footprint and improve the speed of integrated circuits various three-dimensional integrated circuit structures have been proposed. Traditional integrated circuit structures have been two dimensional, in that all the active devices have been formed in a same plane in a same semiconductor layer. Three-dimensional integrated circuits utilize vertically stacked semiconductor layers with active devices formed in each of the stacked semiconductor layers.
[0004] The fabrication of three-dimensional integrated circuits poses many challenges particularly in the methodology for interconnecting devices in the different semiconductor layers together. The total depth of these interconnects can exceed 1.5 um with diameters in the sub 0.2 um range. It is difficult to fill vias having such large depth to width aspect ratios with high quality, defect free metal. In particular, the metal fill of large aspect ratio and very deep vias often contain voids which can increase the resistance of the via and result in yield loss as well as reduce the reliability of the device. Accordingly, there exists a need in the art to overcome the deficiencies and limitations described hereinabove.
SUMMARY OF THE INVENTION
[0005] A first aspect of the present invention is a method, comprising: forming an etch stop layer on a top surface of a substrate; forming a first dielectric layer on a top surface of the etch stop layer; forming a profile modulation layer on a top surface of the first dielectric layer; forming a second dielectric layer on a top surface of the profile modulation layer; forming a photo-imaging layer on a top surface of the second dielectric layer; forming an opening in the photo-imaging layer, a region of the top surface of the second dielectric layer exposed in a bottom of the opening; reactive ion etching the second dielectric layer with a first etch chemistry selective to the profile modulation layer to form an opening through the second dielectric layer; reactive ion etching the profile modulation layer with a second etch chemistry selective to the first and second dielectric layers to extend the opening through the profile modulation layer; reactive ion etching the first dielectric layer with a third etch chemistry selective to the profile modulation layer and selective to the etch stop layer to extend the opening through the first dielectric layer; reactive ion etching the etch stop layer with a fourth etch chemistry selective to the first and second dielectric layers to extend the opening through the etch stop layer; and removing the photo-imaging layer, after the removing the photo-imaging layer, the opening extending from the top surface of the second dielectric layer, through the second dielectric layer, through the profile modulation layer, through the first dielectric layer and through the etch stop layer to the top surface of the substrate.
[0006] A second aspect of the present invention is the first aspect, wherein the third etch chemistry is not selective to the second dielectric layer.
[0007] A third aspect of the present invention is the first aspect, wherein the first and third etch chemistries are a same chemistry.
[0008] A fourth aspect of the present invention is the first aspect, wherein the second and fourth etch chemistries are a same chemistry.
[0009] A fifth aspect of the present invention is the first aspect, wherein the removing the photo-imaging layer is performed between the reactive ion etching the first dielectric layer and the reactive ion etching the etch stop layer.
[0010] A sixth aspect of the present invention is the first aspect, wherein the first dielectric layer and second dielectric layer comprise silicon oxide and the profile modulation layer and the etch stop layer comprise silicon nitride.
[0011] A seventh aspect of the present invention is the first aspect, wherein: a first width of the opening measured in first direction parallel to the top surface of the second dielectric layer at the top surface of the second dielectric layer is greater than a second width of the opening measured in the first direction at the top surface of the profile modulation layer and greater than a third width of the opening measured in the first direction at the top surface of the substrate, the second width greater than or equal to the third width; and wherein a ratio of a depth of the opening measured in a second direction perpendicular to the first direction from the top surface of the second dielectric layer to the top surface of the substrate to the first width is equal to or greater than five.
[0012] An eighth second aspect of the present invention is the first aspect, further including: after the removing the photo-imaging layer, filling the opening with the electrical conductor.
[0013] A ninth aspect of the present invention is the eighth aspect, wherein the filling the opening with an electrical conductor comprises: depositing a tantalum nitride layer over sidewalls and a bottom of the opening; depositing a tantalum layer on the tantalum nitride layer; depositing a seed copper layer the tantalum layer; electroplating an electroplated copper layer on the seed copper layer, the electroplated copper layer completely filling remaining spaces in the opening; and performing a chemical-mechanical-polish to remove the tantalum nitride layer, the tantalum layer, the seed copper layer and the electroplated copper layer from over the top surface of the second dielectric layer.
[0014] A tenth aspect of the present invention is the first aspect, wherein the photo-imaging layer includes a photoresist layer over an antireflective coating on the top surface of the first dielectric layer and the forming the opening in the photo-imaging layer comprises exposing the photoresist layer to actinic radiation through a patterned photomask, developing the exposed photoresist layer and reactive ion etching the antireflective coating with an initial etch chemistry where the anti-reflective coating is not protected by the photoresist layer.
[0015] An eleventh second aspect of the present invention is the tenth aspect, wherein the initial etch chemistry is selective to the photoresist layer and the first dielectric layer and wherein the initial, second and fourth etch chemistries are a same chemistry.
[0016] A twelfth aspect of the present invention is a structure comprising: forming a first substrate, the first substrate including: first transistors electrically connected to a set of wiring levels, each wiring level including electrically conductive wires in a respective dielectric layer; an etch stop layer on a top surface of an uppermost wiring level of the set of wiring levels that is furthest from the substrate, the etch stop layer in contact with a wire of the uppermost wiring level; and a first dielectric bonding layer on a top surface of the etch stop layer; forming a second substrate, the second substrate including: a second dielectric bonding layer; a buried oxide layer on a top surface of the second dielectric bonding layer; a semiconductor layer on a top surface of the buried oxide layer, the semiconductor layer including second transistors electrically isolated from each other by dielectric isolation in the silicon layer; a profile modulation layer on a top of the silicon layer and on a top surface of the dielectric isolation; and a first dielectric layer on a top surface of the profile modulation layer; bonding a top surface of the first dielectric bonding layer to a bottom surface of the second dielectric bonding layer, the first and second dielectric bonding layers, the buried oxide layer and the dielectric isolation comprising a multilayer second dielectric layer; forming a photo-imaging layer on a top surface of the first dielectric layer; forming an opening in the photo-imaging layer, a region of the top surface of the first dielectric layer exposed in a bottom of the opening; reactive ion etching the first dielectric layer with a first etch chemistry selective to the profile modulation layer to form an opening through the first dielectric layer; reactive ion etching the profile modulation layer with a second etch chemistry selective to the first and second dielectric layers to extend the opening through the profile modulation layer; reactive ion etching the second dielectric layer with a third etch chemistry selective to the profile modulation layer and selective to the etch stop layer to extend the opening through the second dielectric layer; reactive ion etching the etch stop layer with a fourth etch chemistry selective to the first and second dielectric layers and to the wire to extend the opening through the etch stop layer; removing the photo-imaging layer, after the removing the photo-imaging layer the opening extending from the top surface of the first dielectric layer, through the profile modulation layer, through the second dielectric layer, through the second dielectric layer and through the etch stop layer to a top surface of the wire; and filling the opening with an electrical conductor, the electrical conductor in electrical contact with the wire.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The features of the invention are set forth in the appended claims. The invention itself, however, will be best understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying drawings, wherein:
[0018] FIGS. 1A through 1J are cross-sections of the fabrication of an exemplary electrically conductive via according to embodiments of the present invention;
[0019] FIGS. 2A through 2C are cross-sections of the fabrication of a first exemplary three dimensional integrated circuit according to embodiments of the present invention; and
[0020] FIG. 3 is a cross-section of additional fabrication steps in the fabrication of three-dimensional integrated circuit according to embodiments of the present.
DETAILED DESCRIPTION OF THE INVENTION
[0021] FIGS. 1A through 1J are cross-sections of the fabrication of an exemplary electrically conductive via according to embodiments of the present invention. In FIG. 1A , formed in a semiconductor substrate 100 is a metal wire 105 . Formed on a top surface 110 of substrate 100 is a dielectric etch stop layer 115 . Formed on top of etch stop layer 115 is a first dielectric layer 120 . Formed on first dielectric layer 120 is a second dielectric layer 125 . Formed on second dielectric layer 125 is a third dielectric layer 130 . Formed on top of third dielectric layer 130 is a profile modulation layer 135 . Formed on profile modulation layer 135 is a fourth dielectric layer 140 . Semiconductor substrate 100 may comprise, for example, Si, SiGe, Ge, GaAs or InP.
[0022] The stack of dielectric materials consisting of dielectric etch stop layer 115 , first dielectric layer 120 , second dielectric layer 125 , third dielectric layer 130 , profile modulation layer 135 and fourth dielectric layer 140 simulates a structure that conductive vias are formed through in fabrication of a three-dimensional integrated circuit according to embodiments of the present invention described infra. Therefore in one example, etch stop layer 115 and first dielectric layer 120 represent layers on a lower semiconductor substrate and second dielectric layer 125 , third dielectric layer 130 , profile modulation layer 135 and fourth dielectric layer 140 represent layers on an upper semiconductor layers with first and second dielectric layers 120 and 125 representing oxide bonding layers that bond the two substrates together. Third dielectric layer 130 represents a dielectric trench isolation (TI) or dielectric shallow trench isolation (STI) on a buried oxide layer (BOX) of a silicon-on-insulator (SOI) substrate.
[0023] In accordance with the simulation of a three-dimensional integrated circuit according to embodiments of the present invention, etch stop layer 115 is silicon nitride and in one example is about 500 Å thick, first dielectric layer 120 is low temperature silicon oxide (LTO) and in one example is between about 2500 Å and about 3500 Å thick, second dielectric layer 125 is LTO and in one example is between about 2500 Å and about 3500 Å thick, third dielectric layer 130 is high density plasma silicon (HDP) oxide thermal oxide and in one example is about 3600 Å thick, profile modulation layer 135 is silicon nitride and in one example is about 500 Å thick and fourth dielectric layer 140 is HDP oxide and in one example is about 4700 Å thick. In one example, metal wire 105 comprises copper. The HDP oxide of third dielectric layer 130 and fourth dielectric layer 140 may be independently replaced with plasma enhanced chemical vapor deposition (PECVD) oxide, ultrahigh density plasma (UHP) oxide, tetraethoxysilane (TEOS) oxide or spin-on-oxide. The silicon nitride of etch stop layer 115 and profile modulation layer 135 may be independently replaced with silicon carbide, silicon oxy nitride, silicon oxy carbide or Nblock (SiCNH). In oxide fusion bonding applications, first and second dielectric layer are LTO, but in other application may be independently thermal oxide, HDP oxide, PECVD oxide, UDP oxide, TEOS oxide or spin-on-oxide. In one example, thicknesses of etch stop layer 115 and profile modulation layer 135 are independently about 5 times less than a thickness of either fourth dielectric layer 140 or a combined thickness of first, second and third dielectric layers 120 , 125 and 130 .
[0024] An LTO oxide is a silicon oxide that is formed at temperatures below about 350° C. In one example, LTO oxides are formed using N 2 O in a plasma enhanced chemical vapor deposition (PECVD) process. An HDP oxide are specifically prepared to be fusion bonded to each other.
[0025] First second, third and fourth dielectric layers 120 , 125 , 130 and 140 are advantageously first similar materials (e.g., silicon oxides) and etch stop layer 115 and profile modulation layer 135 are advantageously second similar materials (e.g. silicon nitrides), where the second materials may be selectively plasma etched relative to the first materials.
[0026] In FIG. 1B , an optional antireflective coating (ARC) 145 is formed on fourth dielectric layer and a photoresist layer 150 formed on top of the ARC. An opening 155 is formed in photoresist layer 150 photolithographically by exposing photoresist layer 150 to actinic radiation through a patterned photomask and then developing the photoresist layer to transfer the pattern of the photomask into the photoresist layer. A region of ARC 145 is exposed in the bottom of opening 155 . ARC 145 is a bottom ARC or BARC since it is formed under photoresist layer 150 . A top ARC (TARC) formed over the photoresist may be substituted or both a TARC and BARC may be used. The combination of a photoresist layer and an ARC (i.e., BARC, TARC or both BARC and TARC) is defined as a photo-imaging layer.
[0027] In FIG. 1C , the region of ARC 145 exposed in opening 155 of FIG. 1B is removed using a reactive ion etch (RIE) that etches ARC 145 faster than photoresist layer 150 (i.e., ARC 145 is RIE'd selective to photoresist layer 150 ) to expose a region of fourth dielectric layer 140 in the bottom of an opening 155 A. An example RIE process for etching ARC 145 includes etching with a mixed CF 4 /CHF 3 /Ar/O 2 gas derived plasma.
[0028] In FIG. 1D , the region of fourth dielectric layer 140 exposed in opening 155 A of FIG. 1C is removed using an RIE that etches fourth dielectric layer 140 faster than profile modulation layer 135 (i.e., fourth dielectric layer 140 is RIE'd selective to profile modulation layer 135 ) to expose a region of the profile modulation layer in the bottom of an opening 155 B. Note, photoresist layer 150 and ARC 145 are eroded by the fourth dielectric layer 140 RIE etch. The opening in the top surface of photoresist layer 150 is larger than the opening in the bottom surface of the photoresist layer. An example RIE process for etching fourth dielectric layer includes etching with a mixed CO/C 4 F 8 /Ar gas derived plasma. This chemistry (at the proper bias, forward and reverse power, pressure and gas flows) etches silicon oxide about 25 times faster than silicon nitride.
[0029] In FIG. 1E , the region of profile modulation layer 135 exposed in opening 155 B of FIG. 1D is removed using an RIE that etches profile modulation layer 135 faster than third dielectric layer 130 (i.e., profile modulation layer 135 is RIE'd selective to third dielectric layer 130 ) to expose a region of the third dielectric layer in the bottom of an opening 155 C. An example RIE process for etching profile modulation layer includes etching with a mixed CHF 3 /CF 4 /Ar gas derived plasma. This chemistry (at the proper bias, forward and reverse power, pressure and gas flows) etches silicon nitride about 4 times faster than silicon oxide. It is advantageous to keep profile modulation layer 135 (and etch stop layer 115 ) as thin as possible.
[0030] In FIG. 1F , the region of third dielectric layer 130 exposed in opening 155 C of FIG. 1E is removed along with regions of second and first dielectric layers 125 and 120 aligned under opening 155 C of FIG. 1E using an RIE that etches third, second and first dielectric layers 130 , 125 and 120 faster than etch stop layer 115 and profile modulation layer 135 (i.e., third dielectric layer 130 is RIE'd selective to etch stop layer 115 and profile modulation layer 135 ) to expose a region of the etch stop layer in the bottom of an opening 155 D. An example RIE process for etching third, second and first dielectric layers 130 , 125 and 120 includes etching with a mixed CO/C 4 F 8 /Ar gas derived plasma. Note, photoresist layer 150 and ARC 145 are further eroded by the third dielectric layer 130 , second dielectric layer 125 and first dielectric 120 RIE etches. This etch is not selective to fourth dielectric layer 140 and in combination with the further erosion of photoresist layer 150 and ARC 145 , a tapered upper region 160 of opening 155 D is formed in the region of opening 155 D formed through fourth dielectric layer 140 . The sidewall of opening 155 D in region 160 taper at an angle “a” measured between the sidewall and a plane parallel to top surface 110 of substrate 100 . A lower region 165 of opening 155 D is formed through profile modulation layer 135 and third, second and first dielectric layers 130 , 125 and 120 . The sidewall of opening 155 D in region 165 is at an angle “b” measured between the sidewall and a plane parallel to top surface 110 of substrate 100 . Opening 155 D has width W 1 measured at the top surface of fourth dielectric layer 140 , a width W 2 measured at a top surface of profile modulation layer 135 and a width W 3 , measured at a top surface of etch stop layer 115 . W 1 is greater than W 2 . In one example W 1 is about 0.28 microns and W 3 is about 0.16 microns.
[0031] In one example, W 2 is equal to W 3 and angle “b” is between about 87° and no greater than 90°. In one example W 2 is greater than W 3 , however angle “b” is less than angle “a.” Again, the presence of profile modulation layer 135 allows the widening of opening 155 D at the top surface of fourth dielectric layer 140 in upper region 160 due to the controlled erosion of photoresist layer 150 while facilitating formation of a straight or sidewall in lower region 165 . Without profile modulation layer 135 , either opening 155 D would be to narrow at the top to be filled with metal without incorporating large voids in the metal fill, or the value of W 1 would need to be much greater to maintain the same value of W 3 obtained with the presence of the profile modulation layer.
[0032] In FIG. 1G , photoresist layer 150 and arc 145 (See FIG. 1F ) are removed using an oxygen ash process (i.e., O 2 plasma etch). Alternatively, this step may be performed after the process illustrated in FIG. 1H . It is advantageous to perform the photoresist removal step with etch stop layer 115 intact to prevent the photoresist removal process from oxidizing wire 105 particularly when wire 105 comprises copper.
[0033] In FIG. 1H , the region of etch stop layer 115 exposed in opening 155 D of FIG. 1G is removed using an RIE that etches stop layer 115 faster than first, second, third dielectric layers 120 , 125 and 130 (i.e., etch stop layer 115 is RIE'd selective to first, second and third dielectric layers 120 , 125 and 130 , metal wire 105 and optionally fourth dielectric layer 140 ) to expose a region of metal wire 105 in the bottom of an opening 155 E. An example RIE process for etching etch stop layer 115 includes etching with a mixed CF 4 /CHF 3 /Ar/O 2 gas derived plasma. Region 160 has a height H 1 measured from the top surface of fourth dielectric layer 140 to the top surface of profile modulation layer 135 in a direction perpendicular to the top surface of wire 105 in substrate 100 . Region 165 has a height H 2 measured from the top surface of profile modulation layer 134 to the top surface of wire 105 in substrate 100 in a direction perpendicular to the top surface of wire 105 in substrate 100 . In one example H 1 is about 0.4 microns and H 2 is between about 1 micron an and about 1.6 microns for total opening depth (i.e., H 1 +H 2 ) of between about 1.4 microns and about 2.0 microns. With a value of W 3 (see FIG. 1F ) of about 0.16 microns the depth to width ratio of opening 155 E is between about 1.4/0.16 about 8.75 and about 2.0/0.16=about 12.5. In one example, H 1 +H 2 is equal to or greater than about 1 micron. In one example, H 1 +H 2 is equal to or greater than about 2 microns. In one example (H 1 +H 2 )/W 1 is greater than or equal to 5. In one example (H 1 +H 2 )/W 1 is greater than or equal to 8.
[0034] In FIG. 1I , an optional direct current (DC) clean (e.g., sputter cleaning with an inert gas) is performed followed by formation of an electrically conductive liner 170 on the sidewall of opening 155 E and top surface of fourth dielectric layer 140 followed by overfilling the opening 155 E with an electrically conductive core conductor 175 . In one example, conductive liner 170 comprises, in the order of deposition, a layer of TaN, a layer of Ta and a layer of Cu and core conductor 175 comprises electroplated copper.
[0035] In FIG. 1J , a chemical-mechanical-polish (CMP) is performed to remove liner 170 and core conductor 175 from over fourth dielectric layer 140 to form an electrically conductive via 180 extending from a top surface 185 of the fourth dielectric layer to a top surface of wire 105 (making electrical contact with wire 105 ). After the CMP, a top surface 190 of via 180 is coplanar with top surface 185 of fourth dielectric layer 140 .
[0036] It should be understood in the simplest form, embodiments of the present invention may be practiced on a dielectric stack where first, second and third dielectric layers 120 , 125 and 130 of FIG. 1 are replaced with a single dielectric layer. In other embodiments, their may be more than three dielectric layers in the stack represented by first, second and third dielectric layers 120 , 125 and 130 of FIG. 1 , though they should all be similar materials (e.g., silicon oxides) or have similar selectivity's to the RIE used to etch stop and profile modulation layers.
[0037] FIGS. 2A through 2C are cross-sections of the fabrication of a first exemplary three-dimensional integrated circuit according to embodiments of the present invention. In FIG. 2A , an upper semiconductor substrate 200 includes a silicon oxide bonding layer 205 , a BOX layer 210 on the bonding layer, a semiconductor layer 215 including semiconductor regions 220 and STI 225 formed in the semiconductor layer, a profile modulation layer 230 on top of semiconductor layer 215 and a dielectric layer 235 on the passivation layer. Exemplary, field effect transistors (FETs) 240 comprising source/drains (S/D) formed in semiconductor regions 220 and gates formed over the silicon regions between the S/Ds are formed in substrate 200 . Semiconductor layer 215 may comprise, for example, Si, SiGe, Ge, GaAs or InP.
[0038] Etch stop layer may also serve as a diffusion barrier layer for copper and/or as a passivation layer.
[0039] A substrate 300 includes a semiconductor base later 305 , a BOX layer 310 on the base silicon layer, a semiconductor layer 315 including semiconductor regions 320 and STI 325 formed in the silicon layer, an interlevel dielectric (ILD) wiring set 330 including contacts 335 and wires 340 and 350 formed in respective dielectric layers of dielectric layers 355 of ILD wiring set 330 . Semiconductor base layer 305 may comprise, for example, Si, SiGe, Ge, GaAs or InP. Semiconductor layer 315 may comprise, for example, Si, SiGe, Ge, GaAs or InP.
[0040] An ILD wiring level comprises a dielectric layer and one or more wires, vias or contacts embedded therein. ILD wiring set 330 is illustrated having three ILD wiring levels. ILD wiring set 330 may include more or less ILD levels (down to one level containing contacts 335 ) or as many levels as required by the integrated circuit design. The ILD wiring levels of ILD wiring set 330 are, by way of example, damascene and dual-damascene ILD levels formed by damascene and dual-damascene processes.
[0041] A damascene process is one in which wire trenches or via openings are formed in a dielectric layer, an electrical conductor of sufficient thickness to fill the trenches is deposited on a top surface of the dielectric, and a chemical-mechanical-polish (CMP) process is performed to remove excess conductor and make the surface of the conductor co-planar with the surface of the dielectric layer to form damascene wires (or damascene vias). When only a trench and a wire (or a via opening and a via) is formed the process is called single-damascene.
[0042] A dual-damascene process is one in which via openings are formed through the entire thickness of a dielectric layer followed by formation of trenches part of the way through the dielectric layer in any given cross-sectional view. All via openings are intersected by integral wire trenches above and by a wire trench below, but not all trenches need intersect a via opening. An electrical conductor of sufficient thickness to fill the trenches and via opening is deposited on a top surface of the dielectric and a CMP process is performed to make the surface of the conductor in the trench co-planar with the surface the dielectric layer to form dual-damascene wires and dual-damascene wires having integral dual-damascene vias.
[0043] Returning to FIG. 2A , exemplary, field effect transistors (FETs) 345 comprising source/drains (S/D) formed in semiconductor regions 320 and gates formed over the silicon regions between the S/Ds are formed in substrate 300 . Contacts 335 and wires 340 electrically connect FETs 345 into circuits or portions of circuits. Substrate 300 further includes an etch stop layer 360 on top of ILD wiring set 355 and a silicon oxide bonding layer 365 on the etch stop layer. Bonding layers 205 and 365 bond substrates 200 and 300 into a single structure. The bonding process includes placing the bonding layers 205 and 365 in contact at a temperature above room temperature but below, for example, 350° C.
[0044] In one example, dielectric layers 235 , 355 and STI 225 are independently selected from the group consisting of thermal oxide, HDP oxide, PECVD oxide, UDP oxide, TEOS oxide and spin-on-oxide, and bonding layers 205 and 365 are LTO. In one example profile modulation layer 230 and etch stop layer 360 are independently selected from the group consisting of silicon nitride, silicon carbide, silicon oxy nitride or silicon oxy carbide. In a second example, dielectric layers 235 , 355 and STI 225 and bonding layers 205 and 365 are advantageously first similar materials (e.g., silicon oxides) and etch stop layer 360 and profile modulation layer 230 are advantageously second similar materials (e.g. silicon nitrides), where the first and second materials may be selectively plasma etched relative to each other. In one example, dielectric layer 235 is between about 2500 Å and about 7500 Å thick. In one example, profile modulation layer 230 is between about 250 Å and about 1000 Å thick. In one example, STI 225 is between about 1500 Å and about 2500 Å thick. In one example, BOX layer 210 is between about 1500 Å and about 2500 Å thick. In one example, bonding layer 210 is between about 2500 Å and about 3500 Å thick. In one example, bonding layer 365 is between about 2500 Å and about 3500 Å thick. In one example, etch stop layer 360 is between about 250 Å and about 1000 Å thick.
[0045] Substrate 200 may be formed from an SOI substrate by removal of the semiconductor (e.g., silicon) base layer under BOX layer 210 after formation of FETs 240 followed by a deposition of a layer of LTO to form bonding layer 205 on BOX layer 225 . Substrate 300 may be formed from an SOI substrate complete with ILD wiring set 330 followed by deposition of etch stop layer 360 and a deposition of a layer of LTO to form bonding layer 365 .
[0046] In FIG. 2A , a photoresist layer 400 is formed on dielectric layer and patterned to form an opening 405 in the photoresist layer in a manner similar to that described supra for opening 155 in photoresist 150 of FIG. 1B . While no ARC (TARC or BARC) is illustrated in FIG. 2A , an ARC (TARC and/or BARC) may be used.
[0047] In FIG. 2B , an opening 410 is formed through dielectric layer 235 , profile modulation layer 230 , STI layer 225 , BOX layer 210 , bonding layers 205 and 365 and etch stop layer 360 to expose a top surface of wire 350 . Then photoresist layer 400 (see FIG. 2A ) is removed. The methodology is similar to that described supra with respect to the formation of opening 155 E of FIG. 1H . First dielectric layer 235 is RIE'd selective to profile modulation layer 230 using for example, a mixed CO/C 4 F 8 /Ar gas derived plasma when dielectric layer 235 is silicon oxide and profile modulation layer 230 is silicon nitride. This chemistry (at the proper bias, forward and reverse power, pressure and gas flows) etches silicon oxide about 25 times faster than silicon nitride. Second, profile modulation layer 230 is RIE'd selective to dielectric layer 235 and STI 225 , using, for example; a mixed CHF 3 /CF 4 /Ar gas derived plasma when dielectric layers 235 and STI 225 are silicon dioxide and profile modulation layer is silicon nitride. This chemistry (at the proper bias, forward and reverse power, pressure and gas flows) etches silicon nitride about 4 times faster than silicon oxide. It is advantageous to keep profile modulation layer 230 (and etch stop layer 360 ) as thin as possible. Third, STI 235 , BOX layer 210 , bonding layers 205 and 365 are RIE'd selective profile modulation layer 230 and etch stop layer 360 using, for example, a mixed CO/C 4 F 8 /Ar gas derived plasma when STI 235 , BOX layer 210 , bonding layers 205 and 365 are silicon oxide and profile passivation layer 230 and etch stop layer 360 are silicon nitride. The third RIE process is not selective to dielectric layer 235 so opening 410 has a tapered profile in dielectric layer 235 , a substantially straight or slightly tapered profile in STI 225 , BOX 210 , and bonding layers 205 and 365 (compared to the taper of opening 410 in dielectric layer 235 ) because of the presence of profile modulation layer 230 . Fourth, photoresist layer 400 (see FIG. 2A ) is removed using an oxygen ash process. Fifth, etch stop layer 360 is RIE'd selective to dielectric layer 235 . STI 225 , BOX layer 210 and bonding layers 205 and 365 using, for example, a mixed CF 4 /CHF 3 /Ar/O 2 gas derived plasma when etch stop layer 360 and profile modulation layer 230 are silicon nitride and dielectric layer 210 , STI 225 , BOX layer 225 and bonding layers 205 and 365 are silicon oxide. Sixth an optional DC clean using N 2 and H 2 (i.e. a mixed N 2 /H 2 gas derived plasma etch) is performed.
[0048] In FIG. 2C , opening 410 (see FIG. 2B ) is filled with an electrical conductor for an electrically conductive via 420 in electrical contact with wire 350 . In one example, via 420 is formed by deposition of an electrically conductive liner on the sidewall of opening 410 (see FIG. 2B ) and top surface of dielectric layer 235 followed by overfilling the opening with an electrically conductive core conductor. In one example, the conductive liner comprises, in the order of deposition, a layer of TaN, a layer of Ta and a layer of Cu and the core conductor comprises electroplated copper. After filling the opening a CMP is performed to remove the liner and core conductor from over dielectric layer 235 to form the via 420 extending from a top surface 425 of dielectric layer 235 to a top surface of wire 350 . After the CMP, a top surface 430 of via 420 is coplanar with top surface 425 of dielectric layer 235 . Thus via 420 is a damascene via.
[0049] Electrically conductive contacts (not shown) may be made through dielectric layer 235 to the S/Ds and gates of FETs 240 . Alternatively, the contacts may be formed prior to formation of photoresist layer 400 (see FIG. 2A ). Additional interlevel dielectric layer containing wires may be formed on top of dielectric layer 235 , the wires therein electrically connecting via 420 to FETs 240 and FETs 345 into circuits. See FIG. 34 .
[0050] FIG. 3 is a cross-section of additional fabrication steps in the fabrication of three-dimensional integrated circuit according to embodiments of the present. In FIG. 3 , an electrically conductive contact 440 is formed to one of FETs 240 and an ILD wiring set 445 is formed on dielectric layer 235 . ILD wiring level set 445 includes wires 450 and a terminal pad 455 . ILD wiring set 445 is illustrated having two ILD wiring levels. ILD wiring level set 445 may include more or less ILD levels (down to one level containing wires/terminal pads 455 ) or as many levels as required by the integrated circuit design. The ILD wiring levels of ILD wiring set 445 are, by way of example, damascene and dual-damascene ILD levels formed by damascene and dual-damascene processes. Contact 440 is illustrated as a damascene contact. One wire 450 connects contact 440 to contact 420 . Thus a three-dimensional integrated circuit is formed comprising FETs 240 and FETs 345 . It should be understood that ILD wiring level set may be formed over dielectric layer 235 of FIG. 2C to generate a structure similar to that illustrated in FIG. 3 , but where the upper substrate is a bulk silicon substrate instead of an SOI substrate.
[0051] In both the examples of FIGS. 2A through 2C and 3 , silicon layer 215 and BOX 210 is an SOI substrate and silicon layer 315 and BOX is an SOI substrate. It should be understood that substrate 300 may be replaced with a bulk silicon substrate.
[0052] Thus the embodiments provide a process methodology for deep vias and semiconductor devices using deep via structures that have profiles that are less susceptible to metal fill problems.
[0053] The description of the embodiments of the present invention is given above for the understanding of the present invention. It will be understood that the invention is not limited to the particular embodiments described herein, but is capable of various modifications, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, it is intended that the following claims cover all such modifications and changes as fall within the true spirit and scope of the invention.
|
A method of forming a high aspect ratio via opening through multiple dielectric layers, a high aspect ratio electrically conductive via, methods of forming three-dimension integrated circuits, and three-dimensional integrated circuits. The methods include forming a stack of at least four dielectric layers and etching the first and third dielectric layers with processes selective to the second and fourth dielectric layers, etching the second and third dielectric layers with processes selective to the first and second dielectric layers. Advantageously the process used to etch the third dielectric layer is not substantially selective to the first dielectric layer.
| 7
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 11/850,012 filed on Sep. 4, 2007. The disclosure of the above application is incorporated herein by reference.
FIELD
[0002] The present disclosure relates to plasma arc torches and more specifically to devices and methods for controlling shield gas flow in a plasma arc torch.
BACKGROUND
[0003] The statements in this section merely provide background information related to the present disclosure and may not constitute prior art.
[0004] Plasma arc torches, also known as electric arc torches, are commonly used for cutting, marking, gouging, and welding metal workpieces by directing a high energy plasma stream consisting of ionized gas particles toward the workpiece. In a typical plasma arc torch, the gas to be ionized is supplied to a distal end of the torch and flows past an electrode before exiting through an orifice in the tip, or nozzle, of the plasma arc torch. The electrode has a relatively negative potential and operates as a cathode. Conversely, the torch tip constitutes a relatively positive potential and operates as an anode during piloting. Further, the electrode is in a spaced relationship with the tip, thereby creating a gap, at the distal end of the torch. In operation, a pilot arc is created in the gap between the electrode and the tip, often referred to as the plasma arc chamber, wherein the pilot arc heats and subsequently ionizes the gas. The ionized gas is blown out of the torch and appears as a plasma stream that extends distally off the tip. As the distal end of the torch is moved to a position close to the workpiece, the arc jumps or transfers from the torch tip to the workpiece with the aid of a switching circuit activated by the power supply. Accordingly, the workpiece serves as the anode, and the plasma arc torch is operated in a “transferred arc” mode.
[0005] In high precision plasma arc torches, both a plasma gas and a secondary gas are provided, wherein the plasma gas is directed to the plasma arc chamber and the secondary gas is directed around the plasma arc to constrict the arc and to achieve as close to a normal cut along the face of a workpiece as possible. The secondary gas flow cannot be too high, otherwise the plasma arc may become destabilized, and the cut along the face of a workpiece deviates from the desired normal angle. With such a relatively low flow of secondary gas, cooling of components of the plasma arc torch becomes less effective, and piercing capacity is reduced due to splash back of molten metal.
[0006] Improved methods of controlling the secondary gas are continuously desired in the field of plasma arc cutting in order to improve both cut quality and cutting performance of the plasma arc torch.
SUMMARY
[0007] In one form of the present disclosure, a shield device for a plasma arc torch includes an inner shield member defining an inner auxiliary gas chamber and an outer shield member surrounding the inner shield member. An outer auxiliary gas chamber is defined between the inner shield member and outer shield member. The shield device allows an auxiliary gas flow to be split into a first flow of auxiliary gas through the inner auxiliary gas chamber and a second flow of auxiliary gas through the outer auxiliary gas chamber. The inner shield member and the outer shield member are configured to be mounted to the plasma arc torch as an integral unit.
[0008] In another form of the present disclosure, a plasma arc torch includes a tip, a shield device, and a retainer. The shield device includes an inner shield member and an outer shield member. The inner shield member surrounds the tip to define an inner auxiliary gas chamber. The outer shield member surrounds the inner shield member to define an outer auxiliary gas chamber between the inner shield member and the outer shield member. The retainer cap secures the shield device to the plasma arc torch. The shield device allows an auxiliary gas flow to be split into a first flow of auxiliary gas and a second flow of auxiliary gas. The inner shield member and the outer shield member are configured to be mounted to the retainer cap as an integral unit.
[0009] Further areas of applicability will become apparent from the description provided herein. It should be understood that the description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the present disclosure.
DRAWINGS
[0010] The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way.
[0011] FIG. 1 is a cross-sectional view of a distal end portion of a plasma arc torch, including a shield device constructed in accordance with the principles of the present disclosure;
[0012] FIG. 2 is an enlarged cross-sectional view of the distal end portion of the plasma arc torch and the shield device in accordance with the principles of the present disclosure;
[0013] FIG. 3 is a perspective view of one form of the shield device in accordance with the principles of the present disclosure;
[0014] FIG. 4 is an exploded perspective view of one form of the shield device constructed in accordance with the principles of the present disclosure;
[0015] FIG. 5 is top view of the shield device in accordance with the principles of the present disclosure;
[0016] FIG. 6 is a cross-sectional view of the shield device, taken along line A-A of FIG. 5 , in accordance with the principles of the present disclosure;
[0017] FIG. 7 is a cross-sectional view of another form of the shield device constructed in accordance with the principles of the present disclosure;
[0018] FIG. 8 is a cross-sectional view of yet another form of the shield device constructed in accordance with the principles of the present disclosure; and
[0019] FIG. 9 is a cross-sectional view of still another form of the shield device constructed in accordance with the principles of the present disclosure.
DETAILED DESCRIPTION
[0020] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses. It should be understood that throughout the drawings, corresponding reference numerals indicate like or corresponding parts and features. It should also be understood that various cross-hatching patterns used in the drawings are not intended to limit the specific materials that may be employed with the present disclosure. The cross-hatching patterns are merely exemplary of preferable materials or are used to distinguish between adjacent or mating components illustrated within the drawings for purposes of clarity.
[0021] Referring to FIGS. 1 and 2 , a plasma arc torch is illustrated and generally indicated by reference numeral 20 . The plasma arc torch 20 generally includes a plurality of consumable components, including by way of example, an electrode 22 and a tip 24 , which are separated by a gas distributor 26 to form a plasma arc chamber 28 . The electrode 22 is adapted for electrical connection to a cathodic, or negative, side of a power supply (not shown), and the tip 24 is adapted for electrical connection to an anodic, or positive, side of a power supply during piloting. As power is supplied to the plasma arc torch 20 , a pilot arc is created in the plasma arc chamber 28 , which heats and subsequently ionizes a plasma gas that is directed into the plasma arc chamber 28 through the gas distributor 26 . The ionized gas is blown out of the plasma arc torch and appears as a plasma stream that extends distally off the tip 24 . A more detailed description of additional components and overall operation of the plasma arc torch 20 is provided by way of example in U.S. Pat. No. 7,019,254 titled “Plasma Arc Torch,” and its related applications, which are commonly assigned with the present disclosure and the contents of which are incorporated herein by reference in their entirety.
[0022] As used herein, a plasma arc torch, whether operated manually or automated, should be construed by those skilled in the art to be an apparatus that generates or uses plasma for cutting, welding, spraying, gouging, or marking operations, among others. Accordingly, the specific reference to plasma arc cutting torches, plasma arc torches, or automated plasma arc torches herein should not be construed as limiting the scope of the present invention. Furthermore, the specific reference to providing gas to a plasma arc torch should not be construed as limiting the scope of the present invention, such that other fluids, e.g. liquids, may also be provided to the plasma arc torch in accordance with the teachings of the present invention. Additionally, as used herein, the words “proximal direction” or “proximally” is the direction as depicted by arrow X, and the words “distal direction” or “distally” is the direction as depicted by arrow Y.
[0023] The consumable components also include a shield device 30 that is positioned distally from the tip 24 and which is isolated from the power supply. The shield device 30 generally functions to shield the tip 24 and other components of the plasma arc torch 20 from molten splatter during operation, in addition to directing a flow of shield gas that is used to stabilize and control the plasma stream. Additionally, the gas directed by the shield device 30 provides additional cooling for consumable components of the plasma arc torch 20 , which is described in greater detail below. Preferably, the shield device 30 is formed of a copper, copper alloy, stainless steel, or ceramic material, although other materials that are capable of performing the intended function of the shield device 30 as described herein may also be employed while remaining within the scope of the present disclosure.
[0024] More specifically, and referring to FIGS. 2-6 , the shield device 30 comprises an inner shield member 32 that surrounds the tip 24 to define an inner auxiliary gas chamber 34 between the inner shield member 32 and the tip 24 . The inner auxiliary gas chamber 34 directs a first flow of auxiliary gas around the plasma stream 36 as the plasma stream 36 exits the tip 24 in order to constrict and shape the plasma stream, thus improving cut quality and cut speed.
[0025] As further shown, the shield device 30 comprises an outer shield member 42 , which is secured to the inner shield member 32 in one form of the present disclosure. In another form, both the inner shield member 32 and the outer shield member 42 form a single piece such that the shield device 30 is a unitary body. An outer auxiliary gas chamber 44 is formed between the outer shield member 42 and the inner shield member 32 , which directs a second flow of auxiliary gas through a distal end portion 46 of the outer shield member 42 . This second flow of auxiliary gas functions to protect the plasma arc torch 20 during piercing and cutting and also cools components of the plasma arc torch 20 such that thicker workpieces may be processed with a highly shaped plasma stream 36 . Moreover, the second flow of auxiliary gas functions to add momentum to the removal of metal and acts as a buffer between the plasma stream 36 and the outside environment. Therefore, the shield device 30 comprises an inner auxiliary gas chamber 34 and an outer auxiliary gas chamber 44 , which provide multiple injection mechanisms of the auxiliary gas around the plasma stream 36 in order to achieve improved cut quality and speed, in addition to improved life of consumable components. Therefore, the shield device 30 in accordance with the teachings of the present disclosure provides a hybrid injection mechanism for the auxiliary gas.
[0026] As used herein, the term “auxiliary gas” should be construed to mean any gas other than the plasma gas, such as a secondary gas, tertiary gas, shield gas, or other gas as contemplated in the art. Additionally, the first and second flow of auxiliary gas in one form are provided from a single gas source (not shown), and in another form, these auxiliary gases are provided from a plurality of gas sources (not shown). The plurality of gas sources may be the same gas type, such as air, or different gas types, such as, by way of example, air, oxygen, nitrogen, and H35, among others, which may be further mixed as required.
[0027] Referring back to FIGS. 1 and 2 , the shield device 30 is adapted for being secured to the plasma arc torch 20 by a retaining cap 50 , which is in one form threaded onto (not shown) the plasma arc torch 20 , but may also be attached by way of a quick disconnect or other mechanical device. The retaining cap 50 comprises an annular shoulder 52 ( FIG. 1 ) as shown, and an extension 54 around a proximal end portion 56 of the outer shield member 42 engages the annular shoulder 52 of the retaining cap 50 to position the shield device 30 within the plasma arc torch 20 . Referring also to FIG. 6 , the outer shield member 42 further comprises a recessed shoulder 58 disposed around its proximal end portion 56 , and the inner shield member 32 comprises an annular flange 60 disposed around its proximal end portion 62 . The annular flange 60 of the inner shield member 32 abuts the recessed shoulder 58 of the outer shield member 42 as shown to position the inner shield member 32 relative to the outer shield member 42 .
[0028] As further shown in FIGS. 4 and 6 , the outer shield member 42 comprises a proximal inner wall portion 64 , and the inner shield member 32 comprises a proximal outer wall portion 66 . The proximal outer wall portion 66 of the inner shield member 32 engages the proximal inner wall portion 64 of the outer shield member 42 to secure the inner shield member 32 to the outer shield member 42 , in a press-fit manner in one form of the present disclosure. It should be understood, however, that in this form of the shield device 30 having separate pieces, the pieces may be joined by any of a variety of methods, including by way of example, threads, welding, and adhesive bonding, among others. Such joining techniques shall be construed as being within the scope of the present disclosure.
[0029] Referring now to FIGS. 2-6 , the inner shield member 32 comprises gas passageways 70 formed through the annular flange 60 , which are radially spaced in one form of the present disclosure. The gas passageways 70 direct the second flow of auxiliary gas to the outer auxiliary gas chamber 44 . The first flow of auxiliary gas is directed through gas passageways 72 formed through an auxiliary gas distributor 74 , which in one form are oriented such that the first flow of auxiliary gas is swirled as it enters the inner auxiliary gas chamber 34 . Accordingly, the inner auxiliary gas chamber 34 directs the first flow of auxiliary gas around the plasma stream 36 in a swirling manner in one form of the present disclosure.
[0030] As further shown, the outer shield member 42 comprises an exit orifice 80 formed through its distal end portion 46 . A recess 84 is also formed in a distal end face 86 of the outer shield member 42 in one form of the present disclosure, wherein edge extensions 88 function to further protect the inner shield member 32 during piercing and cutting. As an alternative to the orifice 80 , the outer shield member 42 may comprise individual gas passageways (not shown) rather than the orifice 80 as illustrated and described herein, wherein the gas passageways direct the second flow of auxiliary gas around the plasma stream.
[0031] The inner shield member 32 comprises a distal extension 90 , which defines an outer distal wall portion 92 as shown. In one form as shown in FIG. 6 , the exit orifice 80 of the outer shield member 42 is aligned with the outer distal wall portion 92 of the inner shield member 32 . In this form, both the exit orifice 80 of the outer shield member 42 and the outer distal wall portion 92 of the inner shield member 32 are axial, and thus the second flow of auxiliary gas directed through the outer auxiliary gas chamber 44 flows in a coaxial manner in one form of the present disclosure.
[0032] In another form as shown in FIG. 7 , the second flow of auxiliary gas directed through the outer auxiliary gas chamber 44 defines an axial component and a radial component. More specifically, in this form, the second flow of auxiliary gas directed through the outer auxiliary gas chamber 44 is angled inwardly, and the outer distal wall portion 92 of the inner shield member 32 is aligned with the exit orifice 80 of the outer shield member 42 .
[0033] In another form as shown in FIG. 8 , the second flow of auxiliary gas directed through the outer auxiliary gas chamber 44 is angled outwardly. It should be understood with these various forms of the second flow of auxiliary gas, the exit orifice 80 of the outer shield member 42 need not be aligned with the outer distal wall portion 92 of the inner shield member 32 .
[0034] Referring to FIG. 9 , yet another form of the outer auxiliary gas chamber 44 is shown, in which the second flow of auxiliary gas is directed in a radial manner around the plasma stream 36 . It should be understood that such variations for the flow of auxiliary gas through the outer auxiliary gas chamber 44 and the inner auxiliary gas chamber 34 , both individually and in combination with each other, may be employed according to specific operational requirements while remaining within the scope of the present disclosure. Additionally, with each of the forms of directing the second flow of auxiliary gas, namely, coaxial, angled, and radial, the flow may also be directed in a swirling manner with each of these forms. For example, the second flow of auxiliary gas may be coaxial with a swirling component, angled with a swirling component, or radial with a swirling component. Therefore, other components to the second flow of auxiliary gas, and also the first flow of auxiliary gas, other than those set forth herein shall be construed as being within the scope of the present disclosure.
[0035] Therefore, in general, the inner auxiliary gas chamber 34 surrounds at least a portion of the tip 24 and directs a portion of the auxiliary gas flow around the plasma stream 36 in one of a swirling manner and a radial manner. The outer auxiliary gas chamber 44 directs another portion of the auxiliary gas flow around the flow through the inner auxiliary gas chamber 34 in one of a coaxial manner, an angled manner, and a radial manner, each of which may also have a swirling component. Accordingly, the outer auxiliary gas chamber 44 may define a coaxial configuration, an angled configuration, or a radial configuration around a distal end portion of the shield device 30 .
[0036] The description of the disclosure is merely exemplary in nature and, thus, variations that do not depart from the substance of the disclosure are intended to be within the scope of the invention. For example, the inner shield member 32 in one form is recessed from the outer shield member 42 proximate the distal end portion 46 of the outer shield member 42 (e.g., FIGS. 6 and 9 ). In another form, the inner shield member 32 is flush with the outer shield member 42 proximate the distal end portion 46 of the outer shield member 42 (e.g., FIGS. 7 and 8 ). However, although not illustrated herein, the inner shield member 32 may extend beyond the distal end portion 46 of the outer shield member 42 while remaining within the scope of the present disclosure. Therefore, the inner shield member 32 may be recessed, flush, or protruding relative to the distal end portion 46 of the outer shield member 42 and be within the scope of the present disclosure. Such variations are not to be regarded as a departure from the spirit and scope of the invention.
|
A shield device for a plasma arc torch includes an inner shield member defining an inner auxiliary gas chamber and an outer shield member surrounding the inner shield member. An outer auxiliary gas chamber is defined between the inner shield member and outer shield member. The shield device allows an auxiliary gas flow to be split into a first flow of auxiliary gas through the inner auxiliary gas chamber and a second flow of auxiliary gas through the outer auxiliary gas chamber. The inner shield member and the outer shield member are configured to be mounted to the plasma arc torch as an integral unit.
| 7
|
This is a division of application Ser. No. 785,130, filed Oct. 30, 1991, already issued on May 17, 1994 as U.S. Pat. No. 5,312,569.
This invention relates to surface marring of a fiber optic substrate to create a fiber optic backlighting device and, in particular, to the use of rotating rollers for this purpose.
BACKGROUND OF THE INVENTION
Fiber optic substrates are comprised of one or more optical fibers grouped together in a ribbon or panel substrate configuration. Typically, the ribbon or panel substrate is about 0.01 to 0.03 inches thick. If one or more surfaces of the substrate are marred or abraded and a light source is applied to one end of the marred substrate, light will emit from the marred area. Accordingly, such a substrate may be marred to create a specific illumination pattern which can be effectively used to backlight a variety of displays. Increased surface marring also results in increased light emission. Accordingly, light intensity can also be varied along the length of the substrate by varied marring.
Previously, marring of fiber optic substrates was achieved by stamping the substrate with a roughened plate. In particular, a substrate would be placed on a cushion and a stamp having a covering, such as emery paper, would be pressed against the substrate to deform its surface. To increase the amount of surface marring along the substrate, the cushion was placed on a plate having a particular profile. For example, placing the cushion on a plate having an uprising surface, then stamping the substrate against the cushion, would result in minimal marring at the low end of the plate and greater marring at the high end of the plate. This marring pattern was particularly desirable when a single light source was to be applied at one end of the marred substrate. The result would be uniform lighting along the device due to the slight marring near the light source and the progressively greater marring as the distance from the light source increased. A symmetrically curved plate was also used wherein the greatest surface marring occurred at the middle of the substrate. Such a device provided uniform illumination when light sources were placed at both ends of the device. For further details, see U.S. Pat. No. 4,929,169 to Fujigaki et al. entitled Working Equipment For Roughening The Side Of Optical Fiber.
The stamping method described above has a number of disadvantages. One problem is that the length of substrate to be treated at one time is limited by the size of the stamp. Different sized stamps may be used, but larger stamps would obviously require more force to achieve the desired pressure profile against the cushion and plate. Furthermore, as the size of the stamp increases, it becomes more difficult to accurately apply the different simultaneous pressures required to produce a desired marring pattern along the substrate due to the larger cross sectional area of the plate. An additional problem is the necessity to change plates on the apparatus whenever a different marring pattern is desired.
Accordingly, a need has arisen for an apparatus that permits marring of substrates having different lengths or that require different marring patterns without interrupting operation of the apparatus to substitute suitable parts. It is also desirable that such an apparatus be capable of gradually and accurately altering the pressure profile applied to the substrate, again without interrupting operation of the apparatus.
SUMMARY OF THE INVENTION
The present invention is directed to a method and apparatus for marring the surface of a fiber optic substrate by feeding the substrate between a pair of rotating rollers. One of the rollers is coated with an abrasive. The second roller may be hard or have a deformable cover. The second roller may also have an abrasive coating. Alternatively, one or both rollers may be serrated to produce a ripple pattern in the substrate. A hydraulic, pneumatic or other device is used for either manually and/or automatically adjusting the gap between the rollers to alter the pressure and action of the abrasive roller over the length of the substrate being processed. Computer controls may also be used. One or both rollers may be heated to further enhance the marring action. One or both rollers may also be pivotable in a vertical direction to create an angle between the rollers. This results in a larger gap at one end of the rollers than the other causing a gradual increase or decrease of nip or contact pressure along the length of the rollers.
Use of the apparatus and method described herein provides a number of advantages over the prior art. First, because surface marring occurs as the substrate is fed through the gap between the rollers, less force is required to mar the substrate than in the prior art stamping method. The nip or contact pressure line between the rollers is easier to control and accurately maintain than pressure developed across a stamping plate. A further advantage of the present apparatus and method is that any marring pattern may be created on the substrate surface by adjusting the speed of the substrate through the nip and/or altering the pressure in the nip as the substrate moves therethrough and/or creating a pressure differential along the nip or contact pressure line between the rollers. In other words, most any illumination profile along the surface of the substrate is possible.
The use of a cam mechanism to adjust the pressure in the nip is also beneficial. For example, a cam is especially useful in achieving gradual differentiation of surface marring along the substrate. A cam may also be used to give substrates of differing lengths the same illumination profile by simply setting the cam speed appropriately. Additionally, the cam mechanism may be used to transmit a repetitive pressure profile to the nip for making a number of identically treated substrates.
Notably, the above advantages are achieved without the necessity of using different shaped plates or different sized stamps, as required in the prior art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a first preferred embodiment of a marring apparatus according to the present invention.
FIG. 2 is a cross-sectional side elevational view of the marring apparatus taken along line 2--2 of FIG. 1.
FIG. 3 is a cross-sectional front elevational view of the marring apparatus taken along line 3--3 of FIG. 2.
FIGS. 4A and 4B are a cross-sectional front view taken along line 4A--4A of FIG. 1 and a cross-sectional side view taken along line 4B--4B of FIG. 4A, respectively, of means for adjusting the height of the bar disposed through the slot in the rocker arm of the marring apparatus.
FIGS. 5A and 5B are cross-sectional side views taken along line 5--5 of FIG. 1, of the screwing mechanism in an engaged position and a disengaged position, respectively.
FIG. 6 is a cross-sectional side elevational view of a second preferred embodiment of the marring apparatus according to the present invention.
FIG. 7 is a cross-sectional front elevational view of the marring apparatus depicted in FIG. 6.
FIG. 8 is a cross-sectional side view of an alternative embodiment of the rollers.
FIG. 9 is a schematic front elevational view of a second alternative embodiment of the rollers.
DETAILED DESCRIPTION
A preferred apparatus for marring a fiber optic substrate embodying the present invention is shown in FIGS. 1-3 at 10. The apparatus includes a top roller 12, a bottom roller 14, side plates 18 and rocker arms 20. The side plates 18 are secured to a plurality of connecting rods 21, 22, 23 that extend between the side plates 18 for lateral support.
The top roller 12 may be made from low carbon, hot rolled bar, A-36 steel. A bore 15 extends through the top roller 12 for receiving a conventional heating element 28 from a conventional heater 30. Preferably, the heater 30 is sufficient to heat the top roller 12 to about 200° F. The top roller 12 is mounted to the side supports 16 and is driven by motor 17. Preferably, the motor is an adjustable speed DC motor. Alternatively, the roller may be operated manually, as by a handcrank (not shown). The surface 26 of the top roller is roughened or, preferably, covered with a diamond coating or, alternatively, 120 grit sandpaper.
The bottom roller 14 may be made from low carbon-free machining steel. The bottom roller 14 has a shaft 16 that is mounted to rocker arms 20 (see FIG. 3). The shaft 16 may, if desired, extend through openings 19 of the side plates 18 to be operatively engaged to a second motor (not shown). The openings 19 are larger in diameter than the shaft of the bottom roller 14 to permit the bottom roller 14 to move closer to or farther from the top roller 12. It is noted that the motor 17 for the top roller may be used to drive the bottom roller e.g., by the frictional forces between the rollers or by meshing gears between the rollers. Alternatively, only the bottom roller 14 may be driven. In the preferred embodiment, the bottom roller is provided with a deformable covering 24, such as rubber or polyurethane, having 90±3 Durometer, shore A.
A nip or contact pressure line 40 is defined between the top roller 12 and the bottom roller 14. A length of substrate, such as a ribbon A, passes through the nip 40 in the direction of the arrow (see FIG. 2). The direction of the rollers may also be reversed to permit the same ribbon to pass back and forth through the nip. A horizontally disposed piece of sheet metal (not shown) may be secured between the side plates 18 and used to support the ribbon as it passes through the nip 40. A second piece of sheet metal may be used to support the ribbon as it passes out from the nip. A clear plastic safety shield (not shown) may also be placed in front of and over the top roller to prevent an operator from getting his or her fingers caught in the nip.
Referring to FIGS. 2 and 3, the rocker arms 20 are rotatably mounted to pivot rods 42 which cantilever out from and are supported by the side plates 18. Preferably, the pivot rods 42 are secured to the rocker arms 20 adjacent the bottom roller 14 and below the nip 40.
Pressure in the nip may be adjusted through the use of a screw mechanism 46 which acts upon a bar 44 mounted to and extending between the rocker arms 20. Preferably, the bar 44 is secured to the rocker arms at a sufficient distance from the nip to act as a lever when the bar 44 is moved upwardly to increase pressure in the nip.
In the preferred embodiment, an extension 43 of the bar 44 is received in a slot 32 of each rocker arm 20 (see FIGS. 4A and 4B). Each rocker arm also has a vertical bore 34 for receiving an adjustable screw 36 for setting an upper limit to which each extension 43 of bar 44 may move in the slot 32 during application of pressure to the nip. In other words, the height of each end of the bar 44 may be separately adjusted to insure that uniform pressure will be applied in the nip along the length of the rollers. Alternatively, the adjustable screws 36 may be set such that pressure in the nip will increase or decrease along the length of the rollers. This would be beneficial if it was desired to insert a ribbon lengthwise into the nip.
The screw mechanism 46 includes a threaded shaft 48, a knob 50 and a sleeve 52. Referring to FIGS. 5A and 5B, the sleeve 52 has a bore 54 for receiving an end 56 of the threaded shaft 48. The threaded shaft 48 also has a notch 58 for receiving a pin 60 for securing the sleeve 52 to the threaded shaft 48. The notch 58 permits a small amount of relative movement between the threaded shaft 48 and the sleeve 52. A spring 62 may also be provided in the bore 54 of the sleeve to press against the end 56 of the threaded shaft 48.
The bar 44 is provided with a threaded bore 64 for receiving the threaded shaft 48 of the screwing mechanism 46. Connecting rod 22 is provided with a countersunk hole 66 for receiving one end 68 of the sleeve 52. To assemble the screwing mechanism, the knob 50 is screwed onto the threaded shaft 48 which in turn is screwed through the threaded bore 64 of the bar 44. The sleeve 52 is then placed over the end of the threaded shaft 48 and the pin 60 is inserted through the sleeve and into the notch 58 of the threaded shaft. The threaded shaft 48 is then further screwed through the bore 64 until the end 68 of the sleeve 52 engages the countersunk hole 66 of connecting rod 22.
In operation, pressure in the nip 40 is increased by turning the knob 50 to cause the bar 44 to ride up the threaded shaft 48. Thus, the bar 44 acts as a lever causing the rocker arms 20 to rotate clockwise about pivot rod 42, moving the bottom roller 14 closer to the top roller 12 and increasing pressure in the nip. To relieve the pressure in the nip, the knob 50 is turned in the opposite direction.
To prevent heat damage to the polyurethane cover 24 of the bottom roller 14, it is desirable that the top roller 12 be fully disengaged from the bottom roller 14 when the apparatus is not in operation. To fully relieve the pressure in the nip, the knob is turned until the sleeve may be released by an operator from the countersunk hole. The spring 62 may be used to permit the screwing mechanism to be more easily engaged and disengaged from the countersunk hole due to movement of the sleeve 52 relative to the threaded shaft 48 (see FIGS. 5A and 5B).
To mar or abrade a particular length of ribbon, one end of the ribbon is inserted into the nip. As the ribbon passes through the nip, the screw mechanism is manually adjusted to increase or decrease the pressure in the nip. For example, if a 0.01 inch ribbon is intended to be used with a single light source, then the gap between the top roller and bottom roller may be initially set at 0.003 inches and progressively widened to 0.005 inches as the ribbon passes through the nip. This will result in the ribbon having greater marring at the end that passed through the nip first. If two light sources are to be used with the ribbon, one at each end, the operator of the apparatus will insert the ribbon into the nip under low pressure, gradually increase the pressure until the middle of the ribbon is in the nip and then gradually decrease the pressure until marring of the ribbon is completed. Of course, the screw mechanism may be automated and/or programmable to obtain any pressure variation in the nip desired. Other variations in marring patterns may be made by placing only a portion of the ribbon through the nip or by moving the ribbon back and forth in the nip. A second set of non-marring rollers (not shown) may be used to keep pulling the substrate through the apparatus when the first set of rollers 12, 14 is open.
Referring to FIGS. 6 and 7, a second preferred embodiment for altering the pressure in the nip comprises at least one cam wheel 70 mounted on a camshaft 72 (two cam wheels are depicted in FIG. 7). An adjustable speed motor 84 is operatively connected to the camshaft 72. The rocker arms 20 in this embodiment each have a main portion 74 and an extension 76 that extends above each cam wheel 70. Each extension 76 also has a bore 78 for receiving an adjustment screw 80 having a stop 81 for setting the distance between the cam wheel 70 and the rocker arm 20. The surface 82 of the cam wheel may be profiled to impart any desired marring pattern onto a ribbon passing through the nip. Adjusting the speed of the cam wheel permits the same marring pattern to be applied to different length substrates. In FIG. 6, the rocker arm is shown, in phantom, in the disengaged position, i.e., the rocker arm is rotated sufficiently counterclockwise such that the bottom roller is released from the top roller.
Referring to FIG. 8, an alternative embodiment of the present invention is shown with rollers having serrated surfaces 86. The serrations are rounded and the top roller 12 meshes with the bottom roller 14. A substrate B passing through the nip will receive a rippled surface such that when the marred substrate is connected to a lightsource, light will emit from the ripples. Alternatively, only one roller may be serrated. As with the previous embodiments, the pressure in the nip may be adjusted during marring and/or the gap between the rollers may be greater at one end of the roller than the other.
Referring to FIG. 9, a second alternative embodiment of the marring apparatus is shown in schematic form wherein the top roller 12 is horizontal and the bottom roller 14 is pivotable vertically about one end. Pressure in the nip will increase or decrease from one end of the rollers to the other depending upon the angle between the rollers. Alternatively, the top roller 12 or both rollers may be pivotable at one or both ends. The top roller 12 may be rotatably supported from above by supports 96, 98, e.g., by a structural frame or cantilevered beam (not shown). The bottom roller 14 is supported at one end through a flex joint 97 that permits rotation. The other end of the bottom roller 12 is supported by a hydraulic, pneumatic or other lift device 99 that can raise or lower the bottom roller, thus adjusting the angle between the rollers. Alternatively, the bottom roller 14 may be cantilevered. In this case, a lift device 99' may be placed on the shaft 95 of the roller near the flex joint 97. To provide suitable leverage, the shaft 95 may be slengthened.
In this embodiment, it is preferable to insert the substrate, e.g., a ribbon substrate, sideways through the nip. In this manner, the full length of the ribbon may be marred at one time. In particular, ribbon substrates often have a tail 90 at one end comprised of unbound optical fibers that need not be marred. An operator 88 (or supporting equipment) holds the tail 90 of the ribbon substrate and manually feeds the portion 92 of the substrate to be marred sideways between the rollers (the direction of movement of the substrate is into the paper in FIG. 9). This apparatus and procedure creates a marring pattern that gradually increases or decreases in intensity along the length of the substrate without the need for continuously adjusting the nip pressure as the substrate is passed through the nip.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principals and applications of the present invention. For example, the specific mechanisms for adjusting the pressure in the nip are merely representative and are deemed to afford the best embodiments known at this time. As an alternative embodiment, hydraulic or pneumatic devices may be used to directly lift the bottom roller closer to the top roller. Indeed, many other ways of changing pressure in the nip, with or without rocker arms, are known to those skilled in the art. Furthermore, it is to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims.
|
A method and apparatus for marring the surface of a fiber optic substrate by feeding the substrate between a pair of rotating rollers. One of the rollers is coated with an abrasive. The second roller may be hard or have a deformable cover. Alternatively, one or both rollers may be serrated to produce a ripple pattern in the substrate. A hydraulic, pneumatic or other device is used for either manually and/or automatically adjusting the gap between the rollers. One or both rollers may also be heated to further enhance the marring action. A cam mechanism may also be used to adjust the pressure in the nip.
| 8
|
ORIGIN OF THE INVENTION
The invention described herein was made by employees of the United States Government and may be used by or for the Government for governmental purposes without the payment of any royalties thereon or therefor.
TECHNICAL FIELD
The present invention relates to a deployable M-braced truss which can be folded for efficient packaging.
BACKGROUND ART
Many space operations of the future will require the use of long lightweight deployable booms. These booms have application in a number of areas such as a mast to support and accurately position the feed-horn for large antennas, to deploy and provide tension in the blankets of a solar array, or to serve as structural components of a space station or operations center. A number of deployable and/or extendable structural configurations have been proposed in the past, most of which are truss-type structures composed of load carrying axial members (longerons) stabilized by cross-members (battens) and diagonals. The prior art truss configurations have either telescoping or folding longerons connected directly by diagonals, which are generally constructed of cable to facilitate folding and/or packaging. The cable must be pretensioned or the structure will have low shear stiffness until the deformation is adequate to load the diagonal members. However, pretension in the diagonals introduces load in the longerons making them less efficient structural members. Column or compression loads applied to the longerons will also reduce the tension in the wire diagonals.
Some of these problems can be overcome by using diagonals fabricated from members that have bending stiffness adequate to support compression loads. However, trusses with single diagonals may introduce bending or kick loads in the longerons when the truss is loaded in compression. Trusses with cross-diagonals, while eliminating this problem, are more difficult to fold and the diagonals must be adequate to support not only loads introduced by shear, but structural redundancy causes part of the axial load to be introduced in the diagonals. Trusses with folding members also require the lengths of all members to be precisely set and the stiffness of the deployed structure is significantly affected by tolerance in the joints.
STATEMENT OF THE INVENTION
The present invention, is directed toward an efficiently packaged deployable M-braced truss, and eliminates or minimizes the problems of prior art systems. In an M-braced truss, the diagonals intersect at the center of the batten which is more structurally efficient than the traditional truss where diagonals intersect at the batten-longeron intersection. The present invention compactly folds and the diagonals and longerons telescope from a base element. Deployment of the M-braced truss can be performed manually, pneumatically, mechanically, by springs or cables, or by a powered reciprocating mechanism in a conventional manner.
Accordingly, it is an object of the present invention to provide a novel truss structure that can be compactly folded for efficient storage.
Another object of the present invention is to provide a structure that allows packaging of very long truss structures into a single bay area.
Another object of the present invention is a deployable truss structure that can be deployed automatically.
A further object of the present invention is a deployable truss structure that will form a stiff structural column or beam once deployed.
BRIEF DESCRIPTION OF THE DRAWINGS
A more complete appreciation of the invention and many of the attendant advantages thereof will be readily apparent as the same becomes better understood by reference to the following description when considered in connection with the accompanying drawings wherein:
FIG. 1 is a part-schematic view of a compactly folded M-braced truss according to the present invention and having telescoping diagonals and longerons that telescope from a base unit;
FIG. 2 is a view similar to FIG. 1 illustrating the M-braced truss shown in FIG. 1 in partially deployed condition; and
FIG. 3 illustrates the M-braced truss shown in FIGS. 1 and 2 when fully deployed.
DETAILED DESCRIPTION OF THE INVENTION
This present invention has the advantages of a fixed M-braced truss while also permitting the structure of the truss to be collapsed for compact storage. In an M-braced truss, the diagonal members intersect at the center of a batten rather than at the batten-longeron intersection. This structure allows loads introduced in the diagonals to be reacted by batten bending. Movement associated with joint tolerances are eliminated and ensure the geometric accuracy of the deployable beam by using bending of the batten to preload the diagonals. Bending the batten limits the contribution or interaction of load in the diagonal due to applied axial load. However, the diagonals are effective in reacting shear loads because the triangular pattern cannot be distorted without introducing loads in the diagonal members. Therefore, the M-braced configuration effectively separates tension-compression and shear in the structure and permits an efficient structural design.
An important aspect of the present invention is that the diagonals and longerons telescope from a base element, permitting several sections of the truss to be packaged into a single bay section for launch. Referring now more particularly to FIG. 1, the truss structure of the present invention is shown compactly folded and designated generally by reference numeral 10. In the illustrated embodiment the base or first unit 11 of truss 10 includes diagonals 16,18, longerons 20,22 and battens 24,26.
The partially deployed truss 10 as shown in FIG. 2 more clearly illustrates diagonals 12,13, longerons 28,29 and batten 32 which, along with batten 26 of unit 11, constitutes the second or intermediate unit of truss 10. Longeron 32 also connects with diagonals 14,15, and longerons 30,31 which, together with batten 34, forms the third or end unit of the illustrated truss structure 10.
Diagonals 16,18 of the base unit are fixed in the extended position shown while diagonals 12, 13, 14 and 15 in the preferred embodiment are formed of three telescoping segments. Also, the converging ends of diagonals 16,18 are fixed to batten 24 via bracket 38 while the converging ends of diagonals 12,13 and 14,15 are pivotally connected to respective battens 26 and 32. Similarly, the extended ends of diagonals 16,18 are rigidly secured to the respective intersections of longerons 20,22 with batten 26.
Diagonals 12,13 are pivotally connected via pivot pins 40,41, respectively, at their converging ends to a bracket 42 fixed intermediate to batten 26. The extended ends of diagonals 12,13 are pivotally connected via respective pivot pins 44,46 to brackets or ears 45,47 which, in turn, are rigidly secured at the inside area of the rigid corner connection elements 49,51 of longerons 28,29 with batten 32. Corner connection elements 49,51 are formed of two tubular sections welded or otherwise rigidly attached to form a right angle that serves to receive and attach to, respectively, longeron 30, batten 32 and longeron 28; and longeron 31, batten 32 and longeron 29. Similar corner connection elements are provided at each end of battens 24, 26 and 34 but are not elaborated on in the interest of clarity. The vertical leg of corner connection elements 49,51 are provided with transverse openings therein for receiving spring urged latch pins 53,54, respectively, to lock or latch longerons 30,31 in the extended position shown in FIG. 3. The other corner connection elements (not designated) on bottom unit 11 are also provided with similar openings for receiving the spring urged latch pins carried by longerons 28,29. Latch pins 53,54 and those not designated are of similar construction to the conventional latch pins employed on telescoping tent poles.
OPERATION
The operation of the invention is now believed apparent. When the compactly folded M-braced structure is stowed or retracted, it is as shown in FIG. 1. As longerons 28,29 and 30,31 are deployed, the M-braced diagonals 12,13,14,15 are telescopically expanded and formed as the battens 32,34 are moved away from base unit 11 as shown in progress in FIG. 2. Upon full deployment, the longerons 28,29,30,31 are locked in place by latch pins 53,54 and the diagonals 12,13,14,15 are also locked by similar spring urged pins, not designated, to result in three basic M-braced truss segments as shown in FIG. 3.
Although the invention has been described relative to a three-unit embodiment, the number of units is a design choice and any multiple of units needed for a specific final configuration may be employed and are considered within the scope of the present invention.
Deployment of the M-braced truss can be performed manually pneumatically, mechanically by springs or cables, or by a powered reciprocating mechanism. Component members for the M-braced truss may be fabricated from conventional metallic materials or non-metallic materials such as graphite-epoxy.
Further, although the diagonals 12,13,14,15 are formed of three telescoping sections, it is to be understood that this number may be varied as the design dictates. The preferred embodiment utilizes the base segment for each diagonal as a one-half length of the adjacent batten to facilitate compact stowage. Although longerons 20,28,30 and 22,29,31 are by necessity of decreasing size due to the telescope stowage thereof, the individual diagonals for the extended units remain of the same size since each diagonal unit is separately stowed.
Although the invention has been described relative to a specific embodiment thereof, it is not so limited and numerous variations and modifications thereof will be readily apparent to those skilled in the art in the light of the above teaching. For example, although the specific embodiment selected for illustrating the present invention utilizes only two longerons in each segment it is to be understood that the invention is equally applicable to triangular, square or other multi-side truss segments and the beam segments of such structures would employ three, four, or more longerons in each beam or column segment. It is therefore to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described.
|
The disclosure relates to a deployable M-braced truss structure that is efficiently packaged into a compact stowed position and expandable to an operative position at the use site. The M-braced configuration effectively separates tension-compression and shear in the structure and permits efficient structural design. Both diagonals and longerons telescope from an M-braced base unit. They are deployed either pneumatically, mechanically by springs or cables, or by powered reciprocating mechanisms. Upon full deployment, the diagonals and longerons lock into place with a simple latch mechanism.
| 4
|
FIELD OF THE INVENTION
The present invention relates to tubing or casing anchors used in the petroleum recovery industry and, more particularly, to tubing anchors of the type utilized to hang liners from downhole casing and having mating threads between a cone sleeve and a locking sleeve.
BACKGROUND OF THE INVENTION
Liner hangers have long been used in oil and gas recovery operations for suspending or hanging a liner from a well casing. As used herein, the term "liner" means a section of tubing, casing, or similar tubular material to be secured to a larger-diameter downhole tubular generally fixed within the well bore. Included in this definition is a "tieback liner", which is a section of tuving extending upward within the well casing from the hanger, and a "scab liner", which is typically used to repair damaged casing.
A liner normally does not extend to the surface, and is a simple yet highly versatile tubular generally utilized as a cost effective solution to various anticipated or unanticipated downhole problems. Liners may be utilized, for example, to prevent loss of circulation in weak upper zones while drilling with weighted mud to control deeper pressurized zone. Scab liners are frequently used to repair corroded or damaged casing either above or below the liner hanger to allow for continued cost-effective production operations. Liners may also be used to economically conduct cased hole tests of questionable zones, since liners may be "run in" a well much faster than full diameter casing, thereby reducing "trip" time and rig expense. Liners often extend down past the well casing several hundred feet or more into "open hole", and may either be cemented in place or remain supported, solely by the liner hanger.
Mechanically or hydraulically set slips are typically used to effectively interconnect the liner hanger to the casing, and various techniques have been devised for securing a liner to the liner hanger. A fixed interconnection of the liner and the liner hanger is often more difficult to obtain than the casing/liner hanger interconnection, however, and accordingly many prior art liner hangers are intended to cooperate with specially prepared liners. In some instances field welding is used to interconnect the liner with liner hanger components. Other liner hangers require the liners to be threaded with special or "premium" threads, thereby increasing costs and reducing versatility of the liner.
Certain types of liner hangers, such as the Brown Flex Lock liner hanger, does not require special preparation of the liner. These hangers utilize an outer cone sleeve and an inner split-ring locking sleeve with mating threads. Right-hand and left-hand interior threads on the inner locking sleeve bite into the outer surface of the liner as the cone sleeve and a jamb nut are threaded together, thereby causing the locking sleeve to bite the liner. This type of liner hanger allows a customer's standard liner or pipe to be suspended from a casing without modification. The desired axial position of the liner with respect to the hanger can thus be readily adjusted at the well site, and thus this type of Brown liner hanger is accordingly preferred by some customers.
The above described Brown liner hangers are, however, frequently not employed when utilizing hard grades of liners. The "teeth" forming the right-hand and left-hand threads on the inner surface of the locking sleeve are designed to bite into the liner as the outer cone sleeve and a jamb nut are torqued together, but the desired bite has heretofore been difficult to obtain in hard grades of steel liners. Since inadvertent downhole separation of the liner and liner hanger must be avoided to prevent an expensive workover operation, customers often require the more expensive and less versatile liners and hangers when utilizing hard grades of liners.
Threads having a straight buttress thread profile have been provided for mating engagement between the cone sleeve and the inner locking sleeve of the above described Brown liner hangers. While at the surface, the torqued engagement of the cone sleeve and the jamb nut thus provides an axial force which causes the threads on the locking sleeve to slide along the corresponding taper of the thread profile on the cone sleeve, thereby driving the inner teeth on the locking sleeve to bite the liner. When utilizing harder grades of liners, operators may question whether the desired tooth penetration of the locking sleeve to the liner will be obtained to prevent slippage of the liner along the liner hanger as it is lowered into the well. Accordingly, use of the above-described Brown liner hangers has been limited.
If an axially directed load is applied to the Flex Lock liner after it is positioned in the well, a slight additional axial movement between the cone sleeve and the locking sleeve may occur as the locking sleeve continues to slide along the thread profile of the cone sleeve thereby driving the teeth of the locking sleeve into deeper engagement with the liner. This motion is, however, unrestricted since the radial biting force applied by the locking sleeve to the liner may continually increase with an increase in the axial load. Moreover, this continued sliding motion along the taper of the thread profiles results in less threaded engagement between the cone sleeve and the locking sleeve, thereby increasing stress on those components, which may cause failure. Finally, this motion may cause the tapered surfaces of threads on the cone sleeve and locking sleeve to pass completely past each other or "jump" to the next thread, which will then likely continue in rapid fashion until the locking sleeve and cone sleeve separate or fail due to increased stress, again resulting in an expensive workover operation.
The disadvantages of the prior art are overcome by the present invention, and improved methods and apparatus are hereinafter disclosed for interconnecting a downhole casing with a liner.
SUMMARY OF THE INVENTION
The liner hanger of the present invention comprises an outer cone sleeve and an inner locking sleeve, with the locking sleeve including right-hand and left-hand threads on its inner surface for biting engagement with the liner. Improved mating threads are provided on the outer surface of the locking sleeve and the inner surface of the cone sleeve to impart an increased radial force to the liner due to the combination of torqued engagement between the locking sleeve and the cone sleeve, coupled with axial movement of the locking sleeve relative to the cone sleeve upon the application of a significant axial force to the downhole liner section being gripped by the locking sleeve.
Mating threads on the cone sleeve and locking sleeve are each provided with a thread profile having oppositely tapered surfaces. Axial movement of a locking sleeve relative to the cone sleeve in either direction thus forces th locking sleeve radially inward as it moves along an adjoining tapered surface of the cone sleeve, thereby increasing the biting force of the locking sleeve on the liner. The taper of adjoining surfaces for the cone sleeve/locking sleeve threads is between 12° to 28° from the vertical axis, and preferably from about 16° to 24°. Stop surfaces on both the cone sleeve and locking sleeve engage to limit axial movement, thereby maintaining the increased radial forces below a preselected limit.
According to the technique of the present invention, the locking sleeve and cone sleeve are initially made up and torqued together at the surface, thereby creating an initial biting force to secure the locking sleeve to the liner. The liner and hanger are then lowered to their desired position in the well, and the liner hanger is secured to the casing utilizing conventional slips. At this stage, the apexes of the thread profiles on the cone sleeve and the locking sleeve will be substantially aligned in the axial direction.
The desired increased biting force imparted to the liner results from the subsequent application of an axially directed force to the liner, which causes the thread profile apexes to move axially out of alignment as the biting force increases. This application of an axially directed force may occur when the weight of the liner and interconnected downhole components are released to the liner hanger, or may occur as the liner and hanger are being retrieved to the surface. Stop surfaces preferably formed as a portion of the thread profile on the locking sleeve and cone sleeve limit axial movement between these components when an extremely high axial force is applied to the liner, and thus prevent failure of liner hanger components or collapse of the liner.
These and further features and advantages of the present invention will become apparent from the following detailed description, wherein reference is made to the figures in the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 1A is a half sectional view of a liner hanger according to the present invention.
FIG. 2 is a sectional view of the lower cone sleeve shown in FIG. 1.
FIG. 3 is a sectional view of the lower locking sleeve shown in FIG. 1.
FIG. 4 is a pictorial view of a thread profile for the locking sleeve with respect to a thread profile for the cone sleeve when the liner hanger is run into the well.
FIG. 5 is a pictorial view of a thread profile for the cone sleeve with respect to a thread profile for the locking sleeve after the liner hanger of the present invention has been subjected to an axially directed force.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1, a suitable embodiment of a liner hanger 8 of the present invention includes an upper cone sleeve 10, and an upper inwardly-positioned locking sleeve 12 which secures the liner section 14 thereto as explained subsequently. A second lower cone sleeve 10' and a locking sleeve 12' are shown at the lower end of the liner hanger, with these components being identical to those described above but positioned in a mirror image arrangement. It can be seen from FIG. 1 that the liner section 14 is not modified in any manner, and accordingly the axial position of the liner with respect to the hanger 8 can be readily changed.
Three circumferentially spaced downwardly projecting legs 16 affixed to the cone sleeve define respective slip seat pockets 17, into which fit slips 18 in conventional fashion. The slips 18 are circumferentially locked to the cone sleeve 10, and an interlocking tongue and groove arrangement between sides of the slips and the legs allows for axial movement of the slips with respect to the legs 16 along the tongue and groove taper. Axial movement of the slips along the taper brings the threads of the slips into fixed engagement with the well casing 20 in a conventional manner.
Each of the slips 18 may be provided with a projection 22 for fitting engagement in slot 24 in the ring portion 26 of the bow spring or drag block assembly 28, thereby interconnecting the slips to the bow spring assembly. The lower cone sleeve 10' and locking sleeve 12' are similarly interconnected to the bow spring assembly 28 by a conventional J-slot arrangement 30. Either one or two cone sleeves and respective locking sleeves may thus be utilized to secure the liner to the casing.
Those skilled in the art recognize that the liner hanger assembly shown in FIG. 1 is generally representative of conventional liner hanger assemblies, with the exception of the cone sleeve and locking sleeve described subsequently. Tubular lengths of liner are conventionally threaded onto the upper or lower threads of the liner section 14, and various types of "setting tools" may be employed to position the assembly as shown in FIG. 1 at its selected depth in the well bore. Once positioned, frictional engagement of the drag blade assembly 28 with the casing 20 allows the operator to "pick up" on the liner, rotate the liner to the right or left to disengage the J-slot assembly, then "set down" to move the slips 18 downward with respect to legs 16 until the slips move radially outward into biting and secured engagement with the casing 20.
Referring now to FIG. 2, the lower cone sleeve 10' is shown in greater detail to include a body portion 32 with threaded end 34 having tapered thread 36 along an inner surface thereof. Each of the threads 36 may be provided at a spacing of two threads per inch, with each thread profile having an apex 38 formed by the intersection of the adjoining planar and oppositely tapered surfaces 40 and 42, each cut at a preferably identical angle of, e.g., 20° from the vertical. Each of the threads 36 therefore has a thread profile which includes tapered surfaces 40,42 forming an exterior angle outside the cone sleeve of 140°. At the end of each of the surfaces 40,42 opposite the apex is a projection 44, having an upper and a lower stop surface 46,48 (see FIG. 4), each preferably perpendicular to the central axis of the liner. As shown in FIGS. 2 and 4, the projection 44 with planar stop surfaces 46,48 is thus a part of the thread profile for the entire length of thread 36, and thus it should be understood that the projection 44 is a spiraling projection spaced between the spiraling apex 38 of thread 36.
Referring to FIG. 3, sleeve 12' includes similar threads 50 on the outer surface thereof, also spaced at two threads per inch for mating engagement with threads 36. The threads 50 have a thread profile which include tapered surfaces 52,54 which meet at apex 56, with the surfaces 52,54 each being cut at the same angle as threads 36, e.g., 20° from the vertical, thereby forming an interior angle inside the locking sleeve of 40°. A recess 58 which is part of the thread profile 50 defines upper and lower stop surfaces 60,62 (see FIG. 5), which also are generally perpendicular to the central axis of the liner. The recess or slot 58 is thus a spiraling slot spaced uniformly between the spiraling apex 56 of threads 50.
The sleeve 12' also includes conventional right-hand wicker profile interior threads 64, and similar interior lefthand threads 66 separated by spacing 68. Each of the interior threads 64,66 has a conventional geometry for biting into the liner. The threads 64,66 may typically be spaced at four threads per inch, with the interior threads 64,66 each having a thread profile defined by intersecting surfaces each 45° from the vertical, as shown. The threads 64,66 bite into the liner section 14, and are oppositely cut in conventional fashion, i.e., right-hand and left-hand threads, so that the liner section 14 cannot unthread itself from the liner hanger assembly.
The threads 36,50 are each provided along a thread taper of, e.g., 3/4" per foot of threads. This thread taper is provided to inherently cause the locking sleeve to move radially inward as the locking sleeve is threaded into the cone sleeve at the surface, and must be distinguished from the tapered surfaces of the thread profile discussed above. After the interior and exterior threads have been formed on the locking sleeves, each sleeve 12 and 12' may be split along its length with a cut approximately 1/2" wide as shown in FIG. 3, so that the locking sleeve will easily move radially inward as the cone sleeve and locking sleeve are subsequently threaded together.
Referring again to FIG. 2, the axial length of the surface 40 is slightly greater than the axial length of 42, since the length and width of the projection 40 preferably remain constant, yet the thread is tapered slightly radially outwardly as one moves axially away from body 32. Accordingly, each projection 40 is preferably uniformly sized, with a typical projection having a 0.060" axial length and a 0.013" radial width. Referring to FIG. 3, slot 58 between adjacent thread profiles may be approximately 0.125" in length and 0.020" in width, thereby allowing approximately 0.03" of axial movement in either the upward or downward direction between the locking sleeve and the cone sleeve. In order that each slot 58 may also be uniformly sized, the surface 52 is axially slightly longer than the surface 54 to accomodate the taper of the threads. Thus, the maximum movement of cone sleeve 10 relative to locking sleeve 12 is substantially less than the axial spacing of the cooperating threads, as shown in FIGS. 4 and 5.
Referring now to FIGS. 1 and 4, the liner hanger assembly may be assembled at the well site with a torque of approximately 5,000 foot pounds applied between the cone sleeve and the locking sleeve to force the right and left-hand wicker threads 64,66 into biting engagement with the liner 14. The assembly 8 may then be lowered into the well, and the mechanical or hydraulical slips 18 set into fixed engagement with the casing 20 in a conventional manner. As the assembly 8 is positioned in the well and prior to setting of the slips 18, the apexes 38,56 of the threads 36,50 will thus be substantially axially aligned, as shown in FIG. 4. In this position, the spiraling projection 44 will be generally centered in the spiraling slot or cavity 58, and will thus be out of engagement with stop surfaces 60,62.
After setting of the slips 18, a substantially axially directed downward force may be applied to the locking sleeve 12. This force, which typically may be a range from 50,000 pounds axial load to 250,000 pounds axial load, will cause the liner 14 and the locking sleeve 12 as a unit to move axially with respect to cone sleeve 10, thereby bringing the upper planar surface 46 of projection 44 closer toward engagement with upper planar surface 60. This axial movement, in turn, will force the inner threads 64,66 of the locking sleeve into deeper biting engagement with the liner 14 as the planar tapered surfaces of the thread profiles for the threads 36,50 slide with respect to each other. If this axial force were increased, the surfaces 46,60 would eventually engage to prohibit any further axial movement between the cone sleeve and the locking sleeve even if the axial directed force were thereafter increased. This feature of the invention thus limits the added radial inward biting motion of the teeth 64,66 to an extent that will not crush the liner 14 or result in fracture of the cone sleeve or locking sleeve.
The above-described substantial axially-directed force may be applied by various techniques. If the liner 14 has sufficient weight, this force may be applied simply by releasing the liner from the setting tool, so that the weight of the liner itself provides the substantial downward force on the locking sleeves 12 and 12'. A potential slippage problem between the liner and the locking sleeve frequently occurs if the assembly as shown in FIG. 1 were to become stuck as it was being retrieved from a well. During this retrieval operation, a substantial pulling force would typically be imparted to the liner 14 to free the stuck assembly. According to the present invention, this upward force would move the locking sleeve upward with respect to the cone sleeve as the upward force was increased, thus again increasing biting of the teeth 4,66 into the liner section. This increased biting movement would be limited by the engagement of the surface 48 of the cone sleeve with the surface 62 of the locking sleeve, thereby again preventing collapse of the liner 14 or fracture of the tubing anchor components.
Upon the application of the axially directed force, the locking sleeve may typically move 0.03" axially with respect to the cone sleeve, thereby causing the locking sleeve to move radially 0.01" with respect to the cone sleeve. This 0.01" radial separation will typically be shared by swell or expansion of the cone sleeve, and additional radial penetration of the locking teeth into the liner. Although only a portion of this 0.01" exemplary separation may result in radial penetration of the locking sleeve into the liner, this penetration is critical to imparting the necessary increased biting force to the liner.
Mating threads on the cone sleeve and locking sleeve may be sized so that the stop surfaces are engaged when a preselected axial force, e.g., 200,000 pounds, is applied to the liner hanger in either the upward or downward direction. This axial force will thus result in a radial biting force by the locking sleeve into the liner many times the biting force obtained by the initial 5,000 pounds makeup torque. Moreover, this increased biting force is obtained while the locking sleeve remains centered on the liner section. In other words, the axial movement of the cone sleeve with respect to the locking sleeve along the taper of the thread profiles does not cause the locking sleeve to move out of alignment with the liner.
One of the features of the present invention is that the application of the substantial axially-directed force on the liner in either the upward or downward direction results in limited or controlled axial movement between the cone sleeve and the locking sleeve. Thus, the entire threaded length of the cone sleeve and locking sleeve as made up at the surface remains available to withstand the axially-directed force, and to transmit increased biting force to the liner. This increased biting force is applied directly as a result of the axial force which otherwise would tend to cause slippage between the liner and the locking sleeve. Accordingly, the present invention provides increased biting force precisely when it is needed, i.e., when the axially-directed load which otherwise would cause slippage is increased.
It should be understood that opposing tapered surface for the mating threads of the cone sleeve and the locking sleeve define the apex of each thread profile, although those opposing tapered surfaces need not physically intersect to form such an apex. In other words, the planar tapered surfaces 40,42 would define a thread profile apex within the scope of the present invention even if the surfaces 40,42 were axially separated by a short cylindrical surface. Similarly, the tapered surfaces 52,54 need not physically meet at apex 56 to achieve the benefits of the present invention.
The planar surfaces of the thread profiles which slidably engage each other are preferably tapered at substantially the same angle, e.g., 20° relative to the axis of the liner or the liner hanger, so that there is substantially area engagement of these surfaces during axial movement of the cone sleeve relative to the locking sleeve. Also, the opposing taper of each thread profile may be identical, so that the same axially directed biting force on the liner is exerted by equal although oppositely directed axial loads on the locking sleeve. Although a taper of from 12° to 28° is considered within the preferred range, the desired angle of the taper can be altered to increase or decrease the desired radial biting force on the liner for a presumed axial load. Each of the stop surfaces 46, 48, 60 and 62 are preferably perpendicular to the axis of the liner, so that no change in the axially directed force to the liner results from an increase in axial load subsequent to the engagement of respect stop surfaces, as described above.
As a further modification of the invention, it should be understood that the stop surfaces for limiting the axial movement of the locking sleeve with respect to the cone sleeve may be provided on the locking sleeve and cone sleeve separate from the thread profiles, with the stop surfaces nevertheless effectively limiting radial biting force on the liner. The embodiment previously described is preferred, however, since the desired spacing between the stop surfaces need not be adjusted depending on the extent the cone sleeve and locking sleeve are torqued together at the surface. Moreover, the previously described embodiment ensures that the increase in axial load after the stop surfaces engage will be evenly distributed along the length of the mating thread. Also, those skilled in the art will appreciate that the projection portion of the thread profile could be provided on the locking sleeve, and a slot provided on the cone sleeve. In the latter described embodiment, the apex defined by the opposing surface on the locking sleeve would then typically form an interior angle within the locking sleeve of 220°, while the apex defined by the opposing surfaces on the cone sleeve would typically form an exterior angle outside the cone sleeve of 220°.
Finally, the concepts of the present invention may be utilized to secure any tubular to a hanger in a well bore. If the hanger were to secure a tubular larger in diameter than the hanger, the outer sleeve would be provided as a split ring, and its outer cylindrical surface would then include teeth for biting the tubular.
Although the invention has been described in terms of the specified embodiments which are set forth in detail, it should be understood that these are by illustration only, and that alternative embodiments and operating techniques will become apparent to those skilled in the art in view of the disclosure. Accordingly, further modifications are contemplated which can be made without departing from the spirit of the described invention.
|
An improved liner hanger is provided suitable for use with conventional slips to interconnect a downhole casing with a smaller-diameter liner. The hanger comprises an outer cone sleeve and an inner locking sleeve, with the cone sleeve interconnected with the conventional slips, and the locking sleeve having right-hand and left-hand inner biting threads for engagement with the outer surface of a tubular liner section. Improved mating threads are provided on the outer surface of the locking sleeve and the inner surface of the cone sleeve. The cone sleeve and locking sleeve are initially made up at the surface with the apexes of the tapered thread profiles substantially in axial alignment. After the liner hanger is initially positioned downhole, an axially directed downward force on the locking sleeve causes the locking sleeve to slide along the tapered surface of its thread profile with respect to a corresponding tapered surface on the thread profile of the cone sleeve, thereby shifting the apexes out of alignment and moving the biting threads radially inward for increased gripping engagement with the tubular liner section. Stop surfaces on both the locking sleeve and the cone sleeve limit axial movement of the locking sleeve with respect to the cone sleeve and thus prevent excessive radial force, which could otherwise cause failure of the liner hanger components or crush the liner.
| 4
|
BACKGROUND OF THE INVENTION
Recombinant Adeno-associated virus (AAV) vectors are promising gene delivery vehicles because, for example, the virus is not pathogenic; the virus transduces both dividing and non-dividing cells; the virus infects a wide range of cells; and the virus integrates into the genome, which results in long term expression of the transgene.
AAV vector delivery can be obstructed by the immune response of a host to the AAV component proteins. In the case of recombinant AAV vectors, the primary target of the immune response is the capsid of the vector particle since the vectors do not encode viral proteins. For example, virus neutralizing antibodies may be generated in response to exposure to the virus.
SUMMARY OF THE INVENTION
Regions of the AAV capsid proteins were mapped to identify immunogenic sites and regions.
An object of the instant invention is to provide the amino acid sequence of such immunogenic sites and regions.
The sites can be modified, for example, to render the recombinant AAV less immunogenic or non-immunogenic; to alter the tropism of the virus; to enhance binding of the virus to a cell; and to identify analogous sites in related viruses, such as canine parvovirus.
Another object of the instant invention is to provide isolated oligopeptides that can intercede or supplant the attachment of virus and cell. Immunogenic equivalent derivatives thereof also are provided.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 summarizes antibody epitope mapping of AAV. Each box represents a 15 amino acid peptide sequence from AAV VP-1 starting at MAADGY . . . and ending with . . . LTRNL. A total of 91 peptides overlapping by 5 amino acids were used. The VP-2 sequence begins with TAPGK . . . (amino acid 149, peptide 17), and the VP-3 sequence with MATGS . . . (amino acid 203, peptide 25). Blackened boxes represent detection of blocking of antibody binding by that peptide in an ELISA. Blocking peptide numbers are shown for reference above and below the grid. Serum sample designations are shown for reference to the left of the grid. Asterisks mark those sera that were positive for neutralizing antibodies.
FIG. 2 summarizes the location of the immunogenic regions of AAV on the primary sequence of the capsid proteins. Shown is the amino acid sequence of the overlapping VP-1,VP-2 and VP-3 proteins that form the AAV capsid. The arrows indicate the start point of the protein sequences of VP1, 2 and 3. Identified immunogenic oligopeptides are underlined in bold and marked with the corresponding peptide designation. “Lip” denotes the insertion site of 4 amino acids that result in “low infectivity particle yield” mutants. The basic regions proposed to interact with heparin sulphate proteoglycan (HSGP) receptor are marked with a checkered line. The structural regions extrapolated from the canine parvovirus (CPV) structure are marked above the corresponding sequence. ▴: Key residues involved in determining tropism of CPV. Dashed box identifies the VFTDSE sequence recognized by CPV neutralizing dog serum.
FIG. 3 is a schematic representation of the parvovirus structure, adapted from Langeveld et al., infra, that shows the approximate structural locations of the immunogenic oligopeptides. The icosahedral structure (left) is composed of 60 icosahedral units (shaded triangle) formed by VP1, VP2 and VP3. The expanded triangle represents one icosahedral unit.
FIG. 4 summarizes the sequences of immunogenic peptides identified by peptide blocking ELISA experiments. Overlapping sequences from two positive peptides are underlined and shown as putative epitopes, and overlapping sequences from three juxtaposed peptides are double underlined. The shaded area corresponds to peptides that comprise a conformational epitope. Reference 23 is Hermonat et al., infra; 24 is Summerford & Samulski, infra; 17 is Tsao et al., infra; 19 is Langereld et al., infra; 18 is Wikoff et al., infra; 20 is Chang et al., infra; 21 is Parker et al., infra; and 22 is Rutledge et al., infra.
FIG. 5 depicts stretches of amino acids that comprise immunologic determinants.
DETAILED DESCRIPTION OF THE INVENTION
For the purposes of the instant invention, an immunogenic (or antigenic) oligopeptide (or peptide) is one that is recognized and bound by an (AAV) antibody or antiserum. The immunogenic peptide also may be one that interferes with the normal functioning of AAV, such as binding of the virus to the cell surface. The immunogenic peptide may be an epitope, a hapten or an antigenic determinant.
The phrase, amino acid, is meant to relate to the known twenty biocompatible L-amino acids that comprise proteins. The known one letter coding therefor is used herein. “Molecular Biology of the Gene”, J. P. Watson et al., Benjamin Cummins, NY (1987).
Also, any one peptide described herein may be used per se as provided herein or may be modified to form an equivalent immunogenic derivative thereof. The derivative may or may not have the exact primary amino acid structure of a peptide disclosed herein so long as the derivative functionally retains the desired properties of the parent peptide disclosed herein, such as binding to an AAV antibody (or antiserum) or blocking of virus binding to a cell. The modifications can include amino acid substitution with one of the commonly known twenty amino acids or with another amino acid, with a derivatized or substituted amino acid with ancillary desirable characteristics, such as resistance to enzymatic degradation or with a D-amino acid or substitution with another molecule or compound, such as a carbohydrate, which mimics the natural confirmation and function of the amino acid, amino acids or peptide; amino acid deletion; amino acid insertion with one of the commonly known twenty amino acids or with another amino acid, with a derivatized or substituted amino acid with ancillary desirable characteristics, such as resistance to enzymatic degradation or with a D-amino acid or substitution with another molecule or compound, such as a carbohydrate, which mimics the natural confirmation and function of the amino acid, amino acids or peptide; or substitution with another molecule or compound, such as a carbohydrate or nucleic acid monomer which mimics the natural conformation, charge distribution and function of the parent peptide.
Therefore, the equivalent immunogenic derivative peptide may be comprised of amino acids, nucleotides, hydrocarbons, carbohydrates and combinations thereof. For example, a derivative may be comprised of a hydrocarbon containing substituents attached thereto.
The synthesis of a derivative can rely on known techniques of peptide biosynthesis, carbohydrate biosynthesis and so on.
The selection and choice of starting materials to construct the derivative is a design choice of the artisan. As a starting point, the artisan may rely on a suitable computer program to determine the conformation of a peptide of interest. Once the conformation of peptide disclosed herein is known, then the artisan can determine in a rational design fashion what sort of substitutions can be made at one or more sites to fashion a derivative that retains the basic conformation and charge distribution of the parent peptide but may possess characteristics which are not present or are enhanced over the found in the parent peptide.
Once candidate derivative molecules are identified, the next step is to determine which derivatives retain the requisite biologic activity of the parent peptide. That can be accomplished practicing known screening methods, some of which are taught herein. For example, an ELISA wherein AAV binding antibody is immobilized to the solid phase can be used. The candidate peptides can be labeled. Alternatively, cold candidate peptides can be exposed to the solid phase antibody and then labeled AAV subsequently added thereto. Alternatively, the labeled AAV can be replaced with unlabeled AAV and a labeled AAV antibody. It should be evident that a number of permutations are possible.
As to desired characteristics of the peptide derivatives, the endpoint will depend on the eventual use of the derivative. If the derivative is to be used as a hapten for generating AAV antibody, a desirable characteristic is to have one end of the molecule carry a substituent known to be useful for conjugating molecules, for example, to a carrier molecule. Known linking molecules or substituents can be incorporated onto a peptide or peptide derivative for ready conjugation to a carrier molecule.
Another desirable feature would be resistance to peptidases. Therefore, certain amino acids of a peptide can be substituted with a replacement molecule, such as another amino acid, which would make the resulting derivative resistant to a certain peptidase.
Human sera samples positive for reactivity with AAV or monoclonal antibodies directed to AAV can be used in an immunoassay, such as an ELISA, with a capsid peptide library to identify immunogenic oligopeptides that are recognized and bound by such antibodies.
Antibodies can bind to determinants composed of amino acid residues from separated portions of the secondary amino acid sequence that are spatially juxtaposed in a folded protein (conformational epitopes) or to adjacent residues on the amino acid sequence of a protein (linear epitopes). Peptides that could block antibody binding in an ELISA generally identify linear antibody epitopes.
The AAV capsid is composed of three related proteins, VP1, VP2 and VP3 of decreasing size, present at a ratio of about 1:1:10, respectively, and derived from a single gene by alternative splicing and alternative start codon usage. Since VP-2 and VP-3 are subfragments of VP-1,a peptide library of AAV capsid protein VP-1 can be used to identify immunogenic oligopeptides of VP-2 and VP-3 as well. For example, a library composed of, for example, 15-mers overlapping by, for example, 5 amino acids, and thus containing all possible 10-mers of the 735 amino acid sequence of VP-1 can be used.
By practicing that strategy, seven regions of immunogenic sequences were identified in the majority of human serum samples reactive with AAV that were tested, as depicted in FIG. 1 and listed in FIGS. 2, 4 and 5 .
Some peptides blocked antibody binding in all seven patient samples tested (e.g., peptides 4 and 5), some in the majority of patient samples (e.g., peptides 16, 17, 61 etc.) and some in only a few patient samples (e.g., peptide 33).
Several tandem peptide pairs or triplets blocked binding presumably due to a shared, overlapping epitope sequence.
The neutralizing antibody samples can be used to recognize AAV conformational epitopes.
A pool of 14 peptides (peptides 4, 5, 16, 17, 33, 61, 62, 41, 43, 44, 45, 53, 58 and 90) that blocked antibody binding in the ELISA using the human serum samples was tested to detect any relationship between and among peptides. The pool inhibited the neutralizing effect of seven different neutralizing positive sera (Ser3, Ser6, Ser7, Ser13, Ser23, Ser24 and Ser31) to the same extent.
The peptides also reduced AAV uptake, suggesting that the series of peptides contain mimetic sequences involved in the binding of AAV to the cognate receptor thereof on the cell surface. The pool then was divided into two smaller pools of 7 peptides each. Pool 1 contained peptides 4, 5, 16, 17, 33, 61 and 62; and pool 2 contained peptides 41, 43, 44, 45, 53, 58, and 90. Those combinations maintained juxtaposed peptides that likely contain a single conformation epitope or determinant within the same pool.
Pool 2 partially reversed the neutralizing effect. A control “negative pool” of 7 peptides (peptides 7, 8, 9, 10, 11, 12 and 85) showed no inhibition. Removal of peptide 90 from pool 2 had no effect on inhibition implying the core neutralizing pool of peptides to be composed of peptides 41, 43, 44, 45, 53 and 58. The same pattern was observed with five serum samples (Ser3, Ser6, Ser7, Ser23, and Ser24) and also with a neutralizing anti-AAV mouse monoclonal antibody, A20. (Wistuba et al., J. Virology 69, 5311-5319, 1995; 71, 1341-1352, 1997).
The blocking of a neutralizing monoclonal antibody suggests that the identified peptide sequences reconstitute a single conformational epitope. As shown in FIG. 4, an overlap analysis and the expendability of peptide 42 point to sequences KEVT and TSTV as key residues within the conformational epitope.
The immunogenic peptides identified would be expected to be on exposed surfaces of the AAV capsid since neutralizing antibodies generally bind to the virus surface to prevent virus binding to cellular receptors and subsequent viral uptake into the cell.
There is a high structural conservation between AAV and canine parvovirus (CPV), which typifies parvovirus in general. Contact points of AAV with the receptors thereof now are identified (Summerford & Samulski, infra; Summerford et al., Nat. Med. 5, 78-82, 1999; Qing et al., Nat. Med. 5, 71-77, 1999).
The alignment of CPV VP-2 with the AAV sequence (beginning at amino acid 176) and superimposition on the CPV structure thereon (Chapman et al., Virology 144, 491-508, 1993) allow the structural location of the antigenic sites identified herein to be extrapolated between the species.
The three-dimensional structure of CPV has been determined (Tsao et al., Science 251, 1456-1464, 1991). The virus is a T=1 icosahedral structure (depicted in FIG. 3) composed of 60 subunits of VP-1, VP-2 and VP-3 and is characterized by several exposed structural regions that are referred to using previously reported nomenclature (Chapman et al., Tsao et al., supra).
Assuming AAV has a structure similar to CPV, as summarized in FIGS. 2 and 3, several of the B cell determinants identified correspond to exposed regions of AAV.
A “cylinder” structure protrudes from each five-fold axis and is encircled by a “canyon”. Each three-fold axis also has a protruding “spike” formed by 4 loops and each two-fold axis contains a depression termed a “dimple”.
Peptide 33 lies in the canyon and peptides 41-45 are located on the cylinder structure. Peptides 58, 61 and 62 are found on the spike region and peptide 90 is located at the two-fold dimple. In addition, peptide 58 binds monoclonal antibodies (Wikoff et al., Structure 2, 595-607, 1994; Langeveld et al., J. Virology 67, 765-772, 1993) and rabbit sera. Furthermore, that region contains critical residues that have been shown to determine the tropism of CPV (Chang et al., J. Virology 66, 6858-6867, 1992; Parker et al., J. Virology 71, 9214-9222, 1997) and to determine different AAV subtypes (Rutledge et al., J. Virology 72, 309-319, 1998).
AAV mutants that produce 0.01 to 1% of the normal virus yield have been described (Hermonat et al., J. Virology 51, 329-39, 1984). The low infectious particle yield (lip) mutants were generated by random insertion of 8 or 9 base pair sequences which results in an in frame addition of 4 amino acids. Two of the three lip mutations map to and disrupt the peptides described herein, suggesting that those regions form surface exposed domains that are critical for virus binding and uptake.
Furthermore, one of several regions of basic amino acid motifs that have been identified and proposed to interact with the glucosaminoglycan component of HSPG of AAV (Summerford & Samulski, J. Virology 72, 1438-1445, 1998) forms part of peptides 16 and 17 (FIG. 2 ).
The peptides identified herein are bound by AAV neutralizing antibodies and inhibit binding of viruses to cells of a host.
As taught hereinabove, the actual amino acid sequence of any one peptide can be varied to yield an immunogenic derivative, for example, by removing one or more amino acids; adding one or more amino acids;
substituting one or more amino acids; or any combination thereof. Moreover, the peptide can be mimicked by another molecule or polymer, such as a carbohydrate or a hydrocarbon. The determinative factor is whether the derivative of a specific peptide retains the distinguishing characteristics thereof, such as, binding to an AAV antibody (or antiserum) or blocking binding of AAV to a host cell.
A reduction in the distinguishing characteristic of up to 50% of that observed for the parent peptide is tolerable in the derivative, particularly if the derivative has other desirable characteristics, such as degradation resistance. Thus, for example, if a peptide is observed to bind antibody to a certain extent, or is observed to inhibit binding of AAV to a cell at a certain level at a certain concentration, a decrease of up to 50% of the observed value of the parent molecule can be found in a derivative within the scope of the instant invention
A suitable way to determine if a derivative is usable in the practice of the instant invention is to use known methods as taught herein, or equivalent methods, which demonstrate the immunogenicity and function of a peptide of the AAV capsid proteins. Therefore, an immunoassay, such as an ELISA, RIA, neutralization assay and so on can be used. Also, an assay that demonstrates binding of virus to a cell can be practiced. Those such assays can afford the necessary comparison of a derivative and the parent peptide.
As taught herein, suitable derivatives are those which are found to carry desirable characteristics. For example, the oligopeptides may be manipulated to find derivatives that are less immunogenic or not immunogenic. When such derivatives are identified, the changes can be configured into the capsid coding sequence of a recombinant AAV using known techniques resulting in the production of virus which will not evoke a strong or any host immune response thereto.
Also, alteration of an oligopeptide may influence the binding of a virus to a cell. A desirable characteristic would be a change that enhances binding of virus to a cell. Another desirable characteristic would be change that influences the tropism of the virus. Controlling the tropism of the virus would enable tissue-specific targeting of the viral vector. Again, once the desired change is identified, the coding sequence of the capsid proteins can be modified so that the expressed capsid proteins of the recombinant virus carry the same desirable change found in any one derivative.
Also, as noted herein, the parvoviruses share a similar structure and function. Therefore, identification of immunogenic peptides in one species of parvovirus will enable identification of similar sites in other parvoviruses, as noted herein.
The oligopeptides of interest will find use in in vitro methods, such as purification schemes. For example, oligopeptides that inhibit binding of virus to receptor can be used as competitive inhibitors to release bound virus in an adsorption-type assay. The same may apply if antibody were used as an immunoadsorbent, an oligopeptide could be used to elute bound virus from a solid support to which AAV antibody is immobilized.
The peptides, and particularly certain immunogenic derivatives thereof, may find use in vivo. Also, the sequence of modified peptides can be incorporated into the capsid sequence of a recombinant AAV by subcloning a polynucleotide encoding such a modified peptide into the nucleic acid encoding a capsid protein. The polynucleotide can replace the sequence found in the wild-type capsid nucleic acid. Methods for manipulating pieces of nucleic acids are known. Methods for making recombinant AAV are known in the art. Moreover, methods for administering peptides or AAV are known in the art. The amounts of peptides or rAAV to be administered to a host in need of treatment will have been determined for the unmodified AAV. Because the peptides of the instant invention, if the sequences therefor are incorporated into a virus, would be, for example, less immunogenic, a lower dosage can be used. An artisan would determine the appropriate new dosage by extrapolating from pre-clinical data or clinical data. Regarding the dosing of peptides, again the artisan would follow accepted methods of extrapolating from pre-clinical and clinical studies. As some derivatives may be stable, that is, resistant to degradation in the host, the long term dosing would have to be adjusted to take those charasteristics into account. The amount of peptide or virus in the host can be determined by sampling, for example, a blood specimen or a tissue biopsy, and determining the levels thereof therein using known techniques, such as those taught therein.
Preclinical and clinical data are used in formulating a range of dosing for human use. The dose may vary depending on the form used and the route of administration. The artisan will know how to make necessary adjustments.
Pharmaceutical compositions comprising AAV may be formulated as known using physiologically acceptable carriers, diluents or exicipients.
The AAV preparations are formulated for administration by any of a variety of routes, such as, inhalation, oral, buccal, parenteral or rectal administration.
For administration by inhalation, the AAV can be delivered as an aerosol spray from pressurized packs or a nebulizer, with the use of a suitable propellant.
For oral administration, the pharmaceutical compositions may take the form of, for example, tablets, lozenges or capsules prepared by conventional means with pharmaceutically acceptable excipients, such as binding agents; fillers; lubricants; glidents; disintegrents; or detergents. The tablets may be coated.
Liquid preparations may take the form of, for example, solutions, syrups or suspensions, or a dry product for constitution with water or other suitable vehicle before use. The liquid preparations can contain pharmaceutically acceptable additives such as suspending agents; emulsifying agents; non-aqueous vehicles; and preservatives. The preparations may also contain buffer salts, flavoring, coloring and sweetening agents.
Preparations for oral administration may be suitably formulated to provide controlled release of the active compound.
The AAV may be formulated for parenteral administration by injection, for example, by bolus injection or infusion. Formulations for injection may be presented in unit dose, for example, in ampoules or in multidose containers, with an added preservative. The compositions may take such forms as suspensions, solutions or emulsions in oily or aqueous vehicles as needed, and may contain additives such as suspending, stabilizing and dispersing agents. Alternatively, the active ingredient may be in a powder or a lyophilized form for constitution with a suitable vehicle, for example, sterile pyrogen-free water, before use.
The AAV also may be formulated for long term release. Such long acting formulations may be administered by implanation (for example, subcutaneously or intramuscularly) or by intramuscular injection. Thus, for example, the therapeutic compounds may be formulated with suitable deposition material, for example, an emulsion.
The compositions may, if desired, be presented in a pack or dispenser device which may contain one or more unit dosage forms containing the active ingredient. The pack may, for example, comprise metal or plastic foil, such as a blister pack. The pack or dispenser device may be accompanied by instructions for administration.
The invention now will be exemplified in the following non-limiting examples.
EXAMPLE 1
Construction and Production of AAV Vectors
AAV vectors expressing green fluorescent protein (GFP) (Klein et al., Exp. Neurol. 150, 183-194, 1998), β-galactosidase (McCown et al., Brain Res. 713, 99-107, 1996) and hFIX were constructed and generated using known techniques, such as taught in Snyder et al., (Nat. Genet. 16 (1997) 270-272). Titers were determined by dot blot analysis.
EXAMPLE 2
Detection of Anti-AAV Antibodies using ELISA
Ninety-six well MaxiSorp flat surface Nunc-Immuno plates were coated with 5×10 7 particles of AAV in 1000 μl/well of 0.1 M carbonate buffer pH 9.6, incubated overnight at 4° C. and washed twice with washing buffer from an AMPAK amplification kit (DAKO, Carpenteria, Calif.). After blocking with 3% BSA in washing buffer for 2 hours at room temperature, the plates were washed once and incubated for 1 hour at room temperature with donor serum at 1:100 dilution in washing buffer, 1% BSA in a total volume 100 μl/well. Next, the plates were washed 5 times and AP conjugated mouse anti-human antibodies (Zymed, San Francisco, Calif.) were added at 1:800 dilution in washing buffer, 1% BSA, 100 μl/well. The plates were incubated for 1 hour at room temperature and washed with washing buffer 4 times. For color development and further amplification of the signal, the AMPAK amplification kit was used. Absorbance was measured at 490 nm.
EXAMPLE 3
Detection of Neutralizing Anti-AAV Antibodies
293 cells were seeded in a 24 well plate at a density of 1×10 5 cells per well, in 1 ml of IMDM media (JRH). The cells were allowed to adhere for 2 hours at 37° C. The media then was removed by aspiration before 6×10 6 particles of adenovirus dl309 (Ferrari et al., J. Virology 70, 3226-3234, 1996), were added in a final volume of 200 μl per well. The cells were incubated further at 37° C. for 1 hour and then washed twice in the same media before the following mix was added. AAV-GFP (1 μl=5×10 8 total particles or 9×10 6 transducing units) virus was incubated with serum sample diluted in PBS for 2 hours at 4° C. in a total volume of 25 μl. The final dilution of the test serum was 1:100 or 1:1000. The mix was added to the washed cells in a final volume of 200 μl, and incubated for 1 hour at 37° C. About 400 μl of media then were added to each well and cells were incubated overnight. Cells were collected, washed in PBS/BSA (1%), and analyzed by FACS. The % inhibition was calculated using a “no antibody” control sample as a reference. Another control was anti-AAV guinea pig sera that showed maximal inhibition.
EXAMPLE 4
Epitope Mapping of Anti-AAV Antibodies
A set of 91 overlapping peptides (15 mers) spanning the entire 735 amino acid AAV-VP1 capsid protein sequence (Genbank #AF043303) were synthesized using the PIN synthesis strategy (Chiron Mimotopes, Clayton, Australia). The peptide sequences overlap by 5 amino acids thus generating all possible 10 mers of VP-1. Two control peptides also were synthesized to verify purity and assess yield. Peptides were resuspended in PBS at a concentration of 5 mg/ml and stored at −20° C.
ELISA analysis was performed in the presence of 1 μl (corresponding to a final concentration of approximately 20 μM) of individual peptides or 10 μl peptide pools which were present at the antibody incubation stage. Similarly, 1 μl of each peptide was added to the 25 μl antibody-AAV-GFP mix in the neutralizing assay to assess the ability to block the binding of neutralizing antibodies to AAV-GFP.
All references cited herein are incorporated by reference in entirety.
It will be readily evident to the artisan that various changes and modifications can be made to the teachings herein without departing from the spirit and scope of the instant invention.
|
Polypeptides of adeno-associated virus (AAV) that bind to AAV antibodies or block binding of AAV to mammalian cells are described. Derivatives of peptides can be less immunogenic, enhance binding to cells, render a virus tissue specific and so on. The nucleic acid sequence encoding those derivatives can be incorporated into a capsid encoding sequence to enable a virus to express such a derivative and be less immunogenic, have enhanced transduction efficiency or be tissue specific.
| 2
|
This is a continuation of application Ser. No. 342,482, filed on Apr. 24, 1989, now abandoned, for a METHOD OF TREATING CONSTRUCTION JOINT IN TOP-DOWN CONSTRUCTION METHOD.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a method of treating construction joints in a top-down construction method in which an injection hole is intentionally formed in a minute clearance which is produced in vertical construction joints of concrete pillars, walls and the like in the case where the up-down construction method is applied to the underground construction of buildings (a clearance produced between an upper concrete and a lower concrete, which is constructed below the upper concrete, due to the sinking of a surface of the lower concrete by the rise of a bleeding water) and an injection material, such as cement paste containing expansive additive and non-shrinkage additive, is injected through said injection hole to integrally construct the upper and lower concretes.
BRIEF DESCRIPTION OF THE PRIOR ART
Frequently some clearance is produced between an upper concrete and a lower concrete due to the sinking of a surface of the lower concrete by the rise of a bleeding water in vertical construction joints created by top-down concreting but also a laitance is accumulated in an upper portion of the clearance however carefully the lower concrete may be constructed.
Accordingly, it has been necessary that the above described construction joints be subjected to some treatments to fill up the above described clearance, whereby the upper and lower concretes are integrated.
One of these treatment methods is a so-called "injection method".
This "injection method" includes: a method, in which the lower concrete C 2 is constructed and then the injection hole 2 is formed from the direction crossing the construction joints by means of a drill, as shown in FIG. 10(A); a method, in which the injection hole 2 is formed along the construction joints by means of a drill and the injection materials, such as cement paste containing expansive additive, epoxy resin and isocyanate resin, are injected through said injection hole 2, as shown in FIG. 10(B); and a method, in which an injection groove 8 opening downward is previously formed in the bottom surface S 1 of the upper concrete C 1 and the lower concrete C 2 is constructed and followed by injecting the similar injection materials 3 through said injection groove 8, as shown in FIG. 11.
However, in the above described methods, in which the injection hole 2 is formed by the use of a drill, steel frames and the like exist within the construction joints, so that a deep hole can not be drilled, and as a result, the injection is conducted merely in portions close to the surface, whereby the injection can not be achieved up to surroundings of the internal steel frames according to the particular circumstances.
In addition, in the method in which the injection groove 8 is previously formed, the injection groove 8 is stopped up by constructing the lower concrete C 2 , whereby the injection is impossible or incomplete in many cases.
The present inventor has proposed an "injection method" capable of eliminating the above described disadvantages in Japanese Patent Publication No. Sho 58-5346 (Japanese Patent No. 117639).
This is a method of treating construction joints, in which a lower concrete C 2 is constructed below an upper concrete C 1 under the condition that a framework 1 for forming an injection hole is mounted on a bottom surface S 1 of said upper concrete C 1 , as shown in FIG. 12(A) to (D), and after the lower concrete C 2 is set, said framework 1 is taken off to form the injection hole 2 followed by injecting the injection materials 3, such as cement paste containing expansive additive, through said injection hole 2. Referring to FIG. 12, reference numeral 4 designates a framework for the lower concrete.
In addition, a measure for taking off the framework 1 for forming an injection hole includes a method, in which said framework 1 is pulled out, and a method, in which said framework 1 is dissolved in solvents.
The present inventor has conducted many experiments aimed at the practical use and the still further improvement in reliability of the method of treating construction joints in the up-down construction method proposed in Japanese Patent Publication No. Sho 58-5346 and found from the results of these experiments that the following problems occur according to a longitudinal sectional shape of the framework 1 for forming an injection hole in the above described method.
That is to say, in the case where the longitudinal section of the framework 1 for forming an injection hole has a circular shape, a shape with rounded corners on right and left side surfaces S and the upper surface S' or a trapezoidal shape, as shown in FIG. 13, even though the lower concrete C 2 is set followed by taking off (pulling off or dissolving) the framework 1 to accurately form the injection hole 2, the injection material 3 has been incompletely injected. The reason for this is that when a surface S 2 of the lower concrete C 2 is settled with the rise of bleeding water, the settlement of concrete portions positioned above the right and left side surfaces S of the framework 1 (portions designated by marks (a), (a) in FIG. 14,) is hindered by said side surfaces S, whereby said concrete portions (a), (a) are set under the condition that they are brought into close contact with or close to the bottom surface S 1 of the upper concrete C 1 , and as a result, the continuity of the injection hole 2 and the clearance in the construction joint is deteriorated, whereby the injection material 3 can not be injected into the clearance through the injection hole 2.
Also in the case where the section of the framework 1 has a regular square shape or similar and both the right and left side surfaces S of the framework 1 meet at right angles with the bottom surface S 1 of the upper concrete C 1 , the similar problem has occurred according to circumstances.
That is to say, the bottom surface S 1 of the upper concrete C 1 is inclined for easy escaping of bleeding water and air bubbles, as shown in FIG. 12, so that, if the framework 1 is installed obliquely relative to the inclination of the bottom surface S 1 or the bottom surface S 1 is inclined in right and left directions due to the poor assembling accuracy of the framework for the upper concrete, as shown in FIG. 15, both the right and left side surfaces S of the framework 1 do not become vertical planes but have an inclination even though they meet at right angles with the bottom surface S 1 .
Accordingly, in these cases, when the surface S 2 of the lower concrete C 2 is settled, the settlement of a portion positioned above one side surface S of the framework 1 (a portion designated by a mark (a) in FIG. 15) is hindered, whereby the similar problem to the above described one occurs on one side of the injection hole.
The present invention has been achieved in view of the above described knowledge. Thus, it is a main object of the present invention to improve the continuity of an injection hole and a clearance in construction joints and completely carry out the injection of injection materials up to the depths by a remarkably simple construction in which merely a sectional shape of a framework for forming an injection hole is devised.
It is another object of the present invention to make angles formed between both side surfaces of the framework and a bottom surface of an upper concrete obtuse whichever surface of the framework for forming an injection hole is, stuck to the bottom surface o the upper concrete, thereby improving the continuity of the injection hole and the clearance in construction joints and getting along without paying attention so as not to misinstall the framework for forming an injection hole.
It is a further object of the present invention to make the formation of the injection hole by taking off the framework and the direct injection of injection materials onto a back side of a steel frame possible even though the framework for forming an injection hole is arranged under the condition that it is bent so as to go around the steel frame and the like.
It is a still further object of the present invention to curtail a quantity of solvents used for taking off said framework in spite of the use of the framework for forming an injection hole having a sufficient size.
In order to achieve the above described objects, the present invention takes the following measures. That is to say, the present invention provides a method of treating construction joints in the top-down construction method, in which a lower concrete is constructed below an upper concrete under the condition that a framework for forming an injection hole in a bottom surface of said upper concrete, after said lower concrete is set, said framework being removed to form an injection hole, and an injection material, such as cement paste containing expansive additive and non-shrinkage additive, being injected through said injection hole, characterized by that said framework for forming an injection hole is brought into close contact with or close to the bottom surface of said upper concrete at upper sides of both right and left side surfaces thereof and has a longitudinal sectional shape so that an angle formed between said both right and left side surfaces and the bottom surface of said concrete may be obtuse.
The longitudinal sectional shape of the framework for forming an injection hole meeting the above described conditions includes an inverted trapezoidal shape, a semicircular shape and similar one but it is effective to select the regular triangular longitudinal sectional shape of the framework for forming an injection hole by the reason which will be mentioned later.
In addition, the framework for forming an injection hole may be removed by pulling off said framework but it is effective to dissolve with solvents for the reason which will be mentioned later.
In this case, the framework for forming an injection hole may be solid or hollow but the latter is desirable for the reason which will be mentioned later.
With the above described construction, since the upper edges of both the right and left side surfaces of the framework for forming an injection hole is brought into close contact with or close to the bottom surface of the upper concrete, a part of the lower concrete does not go around onto the upper surface side of the framework for forming an injection hole when the lower concrete is constructed below the upper concrete.
Since the angle formed between both the right and left side surfaces of the framework for forming an injection hole and the bottom surface of the upper concrete is obtuse, the natural settlement of the concrete portions brought into contact with both the right and left side surfaces of the framework by the gravity is not hindered by both right and left side surfaces when the surface of the lower concrete is settled with the rise of a bleeding water.
Accordingly, the continuity of the injection hole formed by removing said framework for forming an injection hole and the clearance in the construction joints can be secured.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing one example of a framework for forming an injection hole used in the present invention;
FIGS. 2(A) to (C) are longitudinal sectional views showing the principal parts to explain an injection treatment method of construction joints by the use of said framework;
FIGS. 3 to 7 are longitudinal sectional views showing the principal parts to explain other preferred embodiments of the present invention;
FIG. 8 is a cross-sectional plan view showing the principal parts int he basement of buildings to explain an example of the arrangement of the framework for forming an injection hole;
FIG. 9 is a perspective view showing an extractable framework for forming an injection hole according to another preferred embodiment of the present invention;
FIGS. 10(A), (B), and 11 are longitudinal sectional views showing the principal parts to explain the conventional methods.
FIGS. 12(A) to (D) are longitudinal sectional views used for an explanation of another conventional method and the present invention;
FIGS. 13 to 15 are diagrams of points at issue in the conventional methods.
BRIEF DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preferred embodiments of the present invention will be described below with reference to FIGS. 1 to 9 and FIGS. 12(A) to (D) used for the explanation of the conventional method.
As shown in FIG. 1, the framework 1 for forming an injection hole formed of synthetic resins, such as foam styrene, and having the appointed longitudinal sectional shape (for example, inverse trapezoidal shape) is stuck to the bottom surface S 1 of the upper concrete C 1 by the use of adhesives, adhesive tapes and the like, as shown in FIG. 12(A). Under this condition, as shown in FIG. 2(A), the upper sides of both the right and left side surfaces S of said framework 1 are brought into close contact with or close to said bottom surface S 1 . In addition, as shown in FIG. 2(A), the obtuse angle θ is formed between said both right and left side surfaces S and said bottom surface S 1 .
Subsequently, as shown in FIG. 12(B), a suitable framework 4 is constructed below the upper concrete C 1 and the lower concrete C 2 is cast.
The surface of the lower concrete C 2 is gradually settled with the rise of bleeding water but the obtuse angle θ is formed between both the right and left side surfaces S of the framework 1 for forming an injection hole and the bottom surface S 1 of the upper concrete C 1 , so that both the right and left side surfaces S do not hinder the settlement of the surface of the lower concrete C 2 , as shown in FIG. 2(B), and also the concrete portions brought into contact with both the right and left side surfaces S are almost uniformly settled.
After the lower concrete C 2 is set, said framework 4 is dismembered and the solvents, such as thinner, are poured into the position of the framework 1 for forming an injection hole to dissolve said framework 1, whereby forming the injection hole 2, as shown in FIG. 12(C). As above described, also the concrete portions brought into contact with both the right and left side surfaces S are almost uniformly settled, so that the injection hole 2 can be surely connected with the clearance of the construction joint.
Then, the injection material 3 is injected through said injection hole 2, as shown in FIG. 12(D). In this case, as above described, the superior continuity is achieved between the injection hole 2 and the clearance, so that the injection material 3 can be surely injected into the clearances on both sides through the injection hole 2.
In addition, dissolved leavings of the framework 1 for forming an injection hole are almost negligible in quantity, so that the injection material 3 may be injected immediately after the dissolution of the framework 1 but water may be poured into the injection hole 2 prior to the injection of the injection material 3 to wash the injection hole 2 and the clearance. Resinous injection materials, such as epoxy resins and isocyanate resins, and cement pastes containing expansive additive and non-shrinkage additive can be used as said injection material 3. Any synthetic resin soluble in the solvents without leaving harmful substances can be used as a material of the framework 1 for forming an injection hole formed of synthetic resins. A typical example is foam styrene. Aromatic solvents, such as thinner, toluene, benzene and xylene, halogenated hydrocarbons, such as ethylene dichloride and trichloroethylene, ethers, such as butyl acetate, and the like, that is, various kinds of substance, can be used as the solvents.
The longitudinal sectional shape of the framework 1 for forming an injection hole may be triangular, as shown in FIG. 3, or may be semicircular or similar, as shown in FIG. 4. In addition, as shown in FIG. 5, the vicinity of the upper sides (p) of both the right and left side surfaces S may be pleated so as to be elastically deformed, whereby the pleated portion is continued to be brought into close contact with the bottom surface S 1 by the elastic stability thereof under the condition that the upper surface S' of the framework 1 is stuck to the bottom surface S 1 of the upper concrete C 1 .
FIG. 6 shows another preferred embodiment of the present invention. This preferred embodiment is characterized by the quantity of the solvents used being reduced with securing the thickness necessary for the formation of said injection hole 2 by forming the framework 1 for forming an injection hole in a hollow shape (a shape having a hollow portion 1').
FIG. 7 shows a further preferred embodiment. This preferred embodiment is characterized by the longitudinal sectional shape of the framework 1 for forming an injection hole being regular triangular so that the above described condition may be satisfied whichever surface is stuck to the bottom surface S 1 . The hollow portion 1' intends to reduce the quantity of the solvents used in the same manner as in the preferred embodiment shown in FIG. 6.
In the above described respective preferred embodiments, the framework 1 for forming an injection hole is removed by dissolving said framework 1 with the solvents, so that it is not required to arrange the framework 1 linearly. Accordingly, as shown in for example FIG. 8, the bent injection hole 2 can be formed to directly inject the injection material on the back side of the steel frame 5. In addition, in the case where the injection hole 2 is formed in the construction joint of an underground outer wall 6, the inclined arrangement of the respective frames 1 in the same direction is effective for uniformly injecting the injection material into the clearance of the construction joint, as shown in FIG. 8. Referring to FIG. 8, reference numeral 7 designates a barrier-wall.
In addition, after the lower concrete C 2 is set, the framework 1 for forming an injection hole may be pulled out to form the injection hole 2. For example, the framework 1 is formed of materials, to which concrete is not stuck, or the surface of the framework 1 is coated with grease, that is, the framework 1 is subjected to a suitable measure for preventing concrete from sticking thereto, and after the lower concrete is set to some extent, in short, at a point of time when it is still early to dismember the framework 4 for use in the lower concrete but the molding is possible because no big force is applied to the construction joints from above, the framework 1 can be pulled out from a hole which is previously formed in said framework 4 to form said injection hole 2.
In addition, if the framework 1 for forming an injection hole comprising a resinous tape 1a spirally wound in an appointed sectional shape is used, as shown in FIG. 9, the overlap of the resinous tape 1a is reduced and the diameter of the framework 1 is reduced by pulling one end of the framework 1 in the axial direction so that it can be pulled out by a slight force even after the lower concrete is completely set. Although it is not shown, if the framework 1 for forming an injection hole is formed of rubber, its diameter is reduced by pulling one end thereof, so that it can be easily pulled out even though it has a sectional shape as shown in FIGS. 2 to 7.
According to the present invention, since the upper sides of both the right and left side surfaces of the framework for forming an injection hole are brought into close contact with or close to the bottom surface of the upper concrete, a part of the lower concrete does not go around up to the upper surface side of the framework for forming an injection hole when a lower concrete is constructed below an upper concrete, and, since the angles formed between both the right and left side surfaces of the framework for forming an injection hole and the bottom surface of the upper concrete are obtuse, the settlement of the concrete portions brought into contact with both the right and left side surfaces of the framework is not hindered by said right and left side surfaces when the surface of the lower concrete is settled with the rise of bleeding water.
Accordingly, the continuity between the injection hole, which is formed by removing said framework for forming an injection hole, and the clearance of construction joint can be secured to completely inject the injection material.
In one method, the longitudinal sectional shape of the framework for forming an injection hole is a regular triangle, so that the angles formed between both the right and left side surfaces of the framework and the bottom surface of the upper concrete are obtuse whichever surface of said framework is stuck to the bottom surface of the upper concrete. Accordingly, it is not required to pay attention so that the framework may not be misinstalled and thus the efficiency and reliability of the installation of the framework are improved.
Since the framework for forming an injection hole is removed by dissolving it with solvents, it is not required to give the extractable shape to the framework. Accordingly, for example the framework can be arranged so as to go round the steel frame to directly inject the injection material up to the back side of the steel frame.
Since the framework for forming an injection hole is hollow, the quantity of the solvents used can be reduced and thus the method is economical even though the sufficient size is given to said framework so that the injection hole easy in injecting operation may be formed.
|
A method of sealing a concrete joint formed between a pair of concrete castings by creating an injection hole wherein a removable frame member can be attached to the bottom surface of the first concrete casting so as to form obtuse angles with the concrete casting surface. The other concrete casting is then cast around the frame member. The frame member is then removed to form the injection hole of the desired configuration, and sealing material can then be inserted into the injection hole for feeding into, and sealing of, the joint.
| 4
|
BACKGROUND
The present invention relates to thermal management devices, and more specifically, to methods and devices to provide cooling for electronic systems.
Electronic devices perform tasks which are becoming more complicated and computationally intensive with each passing year. In response to the requirements placed on these electronic devices, semiconductor die need to perform at ever-increasing levels of performance. In order to provide the increasing performance, successive generations of electronic devices include semiconductor die having smaller design rules which enable higher data speeds with the tradeoff of generating more heat in successively smaller spatial volumes. Further, as semiconductor die become smaller, packaging and interconnection circuitry coupling the semiconductor die to the larger electrical device becomes more densely packed. This dense interconnection circuitry may become a physical obstacle to remove heat from the semiconductor die and contributes to the heat generated by the electrical device. Heat is often removed from the electrical device as materials making up the electrical device may be altered by temperatures above a certain threshold and these temperatures may adversely change electrical characteristics of the materials. For example, power leakage through transistors on logic circuitry may occur as the temperature is increased and data integrity issues may occur when memory cells are exposed to temperatures outside their operating range. Also, removing heat may reduce extreme temperature fluctuations in the electrical device which can damage components through expansion and contraction when power is cycled on and off.
Conventional cooling approaches for semiconductor die include passive air convection, forced air conduction, and/or thermal sinks. However, these approaches are becoming less effective given the greater amounts of heat being generated in reduced spatial volumes. New cooling approaches for electronic devices are needed.
SUMMARY
According to one embodiment, a method is disclosed. The method includes conductively coupling a first semiconductor die to a substrate with at least one electrical contact element. The method also includes applying a hydrophobic coating directly to the semiconductor die, substrate, and electrical contact element. The hydrophobic coating is selected to transfer heat from the semiconductor die to a cooling fluid. In this manner, the semiconductor die may be efficiently cooled.
In another embodiment, a method is disclosed. The method includes applying power to at least one semiconductor die through at least one electrical contact element. The method also includes flowing a cooling fluid into contact with a hydrophobic coating attached to an exterior of the at least one semiconductor die and at least one electrical contact element. In this manner, local hot spots on the at least one semiconductor die may be prevented as efficient cooling is provided.
In another embodiment, a method is disclosed. The method includes applying power to a plurality of semiconductor die and the at least one electrical contact and the at least one electrical contact element through a second level interconnect of a substrate. The plurality of semiconductor die is in a stacked arrangement to form a 3D chip stack. The method also includes directing a cooling fluid through an inlet port of an enclosure and into a chamber, wherein the chamber is formed by the enclosure. The plurality of semiconductor die is disposed within the chamber, and the enclosure is attached to the substrate. The method also includes flowing the cooling fluid into contact with a hydrophobic coating attached to an exterior of the plurality of semiconductor die. The method also includes flowing the cooling fluid out of the chamber through an outlet port of the enclosure. The hydrophobic coating comprises at least one of: phased-separated spinodal glass powder, ceramic particles, diatomaceous earth, organosilanes, fluorinated organic compounds, silicones, siloxanes, and sol-gel materials including metal oxides. In this manner, temperature swings may be minimized when the 3D chip stack is cyclically turned on and off to reduce a probability of cracks forming in the 3D chip stack associated with cyclical expansion and contraction.
In another embodiment, an electrical assembly is disclosed. The electrical assembly comprises at least one semiconductor die. The electrical assembly also comprises a substrate configured to interface with an electrical source. The electrical assembly also comprises at least one electrical contact element conductively connecting the at least one semiconductor die to a substrate. The electrical assembly also comprises a hydrophobic coating attached to the at least one semiconductor die, substrate, and at least one electrical contact element. In this manner, the semiconductor die may be configured to be efficiently cooled by direct cooling.
In another embodiment, an electrical assembly is disclosed. The electrical assembly includes at least one semiconductor die generating heat. The electrical assembly also includes at least one substrate electrically coupled to an electrical source. The electrical assembly also includes at least one electrical contact element conductively connecting the substrate and the at least one semiconductor die. The electrical assembly also includes a hydrophobic coating disposed on the at least one semiconductor die, at least one substrate, and at least one electrical contact element. The hydrophobic coating includes an inner surface in direct thermal conductive communication with the semiconductor die and an outer surface configured for direct convective heat transfer to a cooling fluid. In this manner, hot spots on the at least one semiconductor die may be prevented as efficient cooling is provided.
In another embodiment, an electrical assembly is disclosed. The electrical assembly includes a substrate configured to interface with an electrical source. The electrical assembly also includes a plurality of semiconductor die. The plurality of semiconductor die including a first semiconductor die and a second semiconductor die. The substrate and the plurality of semiconductor die are in a stacked arrangement to form a 3D chip stack, and the first semiconductor die is disposed between the second semiconductor die and the substrate. The electrical assembly also includes at least one electrical contact element conductively connecting the first semiconductor die to the substrate and the second semiconductor die to at least one TSV (through silicon via) of the first semiconductor die. The electrical assembly also includes a hydrophobic coating attached to each of the plurality of semiconductor die, substrate, and electrical contact element. The electrical assembly also includes an enclosure secured to the substrate and forming a chamber containing the plurality of semiconductor die. The enclosure includes an inlet port and an outlet port configured for a cooling fluid to respectively enter and depart from the chamber. The hydrophobic coating includes an inner surface in direct conductive thermal communication with the semiconductor die and an outer surface arranged for direct convective thermal communication with the cooling fluid. In this manner, temperature swings may be minimized when the 3D chip stack may be cyclically turned on and off to reduce a probability of cracks forming in the electrical assembly associated with cyclical expansion and contraction.
Additional features and advantages will be set forth in the detailed description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the embodiments as described herein, including the detailed description which follows, the claims, as well as the appended drawings.
It is to be understood that both the foregoing general description and the following detailed description are merely exemplary, and are intended to provide an overview or framework to understanding the nature and character of the claims. The accompanying drawings are included to provide a further understanding, and are incorporated in and constitute a part of this specification. The drawings illustrate one or more embodiment(s), and together with the description serve to explain principles and operation of the various embodiments.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIGS. 1A and 1B are a partial cutaway front side view and a partial cutaway right side view, respectively, of an exemplary electrical device including at least one semiconductor die electrically connected to a substrate using electrical contact elements and cooled by a cooling fluid as directed by an enclosure, wherein a hydrophobic coating is applied to the at least one semiconductor die, at least one electrical contact element, and substrate;
FIG. 1C is a top perspective view of the electrical device of FIG. 1A being cooled by the cooling fluid which is in communication with an exemplary pump and an exemplary heat exchanger;
FIGS. 1D and 1E are a front side view and left side view of the electrical device of FIG. 1A including the enclosure;
FIG. 1F is a bottom view of the enclosure of the electrical device of FIG. 1D ;
FIG. 1G is an exploded top perspective view of the electrical device of FIG. 1D ;
FIG. 2 is a flow chart of an exemplary method for cooling the electrical assembly of the electrical device of FIG. 1A ;
FIG. 3 is a flow chart of an exemplary method for creating the electrical device of FIG. 1A ;
FIG. 4A is a top perspective view of an exemplary wafer being diced by a saw to create the at least one semiconductor die of FIG. 1A ;
FIG. 4B is a top perspective view of the at least one electrical contact element being conductively connected to a substrate;
FIG. 4C is a side view of a first semiconductor die being conductively connected to the substrate through the at least one electrical contact element;
FIG. 4D is a side view of a second semiconductor die being conductively connected to the substrate by TSVs (through silicon vias) of the first semiconductor die and the at least one electrical contact element;
FIG. 4E is a side view of a third semiconductor die being conductively connected to the substrate by TSVs (through silicon vias) of the first and second semiconductor dies and the at least one electrical contact element to create an electrical assembly of the electrical device of FIG. 1A ;
FIG. 4F is a top perspective view of the electrical assembly of FIG. 4E created by the conductive connecting of FIGS. 4B through 4E with a masking layer applied to the substrate;
FIG. 4G-1 is a top perspective view of the electrical assembly of FIG. 4F being immersed into a hydrophobic coating solution to apply the hydrophobic coating;
FIG. 4G-2 is a top perspective view of the electrical assembly of FIG. 4F with the hydrophobic coating solution being sprayed thereon with an exemplary spray nozzle as an alternative to FIG. 4G-1 ;
FIG. 4G-3 is a schematic view of the electrical assembly of FIG. 4F with a hydrophobic coating being applied by an evaporation deposition process as an alternative to FIG. 4G-1 ;
FIG. 4G-4 is a schematic view of the electrical assembly of FIG. 4F with a hydrophobic coating being applied by a chemical vapor deposition process as an alternative to FIG. 4G-1 ;
FIG. 4H is a top perspective view of the electrical assembly of FIG. 4F and the hydrophobic coating being rotated about an axis of rotation to create a more uniform thickness of the hydrophobic coating;
FIG. 4I is a top perspective view of the electrical assembly of FIG. 4F with the hydrophobic coating curing within an optional heating oven;
FIG. 4J is a top perspective view of an enclosure being attached to the substrate of the electrical assembly of FIG. 4I ;
FIG. 4K is a side view of the second layer interconnect being conductively attached to the second surface of the substrate of the electrical assembly of FIG. 4J ; and
FIGS. 5A through 5C are a top perspective view, front side view, and left side view, respectively, of another example of an exemplary electrical device comprising a semiconductor die conductively connected to a substrate with electrical contact elements and/or wire bonds, while being cooled by a cooling fluid, wherein the electrical device may have a hydrophobic coating applied which prevents direct contact between the cooling fluid and the substrate, single die, electrical contact elements, and wire bonds.
DETAILED DESCRIPTION
FIGS. 1A and 1B are a partial cutaway front side view and a partial cutaway right side view, respectively, of an exemplary electrical device 10 . The electrical device 10 may be optionally electrically connected to a circuit board 12 through a second layer interconnect 14 . The electrical device 10 may perform arithmetic, logic, and/or memory operations according to information exchanged through the second layer interconnect 14 . In the embodiment depicted in FIG. 1A , the second layer interconnect 14 is shown as a plurality of solder balls 16 in a ball grid array configuration, but in other embodiments the second layer interconnect 14 could include, for example, a plurality of pins in a pin grid array, a plurality of wire bonds connecting a substrate 22 to the circuit board 12 , and/or a plurality of pads in a land grid array (LGA) configuration. The electrical device 10 may also receive electrical power through the second layer interconnect 14 . In this manner, the electrical device 10 may receive power and exchange data.
The electrical device 10 includes an electrical assembly 18 which performs information processing for the electrical device 10 . The electrical assembly 18 comprises at least one semiconductor die 20 A- 20 C; a substrate 22 ; at least one electrical contact element 24 A- 24 C; and hydrophobic coating 26 . The semiconductor die 20 A- 20 C are electrically connected to the substrate 22 by the electrical contact elements 24 A- 24 C. Specifically, the second semiconductor die 20 B may be electrically connected by the electrical contact elements 24 A, 24 B and at least one TSV 25 A (“through silicon via”) to the substrate 22 . The third semiconductor die 20 C may be electrically connected by the electrical contact elements 24 A- 24 C and at least one TSV 25 A, 25 B to the substrate 22 . The substrate 22 receives electrical power from the circuit board 12 via the second layer interconnect 14 as discussed above. In this manner, the semiconductor die 20 A- 20 C receive electrical power to perform arithmetic, logic, and/or memory operations for the electrical device 10 . The semiconductor die 20 A- 20 C, the electrical contact elements 24 A- 24 C, and the substrate 22 contain conductive materials having electrical resistance and generate heat when carrying electrical current associated with the electrical power.
The heat generated by the electrical assembly 18 is transferred by thermal conduction to the hydrophobic coating 26 . The hydrophobic coating 26 includes an inner surface 28 A attached to exterior surfaces of the semiconductor die 20 A- 20 C, the electrical contact elements 24 A- 24 C, and the substrate 22 . The hydrophobic coating 26 may also include an outside surface 28 B configured to transfer the heat through convective heat transfer from the hydrophobic coating 26 to a cooling fluid 30 in an ambient environment 32 . In this manner, the heat may be efficiently removed from the electrical assembly 18 .
FIG. 1C is a top perspective view of heat being removed from the electrical device 10 of FIG. 1A by the cooling fluid 30 . The electrical device 10 may also include an enclosure 34 which directs the cooling fluid 30 to and from the electrical assembly 18 . The enclosure 34 may be secured to the substrate 22 and may form a chamber 36 to contain the at least one semiconductor die 20 A- 20 C and the electrical contact elements 24 A- 24 C. The cooling fluid 30 may enter the chamber 36 through at least one inlet port 38 A of the enclosure 34 and may exit the chamber 36 through at least one outlet port 38 B. The cooling fluid 30 may be in communication with an exemplary pump 40 to ensure a sufficient flow rate of the cooling fluid 30 through the chamber 36 to maintain the electrical assembly 18 within a temperature range. The cooling fluid 30 may also be in communication with an exemplary heat exchanger 42 . The heat exchanger 42 may remove at least a portion of the heat from the cooling fluid 30 to enable the cooling fluid 30 to return to the chamber 36 at a determined temperature to control the temperature of the electrical assembly 18 . The cooling fluid 30 may be directed from the outlet port 38 B to the pump 40 and the heat exchanger 42 , and then to return to the inlet port 38 A with a fluid conduit 44 , for example, plastic tubing. By changing the flow rate of the cooling fluid 30 with the pump 40 and/or the temperature of the cooling fluid 30 departing the heat exchanger 42 , the temperature of the electrical assembly 18 may be maintained below a threshold temperature. In this manner, the temperature-sensitive characteristics of the semiconductor die 20 A- 20 C may be controlled to enable predictable performance of the electrical assembly 18 .
FIGS. 1D and 1E are a front side view and left side view of the electrical device 10 of FIG. 1A depicting the enclosure 34 , secured to the substrate 22 . FIG. 1F is a bottom view of the enclosure 34 of the electrical device 10 of FIG. 1D depicting an interface surface 46 which may be complementary to a mounting surface 48 of the substrate 22 to form a tight seal to restrict entry into and exit from the chamber 36 , except through the inlet port 38 A and the outlet port 38 B. The tight seal may include bonding material, for example, epoxy to secure the enclosure 34 to the substrate 22 or mechanical sealing means. In this manner, the enclosure 34 may be secured to the substrate 22 .
Now that an introduction of the electrical device 10 has been provided, details of the associated components are provided in more detail in relation to FIG. 1G , which is an exploded top perspective view of the electrical device 10 . The electrical device 10 includes the second layer interconnect 14 , the substrate 22 , the electrical contact elements 24 A- 24 C, the at least one semiconductor die 20 A- 20 C, the hydrophobic coating 26 , and the enclosure 34 . These are now discussed in sequence.
The second layer interconnect 14 connects the electrical device 10 to the circuit board 12 . The second layer interconnect 14 may be, in one example depicted in FIG. 1G , a ball grid array (BGA) comprising a plurality of solder balls to attach the electrical device 10 to pads 50 on the circuit board 12 . In other examples the second layer interconnect 14 may be in a pin grid array (PGA) utilizing metal pins to be inserted into holes in a socket that may be soldered to the circuit board 12 . In another example, the second layer interconnect 14 may be pads instead of the solder balls in which the pads are abutted against spring contacts in a socket secured to the circuit board 12 . In another example, the second layer interconnect 14 may be wire bonds instead of solder balls in which wires bonded to pads on the substrate 22 , and the circuit board 12 . The second layer interconnect 14 is made of a strong conductive material which may comprise, for example, copper, tin, gold, and/or aluminum. In this manner, the electrical assembly 18 can be attached to the circuit board 12 .
It is noted that the second layer interconnect 14 may be free of the hydrophobic coating 26 , except in embodiments when the circuit board 12 is to be in contact with the cooling fluid 30 . In some embodiments where the circuit board 12 is to be in contact, then the hydrophobic coating 26 may also be applied to the second layer interconnect 14 .
With continued reference to FIG. 1G , the substrate 22 may serve as a structural foundation upon which the electrical device 10 is constructed and also may provide an electrical interface to a circuit board 12 through the second layer interconnect 14 . As a structural foundation, the substrate 22 may secure the at least one semiconductor die 20 A- 20 C to the circuit board 12 through the second layer interconnect 14 and the electrical contact elements 24 A- 24 C. The substrate 22 also provides an electrical interface between the second layer interconnect 14 and the electrical contact elements 24 A- 24 C which may be electrically connected to the at least one semiconductor die 20 A- 20 C. The substrate 22 may provide electrical pathways 54 separated and supported with dielectric material 56 to minimize crosstalk, electrical shorting, and power leakage. To provide the electrical pathways 54 , the substrate 22 may contain conductive material which may comprise, for example, copper, tin, gold, and/or aluminum. To provide the structural foundation and dielectric characteristics, the substrate 22 may also comprise, for example, thermoplastic, thermosets, ceramic, and/or composite material. In this manner, the substrate 22 may serve as a structural foundation and electrical interface.
It is noted that the substrate 22 may contact the cooling fluid 30 at the mounting surface 48 of the substrate 22 . In order to protect the electrical contact element 24 A from the cooling fluid 30 , the hydrophobic coating 26 may be applied to the mounting surface 48 , for example, in order to prevent electrical crosstalk, electrical shorts and power loss. In this manner, the hydrophobic coating 26 may form a uniform layer preventing the cooling fluid 30 from contacting the electrical contact elements 24 A. The hydrophobic coating 26 may also seal the mounting surface 48 to prevent the cooling fluid 30 from entering into surface irregularities in the substrate 22 , which may cause small surface cracks to propagate and cause leaks.
The electrical contact elements 24 A- 24 C conductively connect the at least one semiconductor die 20 A- 20 C to the substrate 22 . The electrical contact elements 24 A- 24 C may comprise, in one example depicted in FIG. 1G , solder balls 58 which may conductively connect to electrical contacts (not shown) and through silicon vias (TSVs) of the semiconductor dies 20 A- 20 C. In another example, The electrical contact elements 24 A- 24 C may comprise wire bonds, in which wires bonded to electrical contacts on semiconductor die 20 A- 20 C are bonded to other semiconductor die 20 A- 20 C and/or the substrate 22 . The electrical contact elements 24 A- 24 C may comprise a strong conductive material, for example, copper, gold, silver, tin, and/or aluminum. The outside surface of the electrical contact elements 24 A- 24 C may have the hydrophobic coating 26 applied to prevent contact with the cooling fluid 30 . The cooling fluid 30 may cause electrical shorting, cross talk or power loss if not prevented by the hydrophobic coating 26 from contacting the electrical contact elements 24 A- 24 C. In this manner, the electrical contact elements 24 A- 24 C may conductively connect the at least one semiconductor die 20 A- 20 C to the substrate 22 while being protected from contact with the cooling fluid 30 .
The semiconductor die 20 A- 20 C may perform the arithmetic, logic, and/or memory operations of the electrical device 10 . The semiconductor die 20 A- 20 C may comprise, for example, one or more of: a computer processor, an application-specific integrated circuit (ASICS), and/or a dynamic random access memory (DRAM). The at least one semiconductor die 20 A- 20 C may be manufactured, for example, using microlithography techniques on a silicon wafer. The semiconductor die 20 A- 20 C may be cut from one or more wafers and may comprise electrical components to perform arithmetic, logic, and/or memory operations. The semiconductor die 20 A, 20 B may respectively contain TSVs 25 A, 25 B to electrically connect the semiconductor die 20 A- 20 C in a 3D chip stack arrangement. In this manner, a footprint of the electrical device 10 on the printed circuit board 12 may be minimized and connection distances between the semiconductor die 20 A- 20 C minimized to increase processing speed.
Further, the hydrophobic coating 26 may be attached to the external surface of the at least one semiconductor die 20 A- 20 C. The hydrophobic coating 26 may prevent the cooling fluid 30 from contacting electrical connection locations between the electrical contact elements 24 A- 24 C and the at least one semiconductor die 20 A- 20 C. The hydrophobic coating 26 may also prevent the cooling fluid 30 from penetrating into the semiconductor die 20 A- 20 C where materials could be vulnerable to corrosion, electrical cross talk, power loss, and electrical shorting. In this manner, the at least one semiconductor die 20 A- 20 C may be protected from the cooling fluid 30 .
The enclosure 34 directs the cooling fluid 30 to and from the electrical assembly 18 . The enclosure 34 may be made from a strong material resistant to leakage of the cooling fluid 30 , may include a chemical composition inert to the cooling fluid 30 , and may include a melting point higher than operating temperatures of the electrical device 10 . In this regard, the enclosure 34 may comprise, for example, plastic and/or metal. The enclosure 34 may form the chamber 36 within which the at least one semiconductor dies 20 A- 20 C and the electrical contact elements 24 A- 24 C may be disposed. The enclosure 34 may include the at least one inlet port 38 A for the cooling fluid 30 to enter the chamber 36 and remove the heat from the electrical assembly 18 through convective heat transfer. The enclosure may also include the at least one outlet port 38 B for the cooling fluid 30 containing the heat from the electrical assembly 18 to depart from the chamber 36 . The enclosure 34 may be secured to the substrate 22 to prevent the cooling fluid 30 from entering and departing the chamber 36 without use of the inlet port 38 A and the outlet port 38 B. In this manner, the heat may be removed from the electrical assembly 18 .
It is noted that the cooling fluid 30 may be a liquid or a gas. Preferably the cooling fluid 30 is a liquid possessing a relatively low viscosity to efficiently move through the chamber 36 , high thermal conductivity, high specific heat, and thermal stability at operating temperatures. The hydrophobic coating 26 may prevent contact between the cooling fluid 30 and electrical components of the electrical assembly 18 to enable the cooling fluid 30 to be electrically conductive. The cooling fluid 30 may comprise, for example, water, ethylene glycol, propylene glycol, perfluorinated hydrocarbons (e.g., Fluorinert™), synthetic hydrocarbons (e.g., polyalphaolefins), suspended nanoparticles, glycol, and/or any combination thereof. In this manner, the cooling fluid 30 may enter through the inlet port 38 A, receive heat generated by the electrical assembly 18 , and then exit the chamber 36 with the heat through the outlet port 38 B.
With continued reference to FIG. 1G , and also reference back to FIG. 1A , the hydrophobic coating 26 may be attached to the at least one semiconductor die 20 A- 20 C, the electrical contact elements 24 A- 24 C, and the substrate 22 through a cohesive and/or adhesive bond. The hydrophobic coating 26 may comprise at least one of: phased-separated spinodal glass powder, ceramic particles, diatomaceous earth, organosilanes (RnSi(OR)4-n, wherein R is an alkyl, aryl, organofunctional group, fluorinated organic compound, and/or a methoxy, ethoxy, or acetoxy group), other fluorinated organic compounds, silicones, siloxanes, and sol-gel materials including metal oxides. The ceramic particles may, for example, include nanoparticles. The ceramic particles may also include at least one of, for example, aluminum oxide and zinc oxide. In some cases, the hydrophobic coating 26 may comprise at least one of: Nanomyte® coatings made by NEI Corporation of Somerset, N.J.; Ultra Ever Dry made by UltraTech International, Incorporated; Rust-Oleum® NeverWet® made by Rust-Oleum Corporation of Vernon Hills, Ill.; and HydroFoe™ superhydrophobic coating made by Lotus Leaf Coatings, Incorporated of Albuquerque, N. Mex. The hydrophobic coating 26 may include a wetting characteristic associated with an effective contact angle of at least ninety (90) degrees with a drop of water, and preferably more than one-hundred fifty (150) degrees. A thickness D 1 ( FIG. 1A ) of the hydrophobic coating 26 may be in a range from two (2) angstroms to seventy-five (75) microns to minimize an obstruction to the cooling fluid 30 traveling through the enclosure 34 . The hydrophobic coating 26 may prevent the cooling fluid 30 from contacting the at least one semiconductor die 20 A- 20 C, the electrical contact elements 24 A- 24 C, and the substrate 22 . Also, in some embodiments utilizing a solution-based coating application, the hydrophobic coating 26 also may be relatively inexpensive to apply as opposed to more expensive embodiments utilizing, for example, a vapor deposition process and/or an evaporative deposition process. In this manner, the hydrophobic coating 26 may be used as part of the electrical device 10 to enable efficient cooling of the semiconductor die 20 A- 20 C by the cooling fluid 30 while avoiding cross talk and electrical shorts related to contact of the cooling fluid 30 with the electrical contact elements 24 A- 24 C.
The hydrophobic coating 26 may provide several benefits. First, the hydrophobic coating 26 may form a physical barrier to prevent the cooling fluid 30 from contacting the at least one semiconductor die 20 A- 20 C, the electrical contact elements 24 A- 24 C, and the substrate 22 . Secondly, the hydrophobic coating 26 may increase the efficiency of heat transfer, for example, by conducting heat from the inner surface 28 A to the outer surface 28 B, to the cooling fluid 30 . Thirdly, the hydrophobic coating 26 may be applied using various methods including a relatively low-cost, solution-based application instead of more expensive vapor deposition processes. In this manner, the hydrophobic coating 26 may provide efficient cooling to the semiconductor die 20 A- 20 C.
Now that the components and embodiments of the electrical device 10 have been discussed, FIG. 2 depicts a flow chart of an exemplary method 60 for cooling the electrical assembly 18 of the electrical device 10 of FIG. 1C . The method 60 includes the operations 62 A and 62 B which are discussed below using the terminology discussed above.
In this regard, the method 60 may include applying power to the at least one semiconductor die 20 A- 20 C through the electrical contact elements 24 A- 24 C and the TSVs 25 A, 25 B (operation 62 A of FIG. 2 ). The method 60 may also include flowing the cooling fluid 30 into contact with the hydrophobic coating 26 attached to an exterior of the at least one semiconductor die 20 A- 20 C and the electrical contact elements 24 A- 24 C (operation 62 B of FIG. 2 ). In this manner, efficient cooling may be provided to the at least one semiconductor die 20 A- 20 C.
Next, FIG. 3 depicts a flow chart of an exemplary method 64 for creating the electrical device 10 of FIG. 1A . The method 64 , including the operations 66 A through 66 E, is discussed in detail with respect to FIGS. 4A through 4K below using the terminology discussed above.
In this regard, FIG. 4A is a top perspective view of an exemplary wafer 68 being diced by a saw 70 to form the at least one semiconductor die 20 A- 20 C of FIG. 1A (operation 66 A of FIG. 3 ). The wafer 68 may be provided with the electrical interconnection features of the at least one semiconductor die 20 A- 20 C, for example, by utilization of one or more microlithography processes. The saw 70 may be used to cut the wafer 68 into the semiconductor die 20 A- 20 C which may be used as a part of the electrical device 10 . It is noted that the semiconductor die 20 A- 20 C may originate from different ones of the wafers 68 and may have different electrical features to perform different arithmetic, logic, and/or memory operations.
The method 64 may also include conductively coupling the at least one semiconductor die 20 A- 20 C to each other and to the substrate 22 using the electrical contact elements 24 A- 24 C (operation 66 B in FIG. 3 ). In this regard, the electrical contact elements 24 A- 24 C may comprise solder balls 58 . FIG. 4B is a top perspective view of the electrical contact elements 24 A- 24 C being conductively connected to the substrate 22 . As shown in FIG. 4B the solder balls 58 may be precisely placed upon the substrate 22 using a ball placement system 72 . In one example, the ball placement system 72 may comprise a Koses KAM 750 solder ball attach machine manufactured by Korea Semiconductor System, Company, Limited of Bucheon City, Kyunggi-Do, Korea.
Once the solder balls 58 are attached to precise contact locations of the substrate 22 , then the first semiconductor die 20 A may be conductively connected to the substrate 22 through the at least one solder balls 58 of the at least one electrical contact elements 24 A as shown in FIG. 4C using, for example, a robotic tool (not shown). The electrical contact elements 24 C enable an interstitial space 74 A to be disposed between the semiconductor dies 20 B, 20 C which may be later used for the cooling fluid 30 to flow and efficiently provide cooling to the semiconductor die 20 B, 20 C. It is noted that the solder balls 58 are connected to the at least one TSV 25 A of the first semiconductor die 20 A, so that at least a second semiconductor die 20 B may be conductively connected to the substrate 22 .
FIGS. 4D and 4E are side views of the second and third semiconductor dies 20 B, 20 C being conductively connected to the first semiconductor die 20 A and the substrate 22 using the electrical contact elements 24 A- 24 C and the TSVs 25 A, 25 C. This conductive coupling forms interstitial spaces 74 B, 74 C using similar manufacturing approaches discussed in relation to FIGS. 4B and 4C . The interstitial spaces 74 A- 74 C may have a width D 2 (see FIG. 1A ) in a range from one (1) micron to three (3) millimeters. In this manner, the electrical assembly 18 may be created.
As shown in FIG. 4F , a mask layer 75 may be applied to the second surface 85 of the substrate 22 in preparation for the hydrophobic coating 26 to be applied. The mask layer 75 may prevent, for example, the hydrophobic coating 26 from being attached to exterior areas of the substrate 22 where further electrical connections may be established. The mask layer 75 may be a conventional photoresist that may be removed in later stages of the method 64 . Using photoresist enables specific areas of the mask to be exposed to a microlithography stepper (not shown) or pattern generator (not shown) to protect specific areas of the substrate 22 . In the embodiment shown in FIG. 4F , the second surface 85 is fully masked to prevent later attachment with the hydrophobic coating 26 . In this manner, the electrical assembly 18 may be readied for application of the hydrophobic coating 26 .
The method 64 also includes applying the hydrophobic coating 26 to the at least one semiconductor die 20 A- 20 C; the at least one electrical contact element 24 A- 24 C; and the substrate 22 (operation 66 C of FIG. 3 ). In this regard, and in one exemplary approach, FIG. 4G-1 is a top perspective view of the electrical assembly 18 of FIG. 4F being immersed into a hydrophobic coating solution 76 which contains the hydrophobic coating 26 . The electrical assembly 18 may be then spun about an axis of rotation Ai (see FIG. 4H ) to even out the hydrophobic coating solution 76 to a more uniform thickness. In another approach, as depicted in FIG. 4G-2 , the hydrophobic coating solution 76 may be sprayed on to the electrical assembly 18 using at least one spray nozzle 78 . The electrical assembly 18 may also be then spun relative to an axis of rotation Ai (see FIG. 4H ) to also even out the hydrophobic coating solution 76 to a more uniform thickness.
The hydrophobic coating solution 76 may be cured to form the hydrophobic coating 26 . As shown in FIG. 4I the hydrophobic coating solution 76 may be cured by vaporizing solvents 80 within the hydrophobic coating solution 76 to leave a hydrophobic coating 26 applied to the semiconductor die 20 A- 20 C; the electrical contact elements 24 A- 24 C, and the substrate 22 . An optional heating oven 82 (shown in broken lines in FIG. 4I ) may be used to accelerate the curing process. Alternatively, in some cases, curing may be accomplished at room temperature without the heating oven 82 . In this manner, a hydrophobic coating 26 may be applied.
In another approach for applying the hydrophobic coating 26 , FIG. 4G-3 shows a schematic view of the electrical assembly 18 of FIG. 4F with the hydrophobic coating 26 being applied by an evaporation deposition device 100 . The evaporation deposition device 100 includes a low-pressure chamber 102 comprising a heater 104 , crucible 106 , vacuum pump 108 , fixture 110 , electron source 112 , and hydrophobic coating material 114 . The electronic assembly 18 may be placed in the low-pressure chamber 102 which may be pulled to near vacuum with the vacuum pump 108 . The electronic assembly 18 may be supported by the fixture 110 which may be moveable with an actuator 116 . The electron source 112 may form an electron beam 118 which is received by the hydrophobic coating material 114 within the crucible 106 . The hydrophobic coating material 114 may be evaporated and received by the electrical assembly 18 to form the hydrophobic coating 26 . The heater 104 may facilitate a more uniform thickness of the hydrophobic coating material 114 by providing a more uniform temperature of the electrical assembly 18 . In this manner, the hydrophobic coating 26 may be formed having a sub-nanometer thickness.
In another approach for applying the hydrophobic coating 26 , FIG. 4G-4 shows a schematic view of the electrical assembly 18 of FIG. 4F with the hydrophobic coating 26 being applied by a chemical vapor deposition device 120 . The chemical vapor deposition device 120 includes at least one resistance heater 122 A- 122 C, a chamber 122 , a fixture 124 , and volatile precursors 126 . The one or more electrical subassemblies 18 may be supported in the chamber 122 by the fixture 124 as they are exposed to the volatile precursors 126 comprising the hydrophobic coating material 114 . The volatile precursors 126 enter the chamber 122 and react and/or decompose on the electrical assembly 18 to produce the hydrophobic coating 26 . The resistance heaters 122 A- 122 C may be proximate to the electrical assemblies 18 to initiate the reaction and/or decomposition of the volatile precursors 126 and facilitate a uniform distribution of the hydrophobic coating material 114 at the electrical assemblies 18 . In this manner, the hydrophobic coating 26 may also be formed having a sub-nanometer thickness.
The method 64 may also include attaching the enclosure 34 to the substrate 22 (operation 66 D of FIG. 3 ). Attachment as depicted in FIG. 4J may be made using, for example, an adhesive (for example, epoxy) or cohesive substance, mechanical interface means, or thermal bonding. The attachment of the enclosure 34 to the mounting surface 48 of the substrate 22 may prevent the cooling fluid 30 from entering or exiting the chamber 36 of the enclosure 34 , except through the inlet port 38 A and/or outlet port 38 B. The third semiconductor die 20 C may be spaced from the enclosure 34 by a distance D 3 ( FIG. 1A ) which may be the same or substantially the same as the thickness D 1 of the interstitial spaces 74 A- 74 C to facilitate flow of the cooling fluid 30 through the interstitial spaces 74 A- 74 C ( FIG. 4E ). In this manner, the cooling fluid 30 may be precisely directed to the electrical assembly 18 for cooling the semiconductor dies 20 A- 20 C.
The method 64 may also include attaching the second layer interconnect 14 to the substrate 22 (operation 66 E of FIG. 3 ). In this regard, the mask layer 75 may first be removed from the second surface 85 of the substrate 22 . Removal, for example, may include a conventional processing solution to remove the mask layer 75 from the second surface 85 . Once the mask layer 75 is removed, the second layer interconnect 14 may be attached. FIG. 4K is a side view of the second layer interconnect 14 being conductively attached to the second surface 85 of the substrate 22 of the electrical assembly 18 . The second layer interconnect 14 may comprise the solder balls 16 . The solder balls 16 may be precisely placed upon the second surface 85 of the substrate 22 using the ball placement system 72 discussed above. In this manner, the electrical device 10 may be created.
Although the electrical device 10 has been discussed above, other embodiments are possible. In this regard, FIGS. 5A through 5C are a top perspective view, front side view, and left side view, respectively, of another example of an exemplary electrical device 10 ′ comprising a single semiconductor die 20 ′ conductively connected to a substrate 22 ′ with electrical contact elements 24 ′, and wire bonds 88 . The single semiconductor die 20 ′ may be cooled by the cooling fluid 30 which flows past. The single semiconductor die 20 ′, the electrical contact elements 24 ′ and the wire bonds 88 may have a hydrophobic coating 26 ′ applied which prevents direct contact between the cooling fluid 30 and the substrate 22 ′, the single semiconductor die 20 ′, the electrical contact elements 24 ′, and the wire bonds 88 . The hydrophobic coating 26 ′ may have similar dimensions, chemical makeup, and manufacturing application processes as discussed above for electrical device 10 . In this manner, the single semiconductor die 20 ′ may be efficiently cooled.
The descriptions of the various embodiments of the present invention have been presented for purposes of illustration, but are not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein was chosen to best explain the principles of the embodiments, the practical application or technical improvement over technologies found in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
In the following, reference is made to embodiments presented in this disclosure. However, the scope of the present disclosure is not limited to specific described embodiments. Instead, any combination of the following features and elements, whether related to different embodiments or not, is contemplated to implement and practice contemplated embodiments. Furthermore, although embodiments disclosed herein may achieve advantages over other possible solutions or over the prior art, whether or not a particular advantage is achieved by a given embodiment is not limiting of the scope of the present disclosure. Thus, the following aspects, features, embodiments and advantages are merely illustrative and are not considered elements or limitations of the appended claims except where explicitly recited in a claim(s). Likewise, reference to “the invention” shall not be construed as a generalization of any inventive subject matter disclosed herein and shall not be considered to be an element or limitation of the appended claims except where explicitly recited in a claim(s).
Aspects of the present invention may take the form of an entirely hardware embodiment, an entirely software embodiment (including firmware, resident software, microcode, etc.) or an embodiment combining software and hardware aspects that may all generally be referred to herein as a “circuit,” “module” or “system.”
The present invention may be a system, a method, and/or a computer program product. The computer program product may include a computer readable storage medium (or media) having computer readable program instructions thereon for causing a processor to carry out aspects of the present invention.
The computer readable storage medium can be a tangible device that can retain and store instructions for use by an instruction execution device. The computer readable storage medium may be, for example, but is not limited to, an electronic storage device, a magnetic storage device, an optical storage device, an electromagnetic storage device, a semiconductor storage device, or any suitable combination of the foregoing. A non-exhaustive list of more specific examples of the computer readable storage medium includes the following: a portable computer diskette, a hard disk, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or Flash memory), a static random access memory (SRAM), a portable compact disc read-only memory (CD-ROM), a digital versatile disk (DVD), a memory stick, a floppy disk, a mechanically encoded device such as punch-cards or raised structures in a groove having instructions recorded thereon, and any suitable combination of the foregoing. A computer readable storage medium, as used herein, is not to be construed as being transitory signals per se, such as radio waves or other freely propagating electromagnetic waves, electromagnetic waves propagating through a waveguide or other transmission media (e.g., light pulses passing through a fiber-optic cable), or electrical signals transmitted through a wire.
Computer readable program instructions described herein can be downloaded to respective computing/processing devices from a computer readable storage medium or to an external computer or external storage device via a network, for example, the Internet, a local area network, a wide area network and/or a wireless network. The network may comprise copper transmission cables, optical transmission fibers, wireless transmission, routers, firewalls, switches, gateway computers and/or edge servers. A network adapter card or network interface in each computing/processing device receives computer readable program instructions from the network and forwards the computer readable program instructions for storage in a computer readable storage medium within the respective computing/processing device.
Computer readable program instructions for carrying out operations of the present invention may be assembler instructions, instruction-set-architecture (ISA) instructions, machine instructions, machine dependent instructions, microcode, firmware instructions, state-setting data, or either source code or object code written in any combination of one or more programming languages, including an object oriented programming language such as Smalltalk, C++ or the like, and conventional procedural programming languages, such as the “C” programming language or similar programming languages. The computer readable program instructions may execute entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the latter scenario, the remote computer may be connected to the user's computer through any type of network, including a local area network (LAN) or a wide area network (WAN), or the connection may be made to an external computer (for example, through the Internet using an Internet Service Provider). In some embodiments, electronic circuitry including, for example, programmable logic circuitry, field-programmable gate arrays (FPGA), or programmable logic arrays (PLA) may execute the computer readable program instructions by utilizing state information of the computer readable program instructions to personalize the electronic circuitry, in order to perform aspects of the present invention.
Aspects of the present invention are described herein with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the invention. It will be understood that each block of the flowchart illustrations and/or block diagrams, and combinations of blocks in the flowchart illustrations and/or block diagrams, can be implemented by computer readable program instructions.
These computer readable program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the flowchart and/or block diagram block or blocks. These computer readable program instructions may also be stored in a computer readable storage medium that can direct a computer, a programmable data processing apparatus, and/or other devices to function in a particular manner, such that the computer readable storage medium having instructions stored therein comprises an article of manufacture including instructions which implement aspects of the function/act specified in the flowchart and/or block diagram block or blocks.
The computer readable program instructions may also be loaded onto a computer, other programmable data processing apparatus, or other device to cause a series of operational steps to be performed on the computer, other programmable apparatus or other device to produce a computer implemented process, such that the instructions which execute on the computer, other programmable apparatus, or other device implement the functions/acts specified in the flowchart and/or block diagram block or blocks.
The flowchart and block diagrams in the Figures illustrate the architecture, functionality, and operation of possible implementations of systems, methods, and computer program products according to various embodiments of the present invention. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of instructions, which comprises one or more executable instructions for implementing the specified logical function(s). In some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems that perform the specified functions or acts or carry out combinations of special purpose hardware and computer instructions.
|
Devices employing semiconductor die having hydrophobic coatings, and related cooling methods are disclosed. A device may include at least one semiconductor die electrically coupled to a substrate by electrical contact elements. During operation the semiconductor die and the electrical contact elements generate heat. By applying hydrophobic coatings to the semiconductor die and the electrical contact elements, a cooling fluid may be used to directly cool the semiconductor die and the electrical contact elements to maintain these components within temperature limits and free from electrical shorting and corrosion. In this manner, the semiconductor die and associated electrical contact elements may be cooled to avoid the creation of damaging localized hot spots and temperature-sensitive semiconductor performance issues.
| 7
|
FIELD OF INVENTION
The present invention relates to an apparatus for aligning drilling machines.
BACKGROUND OF INVENTION
The alignment of the initial position of a drill collar and therefore the initial direction of the drill hole being created is highly important, especially in areas such as mining where the accuracy of drill holes is crucial in ensuring that the correct blasting patterns or that cable bolts etc used to secure the rock face is correctly positioned. A number of differing methods have been used to limited success to ensure that the relative direction (azimuth) and angle (pitch) of a drill hole are correct.
Inaccuracies in azimuth measurements have a huge affect on the accuracy of the drill hole, with an error of 1 degree in azimuth over a 1000 meter drill hole causing and error of 12.3 meters.
Some methods of aligning the drilling collar rely on the use of a compass to measure magnetic north. Azimuth direction is determined as a bearing relative to magnetic north. Compass based techniques are also affected greatly by the type of ore body that is being worked on as well as the closeness of vehicles with steel frames etc.
Other examples of alignment methods have involved the use of surveyors to determine the relative direction (azimuth) and angle (pitch) that a drilling collar rod should contact the rock face to ensure that the hole is drilled in the correct manner. In underground mining operations especially this can be a laborious task as the limited space and distance requires a significant number of calculations to be performed to ensure that the correct azimuth and pitch are set for the drill rig prior to drilling. This requires that the surveyor take measurement after measurement until the crew operating the drill rig have manoeuvred the drill rig into position.
Other alignment methods rely on the use of GPS survey instruments, however, the nature of these instruments mean that they must have ‘vision’ of the global position system satellites and as such are not usable in heavily wooded areas or underground.
It has also been shown that the drill rig itself may block the ‘vision’ of the GPS survey instruments and therefore reduce the accuracy of the measurements produced. One of the many problems faced by GPS systems is they may take up to 10 minutes to determine the azimuth depending upon the number of satellites that are visible. If there are no available satellites no azimuth may be calculated.
Another known problem of GPS survey instruments is that may not be moved once a bearing has been calculated. Therefore it is often necessary for the satellite detection process to be conducted a number of times to ensure correct azimuth alignment before drilling can commence.
SUMMARY OF THE INVENTION
The present invention attempts to overcome at least in part the aforementioned disadvantages of previous drilling machine alignment apparatus.
In accordance with one aspect of the present invention there is provided an aligning apparatus for aligning the drilling collar of a drilling rig or machine both for relative direction (azimuth) and angle (pitch).
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a perspective view of the aligning device attached to a drill collar with a drill rod inserted in accordance with the present invention.
FIG. 2 is a side elevation view of a vehicle with a drill collar attached thereto and with the aligning device and display mounted to the vehicle rather than to the drill collar.
DESCRIPTION OF THE INVENTION
Referring to the Figures, there is shown apparatus and a method for determining the alignment of a drill collar.
FIG. 1 , shows an aligning apparatus 10 in accordance with the present invention. The aligning apparatus 10 comprises a casing 12 attached to which is a mounting means 14 . Arranged with in the casing 12 is at least one mutually orthogonal fibre optic gyroscope (FOG). The aligning apparatus 10 preferably further comprises at least one set of mutually orthogonal accelerometers. The aligning apparatus 10 may further comprise other electronic measuring devices such as to determine relative magnetic field strength and control electronics with the ability to perform pulse modulation on the laser used within the FOG.
Alternatively, the sensing means may comprise a plurality of true north seeking micro electrical mechanical system (MEMS) devices. The plurality of MEMS devices being chosen for their ability to determine true north, the relative rotation of the earth about its axis. Preferably, the plurality of MEMS devices are arranged to be mutually orthogonal to each other.
Further, the sensing means may comprise other known rotational sensing means capable of determining true north or the relative rotation of the earth about its axis such as gimbal based gyroscopes of strap-down gyroscopes.
The Aligning apparatus 10 preferably further comprises at least one set of mutually orthogonal accelerometers. The aligning apparatus 10 may further comprise other electronic measuring devices, such devices being able to determine relative magnetic field strength or environmental condition data relating to the operating environment of the aligning apparatus.
The aligning device 10 preferably also comprises control electronics with the ability to perform pulse modulation on the laser used within the FOG or equipment for reducing or at least ameliorating signal noise, error or drift in the readings taken from the MEMS sensors.
In accordance with one preferred embodiment of the present invention the mounting means 14 is arranged to allow the aligning apparatus 10 to be mounted directly to a drilling collar rod as shown in FIG. 1 , such that one of the axes of the aligning apparatus 10 is parallel to the drilling rod.
In accordance with yet another preferred embodiment of the present invention, the aligning apparatus 10 may further comprise a connection to a display device 18 which is remote to the aligning apparatus 10 , with relevant information being displayed on a screen 16 . The screen 16 may be configured to display information such as alignment (azimuth) and angle (pitch) of the aligning apparatus 10 . The display device 18 may be a handheld device or may be incorporated or integrated into the dash board of a vehicle 20 ( FIG. 2 ) to which the drilling equipment is mounted.
In accordance with a preferred embodiment the screen display 16 is arranged such that the driver of the vehicle may see the display device 18 so that the displayed information may be used to guide or position the vehicle.
In accordance with yet another preferred embodiment of the present invention the connection between the alignment apparatus 10 and the display device 18 may be in the form of wireless communication such as a Wi-Fi or short range wireless radio wave data transmission system, such as that provided under the certification trademark BLUETOOTH administered by Bluetooth SIG, Inc. of Washington, D.C., USA.
In accordance with a further preferred embodiment of the present invention there is provided a method of determining the alignment of a drilling collar rod. The method begins with the alignment apparatus 10 of the present invention being powered on, provided with the latitude it is to operate at and allowed to stay in a stationary position to complete its calibration and power-on self-test (POST) sequence. Using the provided latitude, and once the alignment apparatus 10 has completed its calibration and POST sequence the alignment apparatus 10 is able to detect the relative rotation of the earth and therefore the direction of true north relative to the alignment apparatus 10 .
Once the alignment apparatus 10 has completed it calibration and POST sequence it will display on the display device 18 the relative bearing that the alignment apparatus is currently on. The operator of the system will then be able to position in the alignment apparatus 10 so that the mounting means 14 engage the drilling collar rod. The FOG and accelerometers of the alignment apparatus 10 captures the movement of the alignment apparatus 10 so that relative bearing of the alignment apparatus 10 to true north is constantly calculated.
In this manner it is then possible to align the drilling collar rod to the required alignment and angle whilst the alignment apparatus 10 is still attached to the drilling collar rod with the relative alignment and angle being constantly calculated.
In use, the apparatus of the present invention is arranged to determine the alignment and angle of a drill collar. This process begins with the aligning apparatus 10 being powered on and being held stationary for a period of time. The aligning apparatus 10 once calibrated determines the direction of true north relative to the aligning apparatus 10 .
Once true north is determined the aligning apparatus 10 is brought into close contact with the drilling collar rod, the aligning apparatus 10 is attached to the drilling collar rod by mounting means 14 . The aligning apparatus 10 unlike many other true north seeking devices (such as the GPS survey instruments discussed above) is able to be moved once true north is detected, with any movement of the apparatus being captured by the FOG and the accelerometers of the aligning apparatus 10 and displayed the display device 18 appropriately.
With the aligning apparatus 10 attached to the drilling collar rod, the drill collar may be moved to the correct azimuth and angle alignment designated for that particular drill hole. As discussed above movement of the aligning apparatus 10 and the drill rod is possible with the advancements made by the combination of the FOG and the accelerometers wherein relative movement recorded by the alignment apparatus 10 is used to calculate relative changes in alignment and position of the aligning apparatus 10 .
Using the information displayed on the screen 16 of the display device 18 , the drilling collar rod alignment is able to be manipulated to ensure that the drilling collar rod is aligned correctly prior to drilling.
In accordance with another preferred embodiment of the present invention the aligning apparatus 10 may be affixed directly to the vehicle to which the drilling equipment is mounted. The aligning apparatus 10 is mounted in a fixed position on the vehicle and all alignment measurements taken are relative to the angle that the equipment is relative to the aligning apparatus 10 . This will require additional sensor to be attached to the vehicle to determine the relative direction, incline and roll of the drilling equipment. In this manner the aligning apparatus 10 may be placed in a position where it will not be damaged during the normal operation of the drilling equipment.
The Applicant has found that it is possible to increase the accuracy of drilling collar placement to within 0.2 degree in both azimuth and pitch. This increase in accuracy allows further improvement in the overall accuracy of drilling operations, as accuracy errors compound during the drilling process. Further, known directional drilling techniques require an accurate assessment of the drilling collar to determine overall direction and accuracy.
The method of the present invention therefore allows the alignment and angle of the drilling collar rod to be determined at a greatly increased speed then any of the previously discussed methods of alignment. Further, the alignment of the drilling collar rod is of a much greater accuracy then other previously described methods.
Modifications and variations as would be apparent to a skilled addressee are deemed to be within the scope of the present invention.
|
An alignment apparatus for aligning drilling machines, the alignment apparatus comprising a casing and mounting means. The mounting means allowing, in use, for a true north seeking sensing means to be aligned with the drilling machinery to be aligned. The alignment apparatus being capable of displaying azimuth and pitch information to a user, so that the drilling machinery can be aligned as required.
| 4
|
CROSS-REFERENCE TO RELATED APPLICATION
This application is the U.S. national stage application of International Patent Application No. PCT/US2009/003595, filed Jun. 16, 2009, which claims the benefit of U.S. Provisional Patent Application No. 61/132,225, filed Jun. 17. 2008, the disclosures of which are hereby incorporated by reference in their entirety, including all figures, tables and amino acid or nucleic acid sequences.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
The United States Federal Government may have rights under this application.
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
Not applicable.
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
None
The Sequence Listing for this application is labeled “Seq-List.txt” which was created on Nov. 23,2010 and is 15 KB. The entire contents of the sequence listing is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to processes that copy oligonucleotides in a polymerase chain reaction (PCR) where these oligonucleotides incorporate nucleotide analogs (“non-standard nucleotides”) that form base pairs joined by hydrogen bonding patterns not found in standard nucleotides A, T, G and C. The invention relates more specifically to processes that amplify oligonucleotides holding more than one non-standard nucleotides, including non-standard nucleotides at adjacent positions in the oligonucleotides chain, and amplification in a nested PCR format.
2. Description of Related Art
Natural oligonucleotides bind to complementary oligonucleotides according to well-known rules of nucleobase pairing first elaborated by Watson and Crick, where adenine (A) pairs with thymine (T) (or uracil, U, in RNA), and guanine (G) pairs with cytosine (C), with anti-parallel complementary strands. In this disclosure, “DNA”, “oligonucleotide”, or “nucleic acid” is understood to include DNA and RNA, as well as derivatives where the sugar is modified, as in 2′-O-methyl and 2′,3′-dideoxynucleoside derivatives, where the nucleobase has an appendage, and these nucleic acids and their analogs in non-linear topologies, including as dendrimers, comb-structures, and nanostructures, and analogs carrying appendages or tags (e.g., fluorescent, functionalized, or binding, such as biotin). Further, “polymerase” in this application is meant to include DNA polymerases of all families, RNA polymerases, and reverse transcriptases.
These pairing rules allow specific hybridization of oligonucleotides to complementary oligonucleotides, making oligonucleotides valuable as probes in the laboratory, in diagnostics, as messages that direct the synthesis of proteins, and in other applications known in the art. Such pairing is used, for example and without limitation, to capture oligonucleotides to beads, arrays, and other solid supports, allow nucleic acids to fold in hairpins, beacons, and catalysts, support function, such as fluorescence, quenching, binding/capture, and catalysis, and as part of complex structures, including dendrimers and nanostructures, and scaffolds to guide chemical reactions.
Further, base pairing underlies the enzymatic synthesis of oligonucleotides complementary to a template. Here, assembly of building blocks from nucleoside triphosphates is directed by a template to form a complementary oligonucleotide with a complementary sequence. This is the basis for replication in living systems, and underlies technologies for enzymatic synthesis and amplification of specific nucleic acids by enzymes such as DNA and RNA polymerase, the polymerase chain reaction (PCR), and assays involving synthesis, ligation, cleavage, immobilization and release, inter alia.
Watson-Crick pairing rules can be understood as the product of two rules of complementarity: (1) size complementarity (a big purine pairs with a small pyrimidine) and (2) hydrogen bonding complementarity (hydrogen bond donors pair with hydrogen bond acceptors). However, as noted by U.S. Pat. Nos. 5,432,272, 5,965,364, 6,001,983, 6,037,120, 6,140,496, 6,627,456, and 6,617,106, Watson-Crick geometry can accommodate as many as 12 nucleobases forming 6 mutually exclusive pairs. Of these, four nucleobases forming two pairs are designated “standard”, while eight nucleobases forming four pairs were termed “non-standard”, and may be part of an “artificially expanded genetic information system” (AEGIS).
To systematize the nomenclature for the hydrogen bonding patterns, the hydrogen bonding pattern implemented on a small component of a nucleobase pair are designated by the prefix “py”. Following this prefix is the order, from the major to the minor groove, of hydrogen bond acceptor (A) and donor (D) groups. Thus, both thymine and uracil implement the standard hydrogen bonding pattern pyADA. The standard nucleobase cytosine implements the standard hydrogen bonding pattern pyDAA. Hydrogen bonding patterns implemented on the large component of the nucleobase pair are designated by the prefix “pu”. Following the prefix, hydrogen bond donor and acceptor groups are designated, from major to minor groove, by “A” and “D”. Thus, the standard nucleobases adenine and guanine implement the standard hydrogen bonding patterns puDA- and puADD respectively.
A central teaching of this disclosure is that hydrogen-bonding patterns are distinct from the organic molecule that implemented them. Thus, guanosine implements the puADD hydrogen-bonding pattern. So does, however, 7-deazaguanosine, 3,7-dideazaguanosine, and many other purines and purine analogs, including those that carry side chains carrying functional groups, such as biotin, fluorescent, and quencher groups. Which organic molecule is chosen to implement a specific hydrogen-bonding pattern determines, in part, the utility of the non-standard hydrogen-bonding pattern, in various applications to which it might be applied.
Claims of U.S. Pat. No. 5,432,272 and its successors covered non-standard bases that implemented the pyDDA hydrogen bonding pattern. Subsequent efforts to use these, however, encountered problems, including epimerization [Voe96a,b], oxidation [Von95], and uncharacterized decomposition. Accordingly, Benner invented a new non-standard nucleoside, 6-amino-5-nitro-3-(1′-beta-D-2′-deoxyribofuranosyl)-2-(1H)-pyridone (dZ) to implement the pyDDA hydrogen bonding pattern. The nitro group rendered the otherwise electron-rich heterocycle stable against both oxidation and epimerization under standard conditions. When paired with a corresponding puAAD nucleotide, duplexes were formed with stabilities that, in many cases, were higher than those observed in comparable strands incorporating the dG:dC nucleobase pair [Yan06]. This invention is covered by U.S. patent application Ser. No. 11/372,400, which is incorporated herein by reference. Contents of this patent application have been published [Hut03].
While Z supports binding of oligonucleotides containing it to complementary strands that match a nucleobase implementing the puAAD hydrogen bond pattern, it was not clear that polymerases would accept this unnatural base pair. Polymerases are known to be idiosyncratic [Hor95], meaning that experimentation is necessary to ascertain whether a specific implementation of a non-standard hydrogen bonding scheme can be accepted by a polymerase.
Thus, it was necessary to show by experiment that polymerases could incorporate dZ and dP. This was done for oligonucleotides containing a single dZ or dP [Yan07], which was published less than a year before the priority date of the instant application. However, [Yan07] showed that the dZ and dP are lost in multiple PCR cycles with Taq and Deep Vent (exo−) polymerases, perhaps via a mechanism where deprotonated dZ mispairs with dG (or deprotonated dG pairs with dZ), while protonated dC mispairs with dP (or protonated dP pairs with dC). Thus, this art teaches away from any use of the non-standard dZ:dP nucleobase pair in higher level PCR, defined as PCR that creates amplicons with multiple non-standard nucleotides.
BRIEF SUMMARY OF THE INVENTION
This invention concerns processes that amplify oligonucleotides containing non-standard nucleotides ( FIG. 1 ) in PCR where those oligonucleotides are not restricted in sequence to containing only a single nonstandard nucleotide, and where those oligonucleotides are not restricted in sequence to those where no adjacent nonstandard nucleotides appear, and amplification is done in a nested PCR format [Bro97].
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 . A set of heterocycles implementing a set of hydrogen bonding patterns. The heterocycles used in the processes of the instant invention are labeled dZ and dP.
FIG. 2 . Schematic showing nested PCR, where nucleotides from an artificially expanded genetic information system (AEGIS) are included in the tags (vertically hashed lines) attached to chimeric PCR primers. Chimeric primers initiating the PCR may be at low concentrations, diminishing the possibility of off-target priming. After their consumption in early PCR cycles, PCR continues via priming with external primers.
FIG. 3 . Autoradiograph of an electrophoresis gel showing PCR products as described in Example 1. _Left: PCR using primers only standard nucleotides in both the amplicon binding region and in the 5′-tag. Right. PCR using primers containing dP in the 5′-tag.
FIG. 4 . Autoradiograph of an electrophoresis gel showing nested PCR products obtained as described in Example 2.
FIG. 5 . Autoradiograph of an electrophoresis gel showing primer extension products obtained as described in Example 3 from amplicons containing adjacent dZs.
FIG. 6 . Autoradiograph of an electrophoresis gel showing primer extension products obtained as described in Example 4.
FIG. 7 . Autoradiograph of an electrophoresis gel showing PCR products obtained as described in Example 5
FIG. 8 . Autoradiograph of an electrophoresis gel showing that nested PCR external primers containing AEGIS components produces cleaner PCR products (right) than with standard external primers (left).
DETAILED DESCRIPTION OF THE INVENTION
6-Amino-5-nitro-3-(1′-beta-D-2′-deoxyribofuranosyl)-2(1H)-pyridone (dZ), its protected phosphoramidite derivatives suitable for chemical oligonucleotides synthesis, its triphosphate and its thiotriphosphate are reported in U.S. patent application Ser. No. 11/372,400 and in [Hut03]; both are incorporated herein by reference. Its complement, 2-amino-8-(1′-β-D-2′-deoxyribofuranosyl)-imidazo[1,2-α]-1,3,5-triazin-4(8H)-one (implementing puAAD, as dP) and these derivative are reported in [Hut03][Yan06], the synthetic procedures therein being incorporated herein by reference. These are preferred as non-standard nucleotides in the instant invention, although any non-standard nucleotide shown in FIG. 1 might be used in an eternal primer in a PCR.
It is known in art published less than a year before the priority date of the instant application [Yan07] that PCR amplification is possible for oligonucleotides that contain a single dP or a single dZ in the amplicon. However, the prior art shows that upon multiple PCR cycles, dP and dZ are removed from the amplicon. The instant invention was made following first the recognition it was possible to place dP and/or dZ in the PCR primers themselves. To amplify standard oligonucleotides, the dP and dZ would not be in the region of the primer that contacts that target, but rather within an oligonucleotide tag (or tail) appended to the 5′-end of the PCR primer that does contact the standard oligonucleotide target. PCR primers having two parts, a 5′-end containing dP and/or dZ (as well as standard nucleotides, optionally) and a 3′-end that is complementary to the target, are called “chimeric primers”. PCR amplification with chimeric primers is then done in a nested fashion [Bro97]. Any loss of the non-standard nucleotide is restored in a subsequence PCR cycle, solving the loss problem described in the literature. After the chimeric primers are consumed in the first cycles, “external primers” having the sequence of only the 5′-tags continue the PCR.
Not known in any art published before the priority date of the instant application, and not anticipatable from the prior art given the idiosyncrasies of polymerases when challenged with unnatural nucleoside triphosphate substrates [Hor95], it was then discovered that PCR could succeed with certain polymerases even for amplicons that contain multiple dPs and/or multiple dZs. Further, we disclose here for the first time that certain polymerases support incorporation of adjacent dZs and adjacent dPs in prime extension reactions
A third discovery was also unanticipated by us or the art. It turned out that by doing nested PCR with dZ and/or dP in the external primers, it was possible to obtain cleaner PCR products. Given this result, it became evident that PCR with dZ and dP in the primers was a useful, patentable invention, as is herein claimed.
Accordingly, the invention together with its associated discoveries provides a process for amplifying an oligonucleotide sequence in a PCR format, where a forward chimeric primer and a reverse chimeric primer are contacted with that target sequence. The forward chimeric primer is complementary to a region at the 3′-end of said sequence (as in any PCR), the reverse chimeric primer is identical in sequence to a region at the 5′-end of said sequence (as in any PCR), and the forward and reverse primers are joined at their 5′-prime ends to oligonucleotide tags having independently selected sequences that contain at least one non-standard nucleotide (see FIG. 1 ), where the presently preferred non-standard nucleotide is dZ or dP, most preferably dP. Then, as with standard OCR, the mixture is incubated the mixture with a DNA polymerase, RNA polymerase, or a reverse transcriptase, depending on the nature of the oligonucleotide to be amplified, together with the triphosphates needed to complement the nucleotides in the primers and sequence. The presently preferred polymerases are Phusion and Vent or Deep Vent having exonuclease activity, as described further in the examples. This process, of course, comprises a simpler PCR process that amplifies an oligonucleotide sequence that contains one or more non-standard nucleotides, preferably dZ or dP. PCR amplification of an oligonucleotide containing just one was disclosed less than a year before the priority date in [Yan07], and therefore is patentable under United States law. PCR amplification of oligonucleotides containing more than one non-standard nucleotide and adjacent non-standard nucleotides was not in the prior art prior to the priority date, and is not rendered obvious by [Tan07], and is therefore internationally patentable.
EXAMPLES
Example 1
PCR with dZ and dP
This example demonstrates that chimeric primers containing dZ and dP in their external segments support PCR. The following oligonucleotides were prepared by phosphoramidite synthesis. These include two reverse chimeric primers, identical except that in R-36-Nest, some of the G's were replaced by P's in the segment not complementary to the template:
R-36-Std: SEQ ID 1 3′- CCATGGTAGCTATGCGCAA CGCTAGCGAGGAAGGAC-5′-P 32 R-36-Nest: SEQ ID 2 3′- CCATGGTAGCTATGCGCAA CPCTAPCGAPGAAPGAC-5′-P 32
a pair of complementary template sequences:
Temp-R-47: SEQ ID 3 5′-CCATGGGAGACCGCGGTGGGCCCGGCCGGGTACCATCGATACGCG TT-3′ Temp-F-47: SEQ ID 4 3′-GGTACCCTCTGGCGCCACCCGGGCCGGCCCATGGTAGCTATGCGC AA-5′
and two forward chimeric primers, one with the same replacements:
(F-34-Nest)
5′-CTAPGACPACGPACTPC CCATGGGAGACCGCGGT -3′
SEQ ID 5
(F-34-Std)
5′-CTAGGACGACGGACTGC CCATGGGAGACCGCGGT -3′
SEQ ID 6
The underlined portions of the primers are complementary to the template. The portions not underlined are the tags that contain non-standard nucleotides. In separate experiments the chimeric and non chimeric primers were incubated under the following conditions:
Final
Components
Volume (μl)
Concentration
Nuclease-Free Water
1.6
(final volume of 20 μl)
Forward Primer: F-34-Nest (2 pmol/μl)
5
500
nM
Reverse Primer: R-36-Nest (1 pmol/μl,
1
50
nM
radiolabeled)
Reverse Primer: R-36-Nest
6
450
nM
(1.5 pmol/μl)
Template:
Temp-F-47(1 pmol/μl)
0.1 for each
5
nM
Temp-R-47(1 pmol/μl)
10 × Reaction Buffer
2
1×
dNTP (2 mM of each dNTP)
2
0.1
mM each
dZTP (2 mM) or Water (for negative
2
0.1
mM
control)
Taq (5 U/μl)
0.2
0.05
U/μl
The products were resolved by gel electrophoresis ( FIG. 3 ). These results show that primers containing multiple dP's support PCR works. The experiment does not show, however, that primers containing consecutive dPs effectively support PCR.
Example 2
Nested PCR
This experiment demonstrated the use of dZ and dP pairing in the external segments of a nested PCR [Bro97], shown schematically in FIG. 2 . The following oligonucleotides were prepared by phosphoramidite synthesis. These were set up in three set of nested PCR experiments. The first used external primers, one containing dP, the other not:
F-17-Nest 32 P-5′-CTAPGACPACGPACTPC-3′ SEQ ID 7 F-17-Std 32 P-5′-CTAGGACGACGGACTGC-3′ SEQ ID 8
applied in a direct PCR experiment for a longer template that included Temp-R-47 in its middle:
Temp-R-81: SEQ ID 9 5′-CTAGGACGACGGACTGCCCATGGGAGACCGCGGT GGGCC C GGCCG GGTACCATCGATACGCGTTGCGATCGCTCCTTCCTG-3′
and two reverse external primers, one containing dP, the other not:
R-17-Std:
3′-CGCTAGCGAGGAAGGAC-5′
SEQ ID 9
R-17-Nest:
3′-CPCTAPCGAPGAAPGAC-5′
SEQ ID 10
These were incubated using the following procedure in Experiment A.
Volume
Final
Components
(μl)
Concentration
Nuclease-Free Water
7.65
(final volume of 20 μl)
Forward Primer: F-17-Std or Nest
2.25
225
nM
(2 pmol/μl)
Forward Primer: F-17-Std or Nest
0.5
25
nM
(1 pmol/μl, radiolabeled)
Reverse Primer: R-17-Std or Nest
2.5
250
nM
(2 pmol/μl)
Template: Temp-R-81 (0.01 pmol/μl)
0.5
0.25
nM
10 × Reaction Buffer (MgCl 2 (15 mM))
2
1 × (MgCl 2 (1.5 mM))
MgCl 2 (25 mM)
0.4
MgCl 2 (0.5 mM)
dNTP (2 mM of each dNTP)
2
0.2
mM each
dZTP (2 mM)
2
0.2
mM
Taq (5 U/μl)
0.2
0.05
U/μl
The standard primers F-17-Std and R-17-Std should amplify the Temp-R-81 target, leading to a band in a gel electrophoresis resolution that migrates as an 81-mer. This is in fact the case ( FIG. 4 , A-Std lane). If dP does not bind to dC, then the AEGIS dP-containing primers should not yield and 81-mer band. This is also the case ( FIG. 4 , A-AEGIS).
In another experiment, the following recipe was used in a nested PCR experiment:
Volume
Components
(μl)
Final Concentration
Nuclease-Free Water
6.65
(final volume of 20 μl)
Forward Primer: F-17-Std or Nest
2.25
225
nM
(2 pmol/μl)
Forward Primer: F-17-Std or Nest
0.5
25
nM
(1 pmol/μl, radio-labeled)
Reverse Primer: R-17-Std or Nest
2.5
250
nM
(2 pmol/μl)
Template: Temp-R-47(0.01 pmol/μl)
0.5
0.25
nM
F-34-Std or F-34-Nest (0.1 pmol/μl)
0.5
2.5
nM
R-36-Std or R-36-Nest (0.1 pmol/μl)
0.5
2.5
nM
10 × Reaction Buffer (MgCl 2 (15 mM))
2
1 × (MgCl 2 (1.5 mM))
MgCl 2 (25 mM)
0.4
MgCl 2 (0.5 mM)
dNTP (2 mM of each dNTP)
2
0.2
mM each
dZTP (2 mM)
2
0.2
mM
Taq (5 U/μl)
0.2
0.05
U/μl
Note:
1 × standard Taq Reaction Buffer (10 mM Tris-HCl, 50 mM KCl, 1.5 mM MgCl 2 , pH 8.3 at 25° C.).
1 × ThermoPol Reaction Buffer (20 mM Tris-HCl, 10 mM (NH 4 ) 2 SO 4 , 10 mM KCl, 2 mM MgSO 4 , 0.1% Tritonx-100, pH 8.8 at 25° C.).
Experiment B used F-34-Std and R-36-Std as chimeric primers. These should generate products when amplified with external primers built without dP, but not when amplification was sought with external primers containing dP. This was in fact the case ( FIG. 4 , B-Std and B-AEGIS, respectively). Experiment C used F-34-Nest and R-36-Nest as chimeric primers. These should not generate products when amplified with external primers built with dP, but should generate when amplification was sought with external primers containing dP. This was in fact the case ( FIG. 4 , C-Std and C-AEGIS, respectively). These experiments shows showed the ability of DNA polymerase to support a six letter PCR with dA, dT, dG, dC, dZ, and dP as the six letters. They also demonstrate the orthogonality of the process. Nested PCR works with AEGIS external primers when it should and not when it should not, and vice versa.
Example 3
Primer Extension Through Adjacent dZs in a Template
Given the well-known idiosyncrasies of polymerases and the possibility of strong neighbor effects [Hor95], it was not clear that these results would be extendable to PCR amplifications where dZ or dP are adjacent in a template, requiring the incorporation of dP and dZ adjacent in the template. The following experiments were done to screen thermophilic polymerases for their ability to incorporate dPTP opposite dZ in the template. This was done at the following concentrations: [dATP]=[dCTP]=[dTTP]=100 microM), dGTP (5 microM to 100 microM), or dPTP (5 microM to 100 microM) at pH7.0 or 7.5, with the following oligonucleotides (R-19-S was P-32 labeled at its 5′-end):
R-19-S:
SEQ ID 11
5′-GGTACCATCGATACGCGTT-3′
R-36-Nest-6Z:
SEQ ID 12
3′-CCATGGTAGCTATGCGCAAGTZZTTZZTCGZTAGZG-5′
5′- 32 P-labeled primer R-19-S (2 pmole, final assay concentration 50 nM) was annealed to a template sequence R-36-Nest-6Z (3 pmole, final assay concentration 75 nM) by heating (5 min 95° C.) and then slow cooling (0.5 h) to room temperature. dATP, dTTP and dCTP (4 nmole each, final 100 microM) and dGTP (final 10 microM), or dPTP (final 10 microM) were added at room temperature. The reaction mixture was pre-incubated at 72° C. for 30 seconds and followed by the addition of Taq DNA polymerase to give a final volume of 40 microL. The mixture was incubated at 72° C. for 4 minutes, and quenched by dilution into PAGE loading/quench buffer (10 microL, 10 mM EDTA in formamide). Samples were resolved by electrophoresis using a 14% PAGE (7 M urea). The gel was analyzed using MolecularImager software.
These results ( FIG. 5 ) showed that Vent and Deep Vent performed better than Taq. Without wishing to be bound by theory, this may be due to their exonuclease activities.
Example 4
Incorporation of dZTP Opposite Consecutive Template dPs
To compare the efficiency and fidelity of DNA polymerases (Taq, Vent (exo+), and DV (exo+)) incorporating dZTP opposite two consecutive dPs in a template, 5′- 32 P-labeled primer T7-Y-RS-S16 (0.2 pmole of hot primer plus 4 pmole of cold primer, final assay concentration 70 nM) was annealed to template T7-PP-Temp (6 pmole, final assay concentration 100 nM) in 1×. Thermopol polymerase reaction buffer (20 mM Tris-HCl, 10 mM (NH 4 ) 2 SO 4 , 10 mM KCl, 2 mM MgSO 4 , 0.1% Triton X-100, pH=8.0 at room temperature) by heating (5 min at 95° C.) and then slow cooling (0.5 h) to room temperature. dNTP (each final 0.1 mM) and dZTP (final 0.1 mM, with (+) or without (−)) were added at room temperature. The reaction mixture was cooled to 4° C. for 1 min and followed by the addition of Taq (2.5 units), Vent (exo+), or Deep Vent (exo+) DNA polymerase (2 units for Vent and Deep Vent) to give a final volume of 60 microL. The primer was extended at 65° C. and aliquots (7 microL) were taken from each reaction at time intervals (1, 2, 4, 8, and 16 min), quenched by PAGE loading/quench buffer (7 microL, 10 mM EDTA in formamide) and resolved by electrophoresis using a 16% PAGE (7 M urea). The gel was analyzed using MolecularImager. These oligonucleotides were used:
Negative control (−): dNTP (each 0.1 mM)
T7-Y-RS-S16:
SEQ ID 13
3′-GAAAT*CACTCCCAATTAAGCG-5′
T7-PP-Temp:
SEQ ID 14
5′-GCGTAATACGACTCACTATAGACGAPPCTACTTTAGTGAGGGTTA
ATTCGC-3′
Positive control (+): dNTP (each 0.1 mM), and
dZTP (0.1 mM)
T7-Y-RS-S16:
SEQ ID 15
3′-GAAAT*CACTCCCAATTAAGCG-5′
T7-PP-Temp:
SEQ ID 16
5′-GCGTAATACGACTCACTATAGACGAPPCTACTTTAGTGAGGGTTA
ATTCGC-3′
The order of performance of the polymerases tested is Deep Vent (exo+)>Vent (exo+)>Taq. In the absence of dZTP, Deep Vent and Vent misincorporates only one dCTP opposite the first dP. However, Taq can misincorporate dCTP opposite two consecutive dPs, and then keep extending primer. All are better than exo(−) polymerases (not reported in [Yan07]).
Example 5
PCR with Amplicons Containing Multiple Adjacent dPs and dZs
To compare the outcome of PCR with templates containing one or two adjacent dPs, the following oligonucleotides were prepared:
T7-Z-RS-S16:
SEQ ID 17
5′-GCGTAATACGACTCAC*TATAG-3′
(Template-A)
T7-G-51-Std:
SEQ ID 18
5′-GCGTAATACGACTCACTATAGACGAGCGTACTTTAGTGAGGGTTA
ATTCGC-3′
(Template-B)
T7-P-Temp:
SEQ ID 19
5′-GCGTAATACGACTCACTATAGACGAPCGTACTTTAGTGAGGGTTA
ATTCGC-5′
(Template-C)
T7-PP-Temp:
SEQ ID 20
5′-GCGTAATACGACTCACTATAGACGAPPCTACTTTAGTGAGGGTTA
ATTCGC-3′
T7-Y-RS-S16:
SEQ ID 21
3′-GAAAT*CACTCCCAATTAAGCG-5′
These were incubated under the following conditions:
Volume
Components
(μl)
Final Concentration
Nuclease-Free Water
17
(final volume of 40 μl)
Forward Primer: T7-Z-RS-S16
1
0.25
μM
(10 pmol/μl)
Reverse Primer: T7-Y-RS-S16
1
0.25
μM
(10 pmol/μl)
Template: Three different Templates
1 + 4 (H2O)
0.25
nM
(A, B, and C) (0.01 pmol/μl)
10 × Thermopol Buffer (pH = 8.0)
4
dNTP (2 mM)
4
0.2
mM each
dZTP (2 mM)
4
0.2
mM
dPTP (2 mM)
4
0.2
mM
Hot Start Taq (5 U/μl)
0.5
0.06
U/μl
ThermoPol Reaction Buffer (20 mM Tris-HCl, 10 mM (NH 4 ) 2 SO 4 , 10 mM KCl, 2 mM MgSO 4 , 0.1% Triton X-100, pH 8.0 at 25° C.).
PCR: one cycle of 95° C. for 15 min; 26 cycles of 95° C. for 20 s, (55° C. for 30 s, 72° C. for 1 min or 2 min; 72° C. for 5 min; then stored at 4° C.
The results are shown in FIG. 7 . All PCRs generates some degree of 51-mer product. Template A contained only standard nucleotides. Template B contained a single dP. Template C contained a series of dPs, including two adjacent dPs.
Example 6
Prevention of Primer Dimerization with AEGIS Containing Primers
To demonstrate that if dP or dZ were incorporated into PCR primers in place of one or more dGs or dCs, then the synthetic primers containing dPs or dZs would not find their perfectly matched complementary strands in a primer pool, a 17-mer, 5′-CAGGAAGGAGCGATCGC-3′ (SEQ ID 35) was deliberately designed to form a self-dimer with 8 base pairs at the 3′-end (underline region, T m =32° C.), and subjected to PCR conditions. As expected, primer-dimer formed rapidly. In contrast, perfectly mismatched primers 5′-CAGGAAGGAGCPATCPC-3′ (SEQ ID 36) and 5′-CAGGAAGGAGZGATZGC-3′ (SEQ ID 37), which would form primer-dimers only by mismatching dP with dC (in the first case) and dZ with dG (in the second) gave no detectable amplicon under the same conditions, even after 45 cycles.
Example 7
Preferred DNA Polymerases and Optimized Amplification Conditions
With several polymerases able to replicate efficiently DNA fragments containing multiple dPs and dZs, the preferred polymerase having the highest PCR efficiency to amplify target using a nested PCR architecture with AEGIS nucleotides in the external primers was determined. Taq, 9° N, Deep Vent (both exo + and exo − ), Vent (both exo + and exo − ), Phusion, and Herculase were tested; the PCR efficiency was monitored by real-time PCR. The polymerase has the higher PCR efficiency generates more PCR amplicon and producing higher fluorescence signal at an earlier cycle of the PCR. Phusion was found to have the highest PCR efficiency among the polymerases tested with proofreading activity; Deep Vent (exo − ) is the most efficient among all the polymerases without exonuclease activity. For all polymerases tested, dP-containing nested PCR, in general, has higher PCR efficiency than that of the dZ-containing nested PCR.
Phusion DNA polymerase generates long templates with an accuracy and speed previously unattainable with a single enzyme. In addition, the error rate of Phusion is 50-fold lower than that of Taq, and about 6-fold lower than that of Vent and Deep Vent. Therefore, Phusion DNA polymerase was further optimized as a presently preferred polymerase for nested PCR with dP-containing external primers. The major infidelity during the 6-nucleotide PCR arises from misincorporation of dGTP opposite template dZs or dZTP opposite template dGs. This infidelity is pH dependent, when the pH of the buffer is low, the rate of misincorporation decreases.
To determine a preferred pH for PCR efficiency and fidelity, three types of nested PCR were conducted with Phusion HF buffer at four different pH values (7.0, 7.5, 8.0, and 8.5). Amplification was monitored by the real-time PCR with SYBR Green. For “type A” nested PCR, standard external and chimeric primers and four standard nucleotide triphosphates (dNTPs) were used; amplification curves in real-time show that PCR efficiency increases when the pH of the buffer decreases. After 30 cycles, the melting temperature of each PCR amplicon was measured and the size of each amplicon was analyzed by agarose (3%) gel. The T m of each PCR amplicon generated under four different pH values is roughly the same (about 91.49±0.5° C.).
The type B nested PCR is identical to the type A nested PCR, except that dZTP was also included into the reaction. By comparing the melting temperature of each PCR amplicon in the type B reaction with that of the type A reaction, misincorporation of dZTP at different pHs was measured. The T m of the amplicon improves as the pH of the reaction buffer decreases. For example, at the highest pH value tested (8.5), the T m of the PCR amplicon is 3.75±0.05° C. below than that of the control PCR (type A); at the lowest pH value (7.0), the ΔT m was to 0.29±0.05° C. below the fully standard PCR. For the type C nested PCR, dP-containing primers were used instead of standard primers, and PCR amplifications were conducted under the same conditions as type B nested PCR. The T m of each PCR amplicon increases as the pH value of the reaction buffer decreases; the effect of pH on PCR efficiency and misincorporation of dZTP opposite template dG agreed with that with type B nested PCR. However, the T m of each PCR amplicon in the type C nested PCR is higher (about 3.6° C.) than in type B nested PCR, this enhancement of the T m is mainly due to the higher thermostability of the Z:P base pairs in the PCR amplicon.
The PCR amplicons obtained at four different pHs in type B nested PCR were cloned, and their sequences were verified by Sanger sequencing. This shows that misincorporation of dZTP opposite template G is insignificant and does not prevent the PCR amplicon of interest to be cloned and sequenced using the conventional Sanger method. This too was not expected given [Yan07], and can be used as a restrictive element of a claim.
Example 8
Nested PCR with AEGIS External Primers Cleans Up Multiplexed PCR
To show whether the dP-containing nested PCR can enhance the capability of multiplexed PCR, this system was applied to human genomic DNA, targeting the three genes associated with cancer: TOP1, HBEGF, and MYC. The oligonucleotides used in this experiment were:
Top-F-External
SEQ ID 22
5′-TPTAPATTTPTATPTATPTATPAT-3′
Top-F-Chimeric
SEQ ID 23
5′-TPTAPATTTPTATPTATPTATPATGACAGCCCCGGATGAGAAC-3′
TOP-R-Chimeric
SEQ ID 24
3′-GTTAGCTCGACAACGTTAAGAACAPAGGPAAATPACTCPCA-5′
Universal-R-4P
SEQ ID 25
3′-CAPAGGPAAATPACTCPCA-5′
HBE-F-External
SEQ ID 26
5′-AAAPTATAPTAAPATPTATAPTAG-3′
HBE-F-Chimeric
SEQ ID 27
5′-AAAPTATAPTAAPATPTATAPTAGCCCCAGTTGCCGTCTAGGA-3′
HBE-R-Chimeric
SEQ ID 28
3′-TTCACGGTTTGTCTCATACAGGCCAPAGGPAAATPACTCPCA-5′
Universal-R-4P
SEQ ID 29
3′-CAPAGGPAAATPACTCPCA-5′
MYC-F-External
SEQ ID 30
5′-GTATTTPAPTAAPTAATTPATTPA-3′
MYC-F-Chimeric
SEQ ID 31
5′-GTATTTPAPTAAPTAATTPATTPATCCTCCTTATGCCTCTATC
AT-3′
MYC-R-Chimeric
SEQ ID 32
3′-CCTGAGAACTAGTTTCGCGCCCAPAGGPAAATPACTCPCA-5′
Universal-R-4P
SEQ ID 33
3′-CAPAGGPAAATPACTCPCA-5′
The external primers were adopted from Luminex's 5′-universal tag sequences, which were designed by the company to have unique sequences to avoid cross-hybridization and have roughly equal melting temperatures. To design the chimeric primers, universal external primer was added to either forward or reverse gene-specific primers, the other three external primers were also attached to gene-specific primers, the combination of each external primer to a certain gene-specific primer was optimized using primer design software (OligoAnalyzer 3.1), and following the general principles of multiplex PCR primer design to avoid cross-hybridization and hairpin structure of primers.
Three cancer genes in human genomic DNA were multiplexed amplified by standard nested PCR and dP-containing nested PCR using Phusion under seven different annealing temperatures. As shown in FIG. 8 , standard nested PCR with all annealing temperatures give messy PCR results (left): at the lower annealing temperatures (from 53.4° C. to 58.8° C.), significant amounts of primer dimer (about 40 nucleotides in length) were generated; at the higher annealing temperatures (from 61.5° C. to 65.5° C.), non-specific PCR artifacts (PCR amplicons longer than the desired length) were produced along with the disappearance of the primer dimer.
However, the dP-containing nested PCR generated the desired PCR amplicons with minimal PCR artifacts (right). For the two control reactions (without genomic DNA), control A (standard nested PCR) gave some primer dimers (a 40-mer amplicon formed by standard external primers) and significant amount of long PCR amplicons, which may caused by the further priming from the primer dimer. The control B (dP-containing nested PCR) gave one band, which was formed by the dimerization of the dP-containing chimeric primers, as the 3′-ends of the chimeric primers are the standard gene-specific oligonucleotides. This dimerization could be further eliminated by reducing the concentration of the dP-containing chimeric primers. We further verified that the dP-containing multiplexed nested PCR also performed better than the standard nested PCR under HF Phusion buffer with other different pH values (8.5, 8.0, and 7.5).
This result was entirely unanticipated. Nested PCR using AEGIS external primers leads to cleaner multiplexed PCR. Without wishing to be bound by theory, this may arise because even with standard primers not having exact matched in a genome, standard primers have sufficient mismatches to prime at off-target sites.
LITERATURE CITED
[Bro97] Brownie, J., Shawcross, S., Theaker, J., Whitcombe, D., Ferrie, R., Newton, C., Little, S. (1997). Nucleic Acids Res. 25, 3235-3241
[Hor95] Horlacher, J., Hottiger, M., Podust, V. N., Hübscher, U., Benner, S. A. (1995) Proc. Natl. Acad. Sci., 92, 6329-6333
[Hut03] Hutter, D. and Benner, S. A. (2003) J. Org. Chem., 68, 9839-9842
[Swi89] Switzer, C. Y., Moroney, S. E., Benner, S. A. (1989) Enzymatic incorporation of a new base pair into DNA and RNA. J. Am. Chem. Soc. 111, 8322-8323
[Voe96a] Voegel, J. J., Benner, S. A. (1996) Helv. Chim. Acta 79, 1863-1880
[Voe96b] Voegel, J. J., Benner, S. A. (1996) Helv. Chim. Acta 79, 1881-1898
[Voe93] Voegel, J. J., von Krosigk, U., Benner, S. A. (1993) Synthesis and tautomeric equilibrium of 6-amino-5-benzyl-3-methylpyrazin-2-one. An acceptor-donor-donor nucleoside base analog. J. Org. Chem. 58, 7542-7547
[Von95] von Krosigk, U., Benner, S. A. (1995) J. Am. Chem. Soc. 117, 5361-5362
[Yan06] Yang, Z., Hutter, D., Sheng, P., Sismour, A. M. and Benner, S. A. (2006) Nucleic Acids Res., 34, 6095-6101.
[Yan07] Yang, Z., Sismour, A. M., Sheng, P., Puskar, N. L., Benner, S. A. (2007) Nucl. Acids Res. 35, 4238-4249
|
The disclosed invention teaches processes to amplify oligonucleotides by contacting templates and primers with DNA polymerases and triphosphates of non-standard nucleotides, which form nucleobase pairs fitting the standard Watson-Crick geometry, but joined by hydrogen bonding patterns different from those that join standard A:T and G:C pairs. Thus, this invention relates to nucleotide analogs and their derivatives that, when incorporated into DNA and RNA, expand the number of replicatable nucleotides beyond the four found in standard DNA and RNA. The invention further relates to polymerases that incorporate those non-standard nucleotide analogs into oligonucleotide products using the corresponding triphosphate derivatives, and more specifically, polymerases and non-standard nucleoside triphosphates that support the polymerase chain reaction (PCR), including PCR where the products contain more than one non-standard nucleotide unit.
| 2
|
This application claims the benefit of U.S. Provisional Application 60/084,096 filed May 4, 1998
BACKGROUND OF THE INVENTION
This invention relates to the generation of electric power from a source of energy whose energy output is highly variable and, in particular, to the efficient generation of electrical power even when the amplitude and frequency of the energy supplied by the source of energy vary over a wide range.
There is growing interest in obtaining electrical power from “clean” sources of energy such as ocean waves and/or air currents. However, these “natural” sources of energy produce energy whose amplitude and frequency vary widely. As a result of these variations, even where a system exists for capturing energy present in ocean waves and/or air currents, a problem exists in how to efficiently transform the captured energy into electric power.
For purpose of illustration, the generation of power from ocean waves will be used in the description to follow. Capturing the energy present in ocean waves is problematic because the amplitude of the waves is constantly varying and the frequency (or period) of the waves also varies constantly. An additional problem in capturing the constantly varying energy present in ocean waves is to do so efficiently because, in typical power conversion systems, the efficiency of power conversion falls off rapidly when the system is operating outside of a relatively narrow range of power conversion rates.
SUMMARY OF THE INVENTION
An electric power generating system embodying the invention includes a mechanical means for capturing energy available from a natural source of energy, where the energy available from the source varies in rate, amplitude and frequency. The variable mechanical energy thus captured is used to drive a generator at a variable rate of rotation. It is known that, dependent upon the parameters of the generator used, for each speed of rotation of the generator, there exists a corresponding preferred output voltage of the generator at which the efficiency of conversion of mechanical energy to electrical energy is a maximum.
In accordance with this invention, both the speed of operation of the generator and the output voltage of the generator are sensed. Then, in response to these sensed values, the impedance of the load into which the generator output power is fed is varied for driving the voltage thereacross towards that preferred output voltage of the generator corresponding to the maximum efficiency operation of the generator at the actual sensed speed of operation of the generator.
In a preferred embodiment, the generator load comprises a capacitor. The generator output power (in d.c. form; either directly from a d.c. generator or rectified from an a.c. generator) is fed directly into the capacitor, and the voltage across the capacitor, corresponding to the output voltage of the generator, is continuously monitored. Simultaneously with the feeding of power to the capacitor, power is extracted from the capacitor during spaced apart short time intervals. By varying the rate of power extraction from the capacitor relative to the rate of power fed thereto by the generator, the voltage across the capacitor is driven towards a preferred voltage corresponding to the instantaneous sensed speed of operation of the generator. The preferred generator output voltage is obtained based upon the known speed versus preferred generator output voltage characteristic of the generator being used, e.g., by calculation or by the use of a look-up table or the like. The rate of power extraction from the generator is controlled in response to an error signal obtained by comparing the sensed output voltage across the capacitor against the looked-up preferred generator output voltage corresponding to the sensed speed of operation of the generator.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a semi-block, semi-circuit diagram of an electric power generating system embodying the invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention has utility in a large variety of embodiments using various components for converting various sources of variable energy into electrical energy with a high degree of conversion efficiency. One example of a complete system using the present invention is first described.
In the embodiment shown in FIG. 1, a buoy 12 , located in a body of water, is used to capture energy present in ocean waves and/or in the movement of a body of water and to produce mechanical forces coupled to a hydraulic cylinder 14 . The hydraulic cylinder is coupled to a hydraulic rectifier 16 whose output is fed to an accumulator 18 whose output is coupled to, and drives, a hydraulic motor 20 . The motor 20 has a shaft 21 which is mechanically coupled to the shaft of an electric a.c. generator 22 .
To the point described, the system for capturing the naturally occurring mechanical energy (via the float) and for using the captured energy for driving an electrical generator can be in accordance with known systems. In the present example, energy is being captured by water motion, e.g., waves on the surface of a body of water. The amount of energy arriving with such waves is, as is typical with most “natural” sources of mechanical energy, e.g., moving fluids, randomly variable from energy levels too small to overcome the inertia of an energy conversion system to energy levels (e.g., during ocean storm conditions) so high as to require at least partial shutdown of the conversion system to avoid system damage. Thus, in general, energy conversion systems, including preferred embodiments of the present invention, are designed to operate in and to capture energy from only a range of energies available from the particular energy source being used.
In many prior known conversion systems, not only must the range of available energies be limited, particularly against damage from excessive energies, but various means must be employed for conditioning the power being transmitted such that the power arriving at the mechanical energy to electrical energy converter or transducer, e.g., an electrical generator, is properly matched with the energy converter. As previously explained, the conversion efficiencies of, for example, electrical generators, are typically a function of the operating speeds of rotation of the generators. Thus, speed control mechanisms are typically employed in known systems for regulating the generator speeds in response to varying input energy levels. Such speed regulating mechanisms reduce the efficiency of the systems. A significant advantage of the present invention, however, is that within a selected range of randomly arriving energies, the range being limited only for preventing damage to the system from excessively high energy levels, all the varying amounts of arriving energies are applied “directly” to the electrical generator, i.e., without regulation. Accordingly, the speed of generator rotation is essentially determined by and directly proportional to the amount of captured and transmitted mechanical energy. Little or no energy is lost to speed regulating means and, most significantly, at all levels of energy being transferred, the generator functions at optimal energy conversion efficiencies.
Returning to a consideration of the illustrative power drive train shown in FIG. 1, the motor 20 drives the electric generator 22 for converting the mechanical energy to electrical energy. Operation of the illustrative system requires generation of a d.c. voltage and, using an a.c. generator 22 , the a.c. output from the generator is coupled to a full wave rectifier 24 . A d.c. voltage V 1 is produced across the output terminals 23 , 25 of the rectifier 24 . A capacitor C 1 is connected across the output terminals 23 and 25 of the full wave rectifier 24 . The output of the rectifier is applied to the input of a switching regulator 26 whose output provides power to a load 28 .
The switching regulator 26 includes a controllable switch T 1 . In this embodiment, T 1 is a bipolar PNP translator with its emitter connected to terminal 23 and its collector connected to a terminal 30 at which is produced a positive going output voltage. An inductor L 1 is connected between terminals 30 and 31 . A diode D 1 is connected at its cathode to node 30 and at its anode to terminal 25 , and a storage capacitor C 2 is connected between terminals 31 and 25 to store the output voltage.
The base of T 1 is connected to an output of a control circuit 32 . The turn on and turn off of T 1 is controlled by the control circuit 32 which is responsive to an error signal determined by a comparison of the amplitude of the voltage V 1 and a target voltage which is a function of the speed at which the motor 20 causes the generator 22 to rotate. The amplitude of the voltage V 1 is applied via line 34 to an input of the control circuit 32 , and the rotational speed of the motor shaft 21 is sensed by a sensor 35 to produce a corresponding signal which is applied via line 36 to the control circuit 32 . The functioning of the control circuit 32 is described hereinafter.
The problem faced by Applicant may be expressed as follows:
It is known that, for any given speed of rotation for most types of electrical energy generators, maximum efficiency of power conversion occurs when the output voltage of the generator falls within a relatively narrow range of values dependent entirely upon the physical parameters of the generator. Typically, in most large power generating systems, variations in loading of the generator are accommodated by variations of the mechanical power applied, e.g., by a steam driven engine, to the generator; the rotational speed of the generator thus remaining substantially constant and at a speed resulting in the generator operating at maximum power conversion efficiency.
In situations where the input power is variable, e.g., from power sources such as the wind and ocean waves, the preferred practice in the past has been to somehow sense the actual rate of arrival of the input power and to control the transmission of the power to the generator so as to maintain the speed of rotation of the generator within the preferred range. A problem with prior art power transmission speed control systems, however, is that they are complex, costly, and introduce efficiency losses.
In accordance with the present invention, little or no control need be provided over the rate of transmission of the input power to the generator which is thus operated at variable rates of operation. Rather, and based upon the recognition, previously discussed, that maximum efficiency of operation of the generator occurs when the generator output voltage is at a preferred voltage dependent upon the rate of rotation of the generator, the output power from the generator is loaded into a storage element (herein, the capacitor C 1 ) having a variable impedance which is a function of the time average amount of power within the storage element. As known, the output voltage of a generator is a function of the generator output current, which is dependent upon the impedance load on the generator. Here, the impedance load is provided by the capacitor C 1 . Thus, by varying the rate at which power is removed from the storage element, the impedance of the storage element is maintained, for any conditions of operation of the generator, at that average value resulting in the voltage across the element (the output voltage of the generator) being the preferred generator voltage for the actual condition of operation of the generator.
Stated slightly differently, for every given generator, it is known what are the preferred output voltages, for maximum efficiency of operation, corresponding to different rotational speeds of operation of the generator. Known means are used for making available such information in real time. For example, preferred voltages versus operational speeds are stored in a look-up table. Accordingly, for any rotational speed of the generator, as determined by the power then being generated by the natural energy power source, a preferred output voltage of the generator is known. Then, by comparing the actual output voltage of the generator, as measured across the storage element, against the desired output voltage, as determined from the look-up table in correspondence with the detected actual speed of rotation of the generator, the rate of removal of power from the storage element is either increased or decreased as necessary to drive the output voltage to the desired output voltage.
In other embodiments, the preferred output voltage for the sensed operating speed is found, in real time, by use of an appropriate equation or by hardware parameters in an analog system. Using an equation, i.e., a mathematical expression describing the known speed versus output voltage relationship, the desired voltage is calculated for every reading of the operating speed.
In the system illustrated in FIG. 1, operation is as follows:
As previously described, the rectified, d.c. output power from the generator 22 is fed directly into the capacitor C 1 . As the power is fed into the capacitor, the voltage V 1 , corresponding to the output voltage of the generator, begins to rise. Simultaneously with the feed of power into the capacitor C 1 , power is removed from the capacitor by the switching regulator 26 . For any given rate of power generation by the generator, the average voltage across the capacitor C 1 is a function of the average ration of the power fed into the capacitor C 1 by the generator and the power extracted from the capacitor by the regulator 26 . While the power being generated by the generator 22 (and being fed to the capacitor C 1 ) is a function of the power available to the generator, the power being extracted from the capacitor is under the control of the switching regulator 26 (it being assumed that all the extracted power is used, e.g., by being fed directly into a storage battery or being fed into a power grid).
As mentioned, the rate of rotation of the generator is variable, as determined by the amount of power instantaneously available from the power source, and the speed of rotation of the generator is constantly measured. A known speed sensor 35 is used to measure the generator speed and to generate a signal voltage indicative of the generator speed. With the generator speed known, the preferred generator output voltage Vp for the then used speed of generator rotation is determined as previously described.
Simultaneously, the actual output voltage of the generator is determined by measuring the voltage (V 1 ) across the capacitor C 1 . Ideally, the measured voltage V 1 should be equal to the preferred voltage Vp. The two voltages V 1 and Vp are compared within the control circuit 32 and an error signal V E is generated. The output error voltage V E is fed to a pulse width modulator circuit. If the error voltage indicates that the capacitor voltage is low, the output of the pulse width modulator is reduced so that the turn-on time of switch T 1 is reduced. This causes less charge to be drawn out of the capacitor C 1 allowing its voltage to rise. Concurrently, the load presented to the generator is changed; in this case the value of the load impedance is effectively increased. Conversely, if the error voltage indicates that the capacitor voltage is high, the output of the pulse width modulator is increased so the turn on time of switch T 1 is increased. This causes more charge to be drawn out of capacitor, reducing its voltage. In this case, the value of the load impedance is effectively decreased.
The switching regulator 26 , shown in FIG. 1, is but one example of known switching regulators which can be used. Basically, when the switch T 1 is turned on, current (and power) is drained from the capacitor C 1 and flows through the inductor L 1 and into the load. At this time, the diode D 1 is reverse biased and non-conductive. As the current begins to flow through the inductor L 1 , energy is stored therein. When the switch T 1 is turned off, the energy stored within the inductor L 1 is converted back into current and driven, by the voltage now generated across the inductor L 1 , into the load in the same direction of current flow as when the switch T 1 was turned on. At this time, the current flows through a circuit including the diode D 1 which is now forward biased.
Based upon the foregoing description, design of suitable arrangements for practicing the invention will be evident to persons of skill in the power generating arts. Variations from the specific arrangement shown in FIG. 1 are possible. For example:
The types of generators which may be used to practice the invention can include any of the following: a DC permanent magnet generator; a three phase AC permanent magnet generator and rectifier; a single phase AC generator and rectifier; a DC controlled field generator; an AC controlled field generator; and various hybrid types of generators.
The types of rate sensors which may be used to practice the invention include any of the following: a DC tachometer; an encoder (optical, magnetic, etc.); a gear and sensor combination; or any other appropriate sensing device.
The collection capacitor C 1 must have sufficient capacitance such that the DC level is stable at low generator rates and ripple peaks do not exceed the voltage of the power extraction electronics. Effective Series Resistance (ESR) is a consideration due to high ripple current.
The switching regulator switch T 1 is shown to be a PNP bipolar transistor. However, any other appropriate solid state device such as an NPN bipolar transistor, an FET, an IGBT, or a DMOS may be used instead.
The inductor L 1 may be any type of inductor which is suitable for use in a switching regulator application.
The error signal could be used to feed a constant pulse width, rate adjustable circuit instead of a PWM circuit. Likewise, a linear control circuit could be used; but efficiency must be considered.
The output load may include any device that can store or consume the energy transferred to it from the generator. Typical devices to store energy may be batteries or capacitor banks. Typical devices to use (consume) the energy may be heaters, lights, etc. (resistance); or inverters (AC output constant frequency and voltage).
|
Energy from a naturally recurring source of variable mechanical energy is captured and transmitted to an electrical generator causing it to rotate at speeds proportional to the amount of energy captured. The output voltage produced by the generator is a function of the rotational speed imparted to the generator and a load impedance which is coupled via controllable switching circuitry to the generator output. The effective load impedance is varied and controlled by means of a control mechanism responsive to the rotational speed of the generator and the output voltage of the generator which selectively turns the controllable switching circuitry on and off.
| 8
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This is a divisional application of co-pending parent application having U.S. application Ser. No. 12/163,944, filed Jun. 27, 2008, which is a continuation of U.S. application Ser. No. 11/106,256, filed Apr. 13, 2005, now U.S. Pat. No. 7,399,401, which is a continuation-in-part (CIP) of U.S. application Ser. No. 10/683,659, filed Oct. 9, 2003, now U.S. Pat. No. 6,916,159, which claims benefit and priority based on U.S. Provisional Application No. 60/417,464, entitled “Disposable Pump For Drug Delivery System,” filed on Oct. 9, 2002, U.S. Provisional Application No. 60/424,613, entitled “Disposable Pump And Actuation Circuit For Drug Delivery System,” filed on Nov. 6, 2002, and U.S. Provisional Application No. 60/424,414, entitled “Automatic Biological Analyte Testing Meter With Integrated Lancing Device And Methods Of Use,” filed Nov. 6, 2002, each of which is incorporated herein in its entirety by this reference. This non-provisional application is also related to U.S. Pat. No. 6,560,471, entitled “Analyte Monitoring Device and Methods of Use,” issued May 6, 2003, which is incorporated herein in its entirety by reference.
FIELD OF INVENTION
This invention generally relates to fluid delivery devices, systems, and methods. This invention further relates to small volume, disposable medical devices for the precision delivery of medicines or drugs such as insulin, and associated systems and methods.
BACKGROUND OF THE INVENTION
Insulin pumps are widely available and are used by diabetic people to automatically deliver insulin over extended periods of time. All currently available insulin pumps employ a common pumping technology, the syringe pump. In a syringe pump, the plunger of the syringe is advanced by a lead screw that is turned by a precision stepper motor. As the plunger advances, fluid is forced out of the syringe, through a catheter to the patient. The choice of the syringe pump as a pumping technology for insulin pumps is motivated by its ability to precisely deliver the relatively small volume of insulin required by a typical diabetic (about 0.1 to about 1.0 cm 3 per day) in a nearly continuous manner. The delivery rate of a syringe pump can also be readily adjusted through a large range to accommodate changing insulin requirements of an individual (e.g., basal rates and bolus doses) by adjusting the stepping rate of the motor. While the syringe pump is unparalleled in its ability to precisely deliver a liquid over a wide range of flow rates and in a nearly continuous manner, such performance comes at a cost. Currently available insulin pumps are complicated and expensive pieces of equipment costing thousands of dollars. This high cost is due primarily to the complexity of the stepper motor and lead screw mechanism. These components also contribute significantly to the overall size and weight of the insulin pump. Additionally, because of their cost, currently available insulin pumps have an intended period of use of up to two years, which necessitates routine maintenance of the device such as recharging the power supply and refilling with insulin.
U.S. Pat. No. 6,375,638 of Clyde Nason and William H. Stutz, Jr., entitled “Incremental Motion Pump Mechanisms Powered by Shape Memory Alloy Wire or the Like,” issued Apr. 23, 2002, and naming Medtronic MiniMed, Inc. as the assignee, which patent is incorporated herein in its entirety by this reference, describes various ratchet type mechanisms for incrementally advancing the plunger of a syringe pump. The ratchet mechanisms are actuated by a shape memory alloy wire. The embodiments taught by Nason et al. involve a large number of moving parts, and are mechanically complex, which increases size, weight and cost, and can reduce reliability.
SUMMARY OF THE INVENTION
A fluid delivery system constructed according to the present invention can be utilized in a variety of applications. As described in detail below, it can be used to deliver medication to a person or animal. The invention can be applied in other medical fields, such as for implantable micro-pump applications, or in non-medical fields such as for small, low-power, precision lubricating pumps for precision self-lubricating machinery.
In its preferred embodiment, the present invention provides a mechanical insulin delivery device for diabetics that obviates the above-mentioned limitations of the syringe pump namely size, weight, cost and complexity. By overcoming these limitations, a precise and reliable insulin delivery system can be produced with sufficiently low cost to be marketed as a disposable product and of sufficiently small size and weight to be easily portable by the user. For example, it is envisioned that such a device can be worn discretely on the skin as an adhesive patch and contain a three-day supply of insulin after the use of which the device is disposed of and replaced.
The present invention relates to a miniature precision reciprocating displacement pump head driven by a shape memory alloy actuator. Shape memory alloys belong to a class of materials that undergo a temperature induced phase transition with an associated significant dimensional change. During this dimensional change, shape memory alloys can exert a significant force and can thus serve as effective actuators. The shape memory alloy actuator provides an energy efficiency about one thousand times greater than that of a conventional electromechanical actuator, such as a solenoid, and a force to mass ratio about ten thousand times greater. Additionally, the cost of shape memory alloy materials compares favorably to the cost of electromechanical devices with similar capabilities.
The device of the present invention is intended to be operated in a periodic dosing manner, i.e., liquid is delivered in periodic discrete doses of a small fixed volume rather than in a continuous flow manner. The overall liquid delivery rate for the device is controlled and adjusted by controlling and adjusting the dosing period. Thus the device employs a precision timing mechanism in conjunction with a relatively simple mechanical system, as opposed to a complex mechanical system, such as that embodied by the syringe pump.
A precision timing device is an inherently small, simple and inexpensive device. It is an underlying assumption of the invention (and a reasonable conclusion of process control theory) that in the treatment of diabetes, there is no clinical difference between administering insulin in periodic discrete small doses and administering insulin in a continuous flow, as long as the administration period of the discrete dose is small compared to the interval of time between which the blood glucose level is measured. For the present invention, a small dose size is regarded as on the order of 0.10 units of insulin (1 microliter) assuming a standard pharmaceutical insulin preparation of 100 units of insulin per ml (U110). A typical insulin dependent diabetic person uses between 10 and 100 units of insulin per day, with the average diabetic person using 40 units of insulin. Thus the present invention would deliver the daily insulin requirements of the average diabetic person in 400 individual discrete doses of 1 μl each with a dosing period that can be programmed by the user. A pump constructed according to the present invention can have a predetermined discrete dosage volume that is larger or smaller than 1 μl, but preferably falls within the range of 0.5 to 5 μl, and more preferably falls within the range of 1 to 3 μl. The smaller the discrete dose is of a particular pump design, the more energy required by the device to deliver a given amount of fluid, since each pump cycle consumes roughly the same amount of energy regardless of discrete dosage size. On the other hand, the larger the discrete dosage is, the less precise the pump can mimic the human body in providing a smooth delivery rate. A device constructed according to the present invention is also suitable for delivery of other drugs that might be administered in a manner similar to insulin.
It is further intended that the present invention could be used as a disposable component of a larger diabetes management system comprised of additional disposable and non-disposable components. For example, the present invention could be coupled with a continuous blood glucose monitoring device and remote unit, such as a system described in U.S. Pat. No. 6,560,471, entitled “Analyte Monitoring Device and Methods of Use,” issued May 6, 2003. In such an arrangement, the hand-held remote unit that controls the continuous blood glucose monitoring device could wirelessly communicate with and control both the blood glucose monitoring unit and the fluid delivery device of the present invention. The monitor and pump could be physically separate units, or could share one or more disposable and/or non-disposable components. For example, a disposable pump constructed according to the present invention and charged with a 3-day supply of insulin, a small battery and a disposable glucose sensor could be integrated into a single housing and releasably coupled with non-disposable components such as control electronics, a transmitter/receiver and a user interface to comprise a small insulin delivery device that could be worn on the skin as an adhesive patch. Alternatively, the battery (or batteries) and/or sensor could be replaced separately from the disposable pump. Such arrangements would have the advantage of lowering the fixed and recurring costs associated with use of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
A detailed description of various embodiments of the invention is provided herein with reference to the accompanying drawings, which are briefly described below.
FIG. 1A shows a schematic representation of a most general embodiment of the invention.
FIG. 1B shows a schematic representation of an alternative general embodiment of the invention.
FIG. 2A shows a schematic representation of a preferred embodiment of the invention.
FIGS. 2B and 2C show enlarged details of a preferred embodiment of the invention.
FIG. 3 shows a schematic representation of a preferred embodiment of a check valve to be used in the invention.
FIG. 4 shows a schematic representation of a preferred embodiment of a pulse generation circuit to be used with the invention.
FIG. 5 shows data from the experimental characterization of the reproducibility of a functional model of the invention.
FIG. 6 shows data from the experimental characterization of the energy utilization of a functional model of the invention.
FIG. 7 shows a schematic representation of a first alternative embodiment of the invention.
FIG. 8 shows a schematic representation of a second alternative embodiment of the invention.
FIG. 9 shows a schematic representation of a first alternative embodiment of a pulse generation circuit to be used with the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A device of the present invention includes a miniature precision reciprocating displacement pump driven by a shape memory alloy wire linear actuator and controlled by a programmable pulse generating circuit. For purposes of description, the device is divided into three subcomponents, a precision miniature reciprocating displacement pump head, a shape memory alloy linear actuator, and a programmable pulse generating circuit. Each subcomponent is comprised of multiple elements. A schematic representation of a most general embodiment of the invention is shown in FIG. 1A and is described below.
The miniature precision pump head is comprised of the following elements: a rigid substrate 101 to which other components may be attached so as to fix their orientation and position relative to one another, a fluid reservoir 102 for storing the fluid to be pumped 103 and a small cavity, henceforth referred to as the displacement cavity 104 , whose volume can be varied between precisely defined limits. The limit corresponding to a state of maximum volume for the displacement cavity 104 is defined as the first limit 105 and the limit corresponding to a state of minimum volume for the displacement cavity 104 is defined as the second limit 106 . An inlet conduit 107 connects the displacement cavity 104 to the fluid reservoir 102 and thus permits fluid flow between the two. An inlet check valve 108 is situated within the inlet conduit 107 such that fluid flow is restricted to flowing from the fluid reservoir 102 to the displacement cavity 104 . An outlet conduit 109 connects the displacement cavity 104 to some point 111 to which it is desired to deliver the fluid. An outlet check valve 110 is situated within the outlet conduit 109 such that fluid flow is restricted to flowing from the displacement cavity 104 to the point 111 to which it is desired to deliver the fluid.
The shape memory alloy actuator is comprised of a shape memory allow material, such as a nickel-titanium alloy material, sometimes referred to as “nitinol.” The shape memory alloy material is sensitive to temperature or heat. For example, the material temporarily shrinks at a certain temperature, or shrinkage temperature, such as about 70° C. above ambient temperature for nitinol, and expands at a relatively lower temperature to return to its original condition. In response to being heated to the above-described shrinkage temperature, the shape memory alloy undergoes a dimensional change, such as a change in its length. In this way, a wire composed of a material such as nitinol, can undergo a change in length and a return toward its original length one or more times via temperature treatment or repeated temperature cycling. It is contemplated that a material that expands by going through a phase transition at a certain temperature and shrinks at a different temperature to return toward its original condition could be used.
In the process of undergoing a dimensional change, as described above, the shape alloy material goes through a reversible phase transition or transformation, or a reversible structural phase transition, upon a change in temperature. Generally, such a transition represents a change in the material from one solid phase of the material to another, for example, by virtue of a change in the crystal structure of the material or by virtue of a reordering of the material at a molecular level. In the case of nitinol, for example, the superelastic alloy has a low temperature phase, or martensitic phase, and a high temperature phase, or austenitic phase. These phases can also be referred to in terms of a stiff phase and a soft and malleable phase, or responsive phase. The particular phase transition associated with a particular alloy material may vary.
The shape memory alloy actuator is also comprised of the following elements. A movable member is referred to as a plunger 112 and is fixed by a rigid restraint 113 such that it is constrained to a periodic motion of precisely fixed limits. The plunger 112 is situated in relation to and/or attached to the displacement cavity 104 such that movement of the plunger 112 within the limits of its constrained motion will cause the volume of the displacement cavity 104 to be varied between its limits 105 , 106 . A biasing spring 115 is situated relative to the rigid restraint 113 and the plunger 112 such that at equilibrium, the biasing spring 115 exerts a force on the plunger 112 whose direction is that which would induce the displacement cavity 104 toward a state of minimum volume, i.e., toward its second limit 106 . A length of shape memory alloy wire 114 is connected at one end to the plunger 112 and at another end to the rigid substrate 101 . The shape memory alloy wire 114 is situated such that its dimensional change will give rise to motion of the plunger 112 . The shape memory alloy wire 114 and the biasing spring 115 are both of sufficient dimension such that when the shape memory alloy wire 114 is heated so as to induce phase transition and associated dimensional change, the wire will move the plunger 112 against the force of the biasing spring 115 “in one generally uninterrupted motion” to its second limit 105 so as to create a state of maximum volume within the displacement cavity 104 , whereas when the shape memory alloy is allowed to cool to ambient temperature, the force imparted by the biasing spring 115 will stretch the shape memory alloy wire 114 until the point where the displacement cavity 104 is in a state of minimum volume.
The programmable pulse generating circuit is comprised of a source of electric power 116 , an electrical connection 117 from the source of electric power 116 to each end of the shape memory alloy wire 114 and a programmable pulse generating circuit 118 situated along the electrical connection 117 such that pulses of electricity from the electric power source 116 may be applied to the shape memory alloy wire 114 automatically in a preset regular periodic manner.
Operation of the device proceeds in a cyclic manner. For purposes of description the beginning of the cycle is defined as the following state. All void space within the fluid reservoir 102 , inlet 107 and outlet 109 conduit, inlet 108 and outlet 110 check valves and displacement cavity 104 are completely filled with the fluid 103 to be pumped. The shape memory alloy wire 114 is at ambient temperature and thus in a state of maximum length. Correspondingly, the position of the plunger 112 is such that the volume of the displacement chamber 104 is at its minimum value. The biasing spring 115 is in a compressed state such that it exerts a force on the plunger 112 consistent with a state of minimum volume of the displacement cavity 104 . Operation of the device involves first a heating of the shape memory alloy wire 114 to a temperature and for a period of time sufficient to induce phase transition and an associated dimensional change. Heating of the shape memory alloy wire 114 is accomplished by passing an electric current though it. The duration of the electric heating period is preset and is controlled by the timing and switching circuit 118 . The dimensional change of the shape memory alloy wire 114 will result in the movement of the plunger 112 against the opposing force of biasing spring 115 so as to vary the volume of the displacement chamber 104 toward its first limit 105 and a state of maximum volume. As the volume of the displacement cavity 104 is increased, fluid 103 is drawn into the displacement cavity 104 from the fluid reservoir 102 through the inlet conduit 107 and inlet check valve 108 . Fluid 103 is not drawn into the displacement cavity 104 through the outlet conduit 109 due to the one-way flow restriction of the outlet check valve 110 . After the preset duration, the current is then switched off by the timing and switching circuit 118 allowing the shape memory alloy wire 114 to cool below its phase transition temperature. Cooling proceeds via natural convection to the ambient environment. When the shape memory alloy wire 114 cools below its phase transition temperature, the force exerted by the biasing spring 115 stretches the shape memory alloy wire 114 to its original maximum length. This allows the movement of the plunger 112 so as to vary the volume of the displacement cavity 104 toward its second limit 106 and a state of minimum volume. As the volume of the displacement cavity 104 is decreased, fluid 103 is pushed out of the displacement cavity 104 through the outlet conduit 109 and outlet check valve 110 . Fluid 103 is not pushed out of the displacement cavity 104 through the inlet conduit 107 due to the one-way flow restriction of the inlet check valve 108 . Thus one complete heating and cooling cycle of the shape memory alloy wire 114 results in the delivery of a volume of fluid 103 from the fluid reservoir 102 to the end of the outlet conduit 111 . The volume of fluid delivered with each cycle is precisely equal to the difference between the maximum and minimum volumes of the displacement cavity 104 as determined by the precisely defined limits 105 , 106 . The overall rate of fluid delivery is controlled by varying the period of time between actuations of the shape memory alloy actuator 104 .
An Alternative General Embodiment of the Invention
A schematic representation of an alternative general embodiment of the invention is shown in FIG. 1B . The alternative general embodiment includes all of the same components and elements as the general embodiment shown in FIG. 1A with the following exceptions. In this embodiment of the invention, heating of the shape memory alloy material 114 so as to cause a phase transition associated shortening of its length results in a minimum volume condition for the displacement cavity 104 . This may be achieved, for example, through the use of a pivoting linkage assembly 119 connecting the biasing spring 115 to the plunger 112 .
Detailed Description of a Preferred Embodiment of the Invention
As stated previously, it is an intention of the present invention that it be sufficiently small and sufficiently inexpensive to be practically used as both a portable device and as a disposable device. For example, a device that can be comfortably worn on the skin as an adhesive patch and can be disposed of and replaced after 3 days of use. A preferred embodiment of the invention includes specific embodiments of the various elements and components of the general embodiment that are consistent with this intention.
A preferred embodiment of the invention is diagrammed schematically in FIGS. 2A , 2 B and 2 C and is comprised of all of the same elements and components of the general embodiment of the invention shown in FIGS. 1A and 1B with the following exceptions. In a preferred embodiment of the invention the displacement cavity is comprised of an elastomeric diaphragm pump head 201 . An enlarged view of the details of the diaphragm pump head 201 is shown by FIG. 2B with pump head 201 in a state of minimum volume and by FIG. 2C with pump head 201 in a state of maximum volume. The diaphragm pump head is comprised of an elastomeric diaphragm 202 set adjacent to a rigid substrate 203 and scaled about a perimeter of the elastomeric diaphragm 202 . The displacement cavity 204 is then comprised of the volume in between the adjacent surfaces of the rigid substrate 203 and the elastomeric diaphragm 202 within the sealed perimeter.
Separate inlet 205 and outlet 206 conduits within the rigid substrate 203 access the displacement volume of the elastomeric diaphragm pump head 201 with the inlet conduit 205 connecting the displacement cavity 204 with a fluid reservoir 207 and the outlet conduit 206 connecting the displacement cavity 204 to the point to which it is desired to deliver fluid 208 . An inlet check valve 209 and an outlet check valve 210 are situated within the inlet conduit 205 and outlet conduit 206 respectively, oriented such that the net direction of flow is from the fluid reservoir 207 to the point to which it is desired to deliver fluid 208 .
The plunger 211 is comprised of a cylindrical length of rigid dielectric material. The plunger 211 is situated within a cylindrical bore 212 of a rigid restraint 213 such that the axis of the plunger 211 is oriented normal to surface of the elastomeric diaphragm 202 . The flat head of the plunger 211 is functionally attached to the non-wetted surface of elastomeric diaphragm 202 opposite the displacement cavity 204 such that movement of the plunger 211 along a line of motion coincident with its axis will cause the concomitant variation in the volume of the displacement cavity 204 . The biasing spring 214 is situated within the cylindrical bore 212 of the rigid restraint 213 , coaxial with the plunger 211 . The relative positions and dimensions of the plunger 211 , the rigid restraint 213 and the biasing spring 214 are such that at equilibrium the biasing spring 214 exerts a force on the plunger 211 along a line coincident with its axis such that the displacement cavity 204 is in a state of minimum volume ( FIG. 2A ).
A straight length of shape memory alloy wire 215 is situated in a position coincident with the axis of the plunger 211 . One end of the shape memory alloy wire 215 is fixed to the rigid restraint 203 and electrically connected by connection 216 to the programmable pulse generating circuit 217 and the electric power source 218 . The other end of the shape memory alloy wire 215 along with an electrical connection 219 to that end is connected to the end of the plunger 211 . The shape memory alloy wire 215 and the biasing spring 214 are both of sufficient dimension such that when the shape memory alloy wire 215 is heated so as to induce phase transition and associated dimensional change, it will pull the plunger 211 against the force of the biasing spring 214 so as to create a state of maximum volume within the displacement cavity 204 , whereas when the shape memory alloy is allowed to cool to ambient temperature, the force imparted by biasing spring 214 will stretch the shape memory alloy wire 215 until the point where the displacement cavity 204 is in a state of minimum volume.
A preferred embodiment of an inlet and outlet check valve is shown in cross-section in FIG. 3 and is comprised of a molded one-piece elastomeric valve which can be press-fit into the inlet or outlet conduit. An important feature for a check valve appropriate for use in the present invention is that it possesses a low cracking pressure and provides a tight seal in the absence of any back pressure. A preferred embodiment of such a check valve is comprised of a thin-walled elastomeric dome 301 situated on top of a thick elastomeric flange 302 . The top of the dome has a small slit 303 cut through it that is normally closed. A fluid pressure gradient directed toward the concave side 304 of the dome will induce an expansion of the dome 301 forcing the slit 303 open so as to allow fluid to flow through the valve in this direction. A fluid pressure gradient directed toward the convex side 305 of the dome will induce a contraction of the dome 301 forcing the slit 303 shut so as to prohibit fluid to flow through the valve in this direction.
A preferred embodiment of a pulse generating circuit is shown in FIG. 4 and is comprised of a 200 milliamp-hour, lithium-manganese oxide primary battery 401 , a high capacitance, low-equivalent series resistance (ESR) electrochemical capacitor 402 , a programmable digital timing circuit 403 , and a low-resistance field effect transistor switch 404 . The shape memory alloy wire is indicated in FIG. 4 symbolically as a resistor 405 . The battery 401 and electrochemical capacitor 402 are electrically connected to each other in parallel and are connected to the shape memory alloy wire 405 through the transistor switch 404 . The programmable timing circuit 403 , also powered by the battery 401 , sends a gating signal to the transistor switch 404 , as programmed by the user in accordance with the user's pumping requirements. During the period of time for which the transistor switch 404 is open, the battery 401 will keep the electrochemical capacitor 402 at a state of full charge. During the period of time for which the transistor switch 404 is closed, power will be delivered to the shape memory alloy wire 405 , primarily from the electrochemical capacitor 402 rather than from the battery 401 , owing to the substantially lower ESR associated with the electrochemical capacitor 402 . As such, the battery 401 is substantially isolated from the high current draw associated with the low resistance of the shape memory alloy wire 405 and the useful life of the battery 401 is significantly extended.
A preferred embodiment of a fluid reservoir 207 appropriate for use with the present invention is one for which the volume of the fluid reservoir diminishes concomitantly as fluid is withdrawn such that it is not necessary to replace the volume of the withdrawn fluid with air or any other substance. A preferred embodiment of a fluid reservoir 207 might comprise a cylindrical bore fitted with a movable piston, for example, a syringe, or a balloon constructed of a resilient material.
Operation of the preferred embodiment of the invention proceeds in a manner analogous to that described for the most general embodiment. In addition to its simplicity, the preferred embodiment has the advantage of physically blocking any fluid flow from the fluid reservoir to the point to which it is desired to deliver the fluid when there is no power being supplied to the system. This provides additional protection against an overdose caused by fluid expanding or being siphoned through the check valves when the system is inactive.
Detailed Description of a Functional Model of the Invention
A functional model of a preferred embodiment of the invention has been constructed and its performance has been characterized. The functional model is similar in appearance to the preferred embodiment of the invention shown in FIGS. 2 , 3 and 4 and is described in more detail below. The fixed rigid components of the pump including the rigid restraint and the rigid substrate of the diaphragm pump head are each machined from a monolithic block of acetal. Inlet and outlet conduits are additionally machined out of the same block. Check valves are commercially available one-piece elastomeric valves (for example, Check Valve, Part # VA4914, available from Vernay Laboratories Inc. of Yellow Springs, Ohio). A length of shape memory alloy actuator is 40 mm long and 125 μm in diameter (for example, Shape Memory Alloy Wire, Flexinol 125 LT, available from Mondo-tronics, Inc. of San Rafael, Calif.). Electrical connections to the ends of the shape memory alloy actuator are made with 30 AWG copper wire. The copper wire is twisted to the shape memory alloy wire to effect a good electrical connection. A plunger is machined out of acetal and has an overall length of 10.0 mm and a shaft diameter of 3.2 mm. An elastomer diaphragm is comprised of 0.025 mm thick silicon rubber film (for example, Silicon Rubber Film, Cat. #86435K31, available from McMaster Carr, of Los Angeles, Calif.). The flat head of the plunger is secured to the elastomer diaphragm with epoxy (for example, Epoxy, Stock #14250, available from ITW Devcon, of Danvers, Mass.). The ends of the shape memory alloy wire-copper conductor assembly are connected to the plunger and to the rigid restraint with epoxy. A stainless steel biasing spring has an overall length of 12.7 mm, an outside diameter of 3.0 mm, a wire diameter of 0.35 mm and a spring constant of 0.9 N/mm (for example, Biasing Spring, Cat. # C0120-014-0500, available from Associated Spring, of Dallas, Tex.).
A pulse generating circuit is comprised of an adjustable analog timing circuit based on a 556 dual timing integrated circuit (for example, 556 Dual Timing Circuit, Part # TS3V556, available from ST Microelectronics, of San Jose, Calif.). Power is supplied by a 3 V lithium-manganese dioxide primary cell (for example, Li/MgO 2 Battery, Part # DL2032, available from Duracell, of Bethel, Conn.). Power load leveling is facilitated by the use of an electrochemical supercapacitor (for example, Electrochemical Supercapacitor, Part # B0810, available from PowerStor Inc., of Dublin, Calif.) in parallel with the battery. High-power switching is achieved with a field effect transistor (for example, Field Effect Transistor Switch, Part # IRLZ24N, available from International Rectifier, of El Segundo, Calif.).
The functional model was characterized with respect to reproducibility, insulin stability and energy consumption. The model was operated by heating the shape memory alloy wire with a short pulse of current and then allowing the shape memory alloy wire to cool. Each heating pulse and subsequent cooling period comprised a single actuation cycle.
A device that is used to automatically deliver a drug to an individual over an extended period of time should do so with extreme precision. This is particularly critical when the drug being delivered is one that might have dangerous health consequences associated with an inappropriate dose. Insulin is one such drug. An excessive dose of insulin can result in dangerously low blood glucose level, which in turn can lead to coma and death. Thus any device to be used for automatically delivering insulin to a diabetic person must be able to demonstrate a very high level of precision. To characterize the precision with which the invention can deliver insulin, the functional model was repeatedly cycled at a constant period of actuation and the total quantity of liquid delivered was measured as a function of the number of actuation cycles. FIG. 5 shows typical results. The data in FIG. 5 were obtained with an actuation period of 28 seconds and a pulse duration of 0.15 seconds. In FIG. 5 markers show actual data points and the line represents a least squares fit of the data points. Data were collected over 8500 cycles at which point the measurement was stopped. The fit to the data has a slope of 1.997 mg/cycle and a linear correlation coefficient of 0.999 indicating that the functional model delivered extremely consistent volumes of liquid with each actuation over the course of the measurement.
Another important requirement for any medical device that handles insulin is that the device does not damage the insulin. Insulin is a large and delicate biomolecule that can readily be damaged by the mechanical action (e.g., shear stress) of a pumping device. Three common modes of insulin destruction which result in a loss of bioactivity are aggregation, where individual insulin molecules bond together to form various polymer structures, degradation, where individual insulin molecules are broken apart, and denaturing, where individual molecules remain intact but lose their characteristic conformation. All three modes of insulin destruction are exacerbated by elevated temperatures. Thus, in the development of a practical insulin pumping device, preferably, it should be demonstrated that the device does not damage insulin. To characterize the insulin stability associated with the invention, a quantity of insulin (Insulin, Humalog U100, available from Eli Lilly, of Indianapolis, Ind.) was set up to recycle continuously through the functional model over the course of several days at 37° C. Samples of the insulin were collected each day for evaluation. This resulted in a series of pumped insulin samples with an increasing amount of pump stress. The insulin samples were then analyzed by reverse-phase high performance liquid chromatography. The chromatography indicated a 2% loss of insulin concentration after a single pass through the pump and a further loss of another 5% of the insulin concentration after 3 days of recycling.
It is desirable for a small and inexpensive insulin delivery device to be able to execute its maximum intended term of use with the energy from a single small inexpensive primary battery. Based on a 0.1 unit dose size and a maximum insulin consumption of 100 units per day for 3 days, a maximum term of use for the inventive device might be considered to be 3000 cycles. To characterize the energy consumption of the invention, the functional model was operated continuously for several days at an actuation period of 85 seconds while the voltage of a 200 milliamp-hour, 2032 lithium/manganese dioxide battery was monitored. FIG. 6 shows typical results. A typical voltage vs. capacity curve for the lithium/manganese dioxide battery is characterized by an initial drop in voltage from about 3.2 V to a plateau voltage of about 2.8 V. The voltage of the battery remains at this plateau level for the duration of its useful life. The battery voltage will then drop precipitously to a value below 2 V when its capacity expires. The data in FIG. 6 indicate that the battery is still at its plateau voltage after 4000 pump cycles and thus the 200 milliamp-hour, lithium/manganese dioxide battery is more than adequate to power the device of the present invention for its intended term of use.
Alternative Embodiments of the Invention
A first alternative embodiment of the invention is diagrammed schematically in FIG. 7 and is comprised of all of the same subcomponents and elements of the most general embodiment of the invention shown in FIG. 1 with the following exceptions. In a first alternative embodiment of the invention, the displacement cavity, as well as the inlet and outlet conduit, are all comprised of a single length of small-diameter flexible and resilient tubing 701 . The tubing 701 is situated within a restraining fixture 702 secured to a rigid base 703 so as to fix the position and orientation of the tubing 701 relative to the other elements of the device. Inlet 704 and outlet 705 check valves are located within the bore of the tubing 701 such that they have a common orientation for flow direction and such that a length of empty tubing 701 exists in between the two check valves 704 , 705 . The volume within the inner diameter of the tubing 701 and in between the two check valves 704 , 705 comprises a displacement cavity 706 . The volume of the displacement cavity 706 is varied by compressing the resilient tubing 701 with a plunger 707 (described below) at a position midway between the two check valves 704 , 705 . The volume within the inner diameter of the tubing 701 and in between the two check valves 704 , 705 when the tubing 701 is uncompressed defines the maximum volume of displacement cavity 706 . The volume within the inner diameter of the tubing 701 and in between the two check valves 703 , 704 when the tubing 701 is fully compressed by the plunger 707 defines the minimum volume of the displacement cavity 705 .
The plunger 707 is comprised of a cylindrical length of rigid dielectric material and includes a flange 708 and a tapered end 709 . The plunger 707 is situated within a cylindrical bore 710 of a rigid restraint 711 such that the axis of the plunger 707 is oriented normal to the axis of the resilient tubing 701 and such that the tapered head 709 of the plunger 707 may be alternately pressed against the resilient tubing 701 and removed from contact with the resilient tubing 701 with movement of the plunger 707 along a line of motion coincident with the its axis. A biasing spring 712 is fitted around the shaft of the plunger 707 in between the rigid restraint 711 and the plunger flange 708 . The relative positions and dimensions of the plunger 707 , the rigid restraint 711 and the biasing spring 712 are such that at equilibrium the biasing spring 712 exerts a force on the plunger 707 along a line coincident with its axis that is sufficient to fully collapse the resilient tubing 701 and thus create a state of minimum volume of the displacement cavity 706 .
A straight length of shape memory alloy wire 713 is situated in a position coincident with the axis of the plunger 707 . One end of the shape memory alloy wire 713 is attached to the rigid base 703 and electrically connected by connection 716 to the pulse generating circuit 714 and the electric power source 715 . The other end of the shape memory alloy wire 713 along with an electrical connection 717 to that end is attached to the shaft of the plunger 707 . The shape memory alloy wire 713 is of sufficient length and strength that when heated so as to induce phase transition and associated dimensional change it will pull the plunger 707 away from contact with the resilient tubing 701 against the opposing force of the biasing spring 713 .
A second alternative embodiment of the invention is diagrammed schematically in FIG. 8 and is comprised of all of the same subcomponents and elements of the most general embodiment of the invention shown in FIG. 1 with the following exceptions. A displacement cavity 801 is comprised of a cylindrical shell 802 and tube 803 arrangement where the tube 803 is coaxial with the shell 802 and can move freely within the shell 802 along a line coincident with that axis. The volume of the displacement cavity 801 is varied by moving the tube 803 relative to the shell 802 . Movement of the tube 803 into the shell 802 reduces the volume of the displacement cavity 801 whereas movement of the tube out of the shell increases the volume of the displacement cavity 801 . A dynamic seal 804 , for example and elastomer o-ring, seals the displacement cavity 801 while not interfering adversely with the relative motion of the shell 802 and tube 803 . Outlet 805 and inlet 806 conduits access the displacement cavity 801 through the ends of the shell 802 and tube 803 respectively. Outlet 807 and inlet 808 check valves are situated within the shell 802 and tube 803 respectively. A biasing spring 809 is situated within the displacement cavity 801 so as to resist the motion of the displacement cavity 801 toward a state of reduced volume. A shape memory alloy wire 810 is attached between the shell 802 and the tube 803 along the outside of the assembly such that when the shape memory alloy wire 810 is heated so as to induce phase transition and associated dimensional change it will incline the displacement cavity 801 toward a state of reduced volume. The shape memory alloy wire 810 is electrically connected by connector 811 to a programmable pulse generating circuit 812 and a source of electric power 813 . Hard stops (not shown) on the limits of the relative positions of the shell 802 and tube 803 define the maximum and minimum volumes of the displacement volume 801 .
Operation of both the first and second alternative embodiments of the invention proceed in a manner analogous to that described for the most general embodiment and preferred embodiment of the invention.
In all of the embodiments described above, a shape memory alloy wire acts as an actuator to drive a movable member to increase or decrease the fluid volume in the pump head, and once the wire cools a spring is used to return the movable member back to its original position. Those of reasonable skill in this field will appreciate that a multitude of other biasing means exist, one or more of which can be used in place of or in addition to the spring. In fact, a shape memory alloy can be constructed in such a way that it drives the movable member in both directions to act as both an actuator and a return biasing element. For example, the shape memory alloy can be coiled much like a spring to drive the movable member in one direction when heated and in the other direction when cooled.
A first alternative embodiment of a pulse generating circuit is diagrammed schematically in FIG. 9 and is comprised of a 200 milliamp-hour lithium-manganese dioxide primary battery 901 , a DC to DC converter 902 , a capacitor 903 , a low-resistance field effect transistor switch 904 , a programmable digital timing circuit 905 , an inductor 906 and a diode 908 . The shape memory alloy wire is indicated in FIG. 9 symbolically as a resistor 907 . The objective of this embodiment of a pulse generating circuit is that the pulses of power delivered to the shape memory alloy wire 907 can be of a higher voltage, and thus higher current, than that associated with the preferred embodiment of a pulse generating circuit diagrammed in FIG. 4 and described previously. A high voltage, high current power pulse has the advantage that it can actuate the circuit in a shorter more efficient time period. Additionally, the alternative embodiment of a pulse generating circuit allows the useful life of the battery 901 to be extended to a lower voltage and can prevent other circuitry powered by the battery from resetting when the battery voltage droops as is likely to happen in the preferred embodiment. The battery 901 and capacitor 903 are electrically connected to each other in parallel through the DC to DC converter 902 . The capacitor 903 is further connected to the shape memory alloy wire 907 through the transistor switch 904 . The programmable timing circuit 905 , also powered by the battery 901 sends a gating signal to the transistor switch 904 as programmed by the user in accordance with their pumping requirements. During the period for which the transistor switch 904 is open, the DC to DC converter 902 draws energy from the battery 901 and stores it in the capacitor 903 . Use of the DC to DC converter 902 allows the voltage of the capacitor 903 to be charged to a significantly higher value than that associated with the battery 901 and to be charged to the same voltage throughout the life of the battery 901 regardless of the battery voltage. It is intended that the transistor switch 904 may be modulated to send an overall energy pulse as a single pulse or as a sequence of discrete smaller pulses. It is intended that these smaller pulses may be sequenced so as to tailor a custom profile for the overall energy pulse. The custom profile would ensure optimal energy delivery to the shape memory alloy without exceeding its fusing characteristics. The inclusion of the inductor 906 and diode 908 allows current to continue to flow through the shape memory alloy wire 907 after the transistor switch 904 is opened when the pulse is modulated. This allows further control of the energy delivered to the shape memory alloy.
Various references, publications, provisional and non-provisional United States patent applications, and/or United States patents, have been identified herein, each of which is incorporated herein in its entirety by this reference. Various aspects and features of the present invention have been explained or described in relation to beliefs or theories or underlying assumptions, although it will be understood that the invention is not bound to any particular belief or theory or underlying assumption. Various modifications, processes, as well as numerous structures to which the present invention may be applicable will be readily apparent to those of skill in the art to which the present invention is directed, upon review of the specification. Although the various aspects and features of the present invention have been described with respect to various embodiments and specific examples herein, it will be understood that the invention is entitled to protection within the full scope of the appended claims.
|
A system for the metering and delivery of small discrete volumes of liquid is comprised of a small or minimal number of inexpensive components. One such component is a movable member, such as a miniature precision reciprocating displacement pump head, which is driven by an actuator that comprises a shape memory alloy material. The operating mechanism of the system is of little or minimal complexity. The system facilitates the precise metering and delivery of the small discrete volumes of liquid. Potential applications for the system include subcutaneous, long-term, automated drug delivery, for example, the delivery of insulin to a person with diabetes. In such an application, the small, simple and inexpensive nature of the invention would allow for its use as both a portable and a disposable system.
| 0
|
FIELD OF THE INVENTION
[0001] This invention relates to Group 8 transition metal catalysts and method for making same and process for use of same in metathesis reaction.
BACKGROUND OF THE INVENTION
[0002] Olefin metathesis is a catalytic process including, as a key step, a reaction between a first olefin and a first transition metal alkylidene complex, thus producing an unstable intermediate metallocyclobutane ring which then undergoes transformation into a second olefin and a second transition metal alkylidene complex according to equation (1) hereunder. Reactions of this kind are reversible and in competition with one another, so the overall result heavily depends on their respective rates and, when formation of volatile or insoluble products occurs, displacement of equilibrium.
[0000]
[0003] Metathesis reactions are extensively applied in the field of chemical reactions, e.g. Ring closing metathesis (RCM), Cross metathesis (CM), Ring opening metathesis (ROM), Ring opening metathesis polymerization (ROMP), acyclic diene metathesis (ADMET), self-metathesis, conversion of olefins with alkynes (enyne metathesis), polymerization of alkynes, and so on.
[0000]
[0004] Typical applications of olefin metathesis but not limited are Reaction Injection Molding (RIM), filament winding, pultrusion of dicyclopentadiene (DCPD), which is an example of the ring opening metathesis polymerization. Industrial application in DCPD polymerization requires latent catalysts, which can allow for longer handling of a monomer-catalyst mixture before the polymerization starts. Other examples of ring opening metathesis polymerization are ROMP of norbornene and its derivatives, copolymerization of different cyclic olefins. Ethenolysis, a chemical process in which internal olefins are degraded using ethylene as the reagent, is an example of cross metathesis; CM of ethene with 2-butene; depolymerization of unsaturated polymers and so fort.
[0005] Although homo-coupling (equation 3a) is of high interest, the same is true for cross-coupling between two different terminal olefins (equation 3b). Coupling reactions involving dienes lead to linear and cyclic dimers, oligomers, and, ultimately, linear or cyclic polymers (equation 6). In general, the latter reaction is favoured in highly concentrated solutions or in bulk, while cyclisation is favoured at low concentrations. When intra-molecular coupling of a diene occurs so as to produce a cyclic alkene, the process is called ring-closing metathesis (equation 2). Cyclic olefins can be opened and oligomerised or polymerised (ring opening metathesis polymerisation shown in equation 5). When the alkylidene catalyst reacts more rapidly with the cyclic olefin (e.g. a norbornene or a cyclobutene) than with a carbon-carbon double bond in the growing polymer chain, then a “living ring opening metathesis polymerisation” may result, i.e. there is little termination during or after the polymerization reaction. Strained rings may be opened using an alkylidene catalyst with a second alkene following the mechanisms of the Cross Metathesis. The driving force is the relief of ring strain. As the products contain terminal vinyl groups, further reactions of the Cross Metathesis variety may occur. Therefore, the reaction conditions (time, concentrations, . . . ) must be optimized to favour the desired product (equation 4). The enyne metathesis is a metalcarbene-catalysed bond reorganization reaction between alkynes and alkenes to produce 1,3-dienes. The intermolecular process is called Cross-Enyne Metathesis (7), whereas intramolecular reactions are referred as Ring-Closing Enyne Metathesis (RCEYM).
[0006] The cross-metathesis of two reactant olefins, where each reactant olefin comprises at least one unsaturation site, to produce new olefins, which are different from the reactant olefins, is of significant commercial importance. One or more catalytic metals, usually one or more transition metals, usually catalyse the cross-metathesis reaction.
[0007] One such commercially significant application is the cross-metathesis of ethylene and internal olefins to produce alpha-olefins, which is generally referred to as ethenolysis. More specific, the cross-metathesis of ethylene and an internal olefin to produce linear α-olefins is of particular commercial importance. Linear α-olefins are useful as monomers or co-monomers in certain (co)polymers poly α-olefins and/or as intermediates in the production of epoxides, amines, oxo alcohols, synthetic lubricants, synthetic fatty acids and alkylated aromatics. Olefins Conversion Technology™, based upon the Phillips Triolefin Process, is an example of an ethenolysis reaction converting ethylene and 2-butene into propylene. These processes apply heterogeneous catalysts based on tungsten and rheniumoxides, which have not proven effective for internal olefins containing functional groups such as cis-methyl oleate, a fatty acid methyl ester.
[0008] 1-Decene is a co-product typically produced in the cross-metathesis of ethylene and methyl oleate. Alkyl oleates are fatty acid esters that can be major components in biodiesel produced by the transesterification of alcohol and vegetable oils. Vegetable oils containing at least one site of unsaturation include canola, soybean, palm, peanut, mustard, sunflower, tung, tall, perilla, grapeseed, rapeseed, linseed, safflower, pumpkin, corn and many other oils extracted from plant seeds. Alkyl erucates similarly are fatty acid esters that can be major components in biodiesel. Useful biodiesel compositions are those, which typically have high concentrations of oleate and erucate esters. These fatty acid esters preferably have one site of unsaturation such that cross-metathesis with ethylene yields 1-decene as a co-product.
[0009] Vegetables oils used in food preparation (fritting of meat, vegetables, . . . ) can be recuperated and after purification, be converted applying e.g. ethenolysis into useful products applicable in biodiesel.
[0010] Biodiesel is a fuel prepared from renewable sources, such as plant oils or animal fats. To produce biodiesel, triacylglycerides, the major compound in plant oils and animal fats, are converted to fatty acid alkyl esters (i.e., biodiesel) and glycerol via reaction with an alcohol in the presence of a base, acid, or enzyme catalyst. Biodiesel fuel can be used in diesel engines, either alone or in a blend with petroleum-based diesel, or can be further modified to produce other chemical products.
[0011] Several metal-carbene complexes are known for olefin metathesis however the difference between those structures can be found in the carbene part. Patents WO-A-96/04289 and WO-A-97/06185 are examples of metathesis catalysts having the general structure
[0000]
[0012] Where:
[0013] M is Os or Ru, R and R 1 organic parts from the carbene fragment which have a great structural variability, X and X 1 are anionic ligands and L and L 1 represents neutral electron donors. “Anionic ligands” are, according the literature in the field of olefin metathesis catalysts, ligands which are negative charged and thus bearing a full electron shell when they are removed from the metal center
[0014] A well-known example of this class of compounds is the Grubbs 1 st generation catalysts
[0000]
[0015] Another well-known example of this class of compounds is the Grubbs' 2 nd generation catalyst which is described in WO-A-0071554 and the hexa-coordinated “Grubbs 3 rd generation catalyst described in WO-A03/011455.
[0000]
[0016] There are still some other well-known catalysts described in literature which are very useful in the area of olefin metathesis, and which serve as background information for this application.
[0017] Furthermore, other catalysts are known where both carbon atoms of the carbene fragment are bridged; a few of these representatives are given:
[0000]
[0018] The bridged carbene fragment was firstly synthesized by Hill et al. (K. J. Harlow, A. F. Hill, J. D. E. T. Wilton-Ety, J. Chem. Soc. Dalton Trans. 1999, 285-291), however the structure was wrongly interpreted. Fürstner et al. corrected this misinterpretation (J. Org. Chem. 1999, 64, 8275-8280) and a full characterization was described. It followed that reorganization takes place whereby the carbon atoms of the carbene fragment are bridged and generating in this specific case a “3-phenyl-indenylidene carbene” (Chem. Eur. J. 2001, 7, No 22, 4811-4820). Analogues of this catalyst bearing one NHC-ligand and one phosphine ligand where described by Nolan in WO-A-00/15339. These types of compounds are not only catalysts for the olefin metathesis; they also can be used as starting product to produce other ruthenium-carbene compounds via cross metathesis (WO-A-2004/112951).
[0019] Furthermore, in US-A-2003/0100776 on page 8, paragraph [0087] are catalysts described where the carbon atoms of the carbene part are bridged and whereby the newly formed cyclic group can be aliphatic or aromatic and can bear substituents or hetero atoms. Additionally, it is said that the generated ring structure is constructed of 4 to 12 and preferable 5 to 8 atoms contains. However, no explicit ring structures or examples are described or given.
[0020] For some processes it is desirable that catalyst initiation be controllable. Much less work has focused on decreasing the initiation rate of ruthenium-based catalysts. In these cases, the use of a trigger such as light activation (e.g. photoirradiation), chemical activation (e.g. acid addition), temperature activation (e.g. heating of the sample) or mechanical activation (e.g. ultrason) can help to control initiation. Efficient ring-opening metathesis polymerization (ROMP) reactions require adequate mixing of monomer and catalyst before polymerization occurs. For these applications, catalysts that initiate polymerization at a high rate only upon activation are desirable. However, both Grubbs 2 nd gen and Hoveyda 2 nd gen. are competent metathesis catalysts at or below room temperature, so alone are not suited for applications where catalyst latency is beneficial ( Org. Lett. 1999, 1, 953-956; J. Am. Chem. Soc. 2000, 122, 8168-8179 ; Tetrahedron Lett. 2000, 41, 9973-9976).
[0021] Experimental studies have shown that, for the majority of ruthenium catalysts, dissociation of a donor ligand provides entry to the catalytic cycle. Several design strategies for slowing ligand dissociation can be envisioned. An important consideration is that the method used to slow initiation should not disrupt the catalyst activity. The addition of excess phosphine to the reaction can serve to slow initiation as shown in case I (Scheme 1)( J. Am. Chem. Soc. 1997, 119, 3887-3897). Unfortunately the addition of phosphine commonly results in propagation rates also being reduced.
[0000]
[0022] Another strategy to slow catalyst initiation is to replace the Schrock-type ruthenium carbene with a Fischer carbene (Type II, Scheme 1). This approach has been used to generate several latent metathesis catalysts with Fischer carbenes featuring oxygen, sulphur, and nitrogen substitution. ( Organometallics 2002, 21, 2153-2164; J. Organomet. Chem. 2000, 606, 65-74). In some cases, the decrease in activity with these systems is so great that they are considered metathesis-inactive. In fact, addition of ethyl vinyl ether to form a Fischer carbene complex is a standard method of quenching ROMP reactions.
[0023] Van der Schaaf and co-workers followed another approach (type IV, scheme 1) to develop the temperature activated, slow initiating olefin metathesis catalyst (PR 3 )(CI) 2 Ru(CH(CH 2 ) 2 —C,N-2-C 5 H 4 N) (1 in Scheme 2) in which initiation temperatures were tuned by changing the substitution pattern of the pyridine ring (J. Organomet. Chem. 2000, 606, 65-74). Unfortunately, activities of the reported complexes were undesirably low; restricted to 12000 equiv DCPD. Later, Ung reported on analogous tunable catalytic systems obtained by partially isomerizing trans-(SIMes)(CI) 2 Ru(CH(CH 2 ) 2 —C,N-2-C 5 H 4 N) (2 in scheme 2) into the cis analogue (Organometallics 2004, 23, 5399-5401). However, none of these catalysts allowed for storage in DCPD monomer for long time as the ROMP of DCPD is completed in 25 minutes after catalyst introduction.
[0000]
[0024] In another methodology towards rationally designed thermally stable olefin metathesis catalyst for DCPD polymerization, efforts were directed towards the development of an O,N-bidentate Schiff base ligated Ru-carbene catalysts elaborated by Grubbs (U.S. Pat. No. 5,977,393; Scheme 3, 4 wherein L=PR 3 ) and Verpoort (WO 03/062253; Scheme 3, 4 wherein L=SIMes and 5 wherein L=PR 3 , SIMes). It was shown that such complexes are extremely inactive at room temperature towards the polymerization of low-strain, cyclic olefins, allow for storage in DCPD for months and can be thermally activated to yield increased activity for the bulk-polymerization of DCPD, but from industrial point of view, catalysts of which their performance is easy tunable by a simple straightforward modification are not described (EP1468004; J. Mol. Cat. A: Chem. 2006, 260, 221-226).
[0000]
[0025] Recently a series of latent olefin metathesis catalysts bearing bidentate K 2 —(O,O) ligands were synthesized (Scheme 3, 3). Complex 3, proved to be inactive for the solvent-free polymerization of DCPD. It was furthermore illustrated that complex 3 (Scheme 3, L=PCy 3 , SIMes) is readily activated upon irradiation of a catalyst/monomer mixture containing a photoacid generator and was found applicable in ROMP of DCPD (WO 99/22865). Nevertheless irradiation of a solution of DCPD and 3 (L=SlMes) in a minimal amount of CH 2 CI 2 resulted in complete gelation within 1 h but solidified and cross-linked monomer was not obtained.
[0026] This indicates low catalyst activity and the operation on a low amount of the active species. Summarizing, the latent catalysts are of prominent importance for Ring-Opening Metathesis Polymerizations of low-strained cyclic olefins, as they allow for mixing of monomer and catalyst without concomitant gelation or microencapsulation of the precatalyst.
[0027] All the above-described catalysts bearing an indenylidene carbene part are based on a non-chelating phenyl-indenylidene structure without any substituents or functional groups. Catalysts with a chelating phenyl-indenylidene structure have been described in PCT/US2010/059703 (WO 2011/100022 A2) an indenylidene based catalyst is described whereby one phosphine ligand is substituted by a neutral donor ligand which is linked to the indenylidene carbene. The resulting catalyst is a 3-phenylindenylidene Hoveyda analogue catalyst.
[0028] In PCT/US2011/029690 (WO 2011/119778 A2) a hexa-coordinated catalyst is claimed, however in this document no catalysts were isolated; a synthetic method for the in-situ generation of olefin metathesis catalysts is disclosed since according to Schrödi the synthesis of these complexes is relatively cumbersome. The synthesis usually involves more than one step and requires isolation of the catalysts to remove catalyst-inhibiting byproducts such as liberated phosphines. The resulting in-situ generated catalysts are all phenylindenylidene Hoveyda analogue catalysts.
[0029] Other non-chelating indenylidene catalysts bearing functional groups or substituents on the indenylidene part, different from phenylindenylidene, are until now not known.
[0000]
[0030] In WO 2011/009721 A1 bis-Schiff base catalysts are described on page 18-20 “via route B” starting from 5 with L=SIMes wherein it is said that the reaction mixture was investigated with 1 H and 31 P NMR revealing a quantitative transformation to the desired bis-Schiff Base catalyst. However, none of those compounds contain any P-ligand. Furthermore, the catalysts prepared via “route A” were investigated with 1 H and 31 P NMR revealing a quantitative transformation to the desired bis-Schiff Base catalyst, though, no values are given.
[0031] Moreover, it is said that the bis-Schiff base catalyst (catalyst 4 on page 22) has an extreme latent character even at 200° C. (catalyst 4/DCPD ratio: 1/15000) as was proven with DSC. However, it is well-know that DCPD when heated above 150° C., undergoes a retro-Diels-Alder reaction to yield cyclopentadiene and the boiling point is 170° C.
[0032] Additionally, it is said in the “summary of the invention” page 4 that the catalysts are obtained by a simple, efficient, green and highly yielding synthetic process. However, the catalysts procedure for the catalysts synthesis is 72 h (without purification steps) which can not be called “efficient” or industrial attractive. Besides of all the synthesized catalysts no yield is mentioned.
[0033] The ruthenium carbene part (indenylidene) in WO 2011/009721 A1 is defined as in WO 00/15339. The most preferably carbene part is a phenylindenylidene ligand. Yet, no substituted phenylindenylidene ligands are claimed.
[0034] Despite the advances achieved in the preparation and development of olefin metathesis catalysts, a continuing need exists for new improved synthetic methods and new catalysts. Of particular interest are methods that provide the preparation of new catalysts, which easily can be prepared on industrial scale.
[0035] Notwithstanding the different available catalysts, from industrial point of view, catalysts of which their performance is easy tunable by a simple straightforward modification are highly desired. Of particular interest are catalysts which can be modified from completely latent to highly active; latent catalysts find easily application in ROMP e.g. DCPD polymerization via RIM, highly active catalysts find easily application in cross metathesis e.g. ethenolysis.
[0036] Moreover, easy tunable catalysts can be obtained by tuning of the electron density of the catalyst by variation of the alkylidene (e.g. indenylidene) in combination with ligands (e.g. ditopic or multitopic ligands). However, the combination of non-chelating substituted/functionalised indenylidene with ditopic or multitopic ligands is still not existing and offers extra advantage in terms of initiation tunability which results in catalysts which can be varied from real latent to highly active.
[0037] Additionally, the catalysts of present invention afford latent catalysts stable in the monomer and highly active after an industrially acceptable activation process, a property of which there is still a high demand.
[0038] Furthermore, the instant invention's metathesis catalyst compounds provide both a mild and commercially economical and an “atom-economical” route to desirable olefins, which in turn may be useful in the preparation of linear alpha-olefins, unsaturated polymers, cyclic olefins, etc. . . . .
[0039] Another important parameter for the evaluation of metathesis catalysts is the need for catalysts that can be separated from the final metathesis product easily. For applications of metathesis reactions in pharmaceutical industry, the ruthenium level in drugs must not exceed 5 ppm. (http://www.emea.europa.eu/pdfs/human/swp/444600en.pdf for EMEA regulations) Up to date, different protocols were reported to remove ruthenium from metathesis products to meet these criteria. The employed protocols include removal of ruthenium by oxidation reactions (H 2 O 2 , PPh 3 O, DMSO or Pb(OAc) 4 , water extraction, scavengers, supported phosphine ligands, or treatment with active charcoal combined with chromatography. These protocols only decreased the ruthenium concentration in the final product to 100-1200 ppm, which is far from the required criteria for pharmaceutical applications. The immobilization of catalysts (organic or inorganic support) gave promising results with moderate success for efficient removal of ruthenium. As another strategy, modification of the ligands by more polar groups or alternation of their steric hindrance to ease their separation from metathesis products was also reported. Grela successfully modified Hoveyda-Grubbs type catalysts with ionic-tagged ligands which exhibits a good affinity towards silica gel. (Green Chem., 2012, 14, 3264.) However, the synthesis of an ionic-tagged ligand is cumbersome. The catalysts of this invention, obtained via a straightforward synthesis procedure, show an extremely high affinity for silica especially catalysts bearing multitopic ligands making them extremely useful and attractive for pharmaceutical and fine chemical applications.
[0040] The synthesis of RuCl 2 (PCy 3 ) 2 (3-phenylindenylidene) has proven useful in providing an easy route to ruthenium alkylidenes which avoids costly diazo preparations (Platinum Metals Rev. 2005, 49, 33).
[0041] In order to obtain an economically viable process for linear α-olefins (e.g. 1-decene) production via the cross-metathesis of ethylene and biodiesel (such as animal or vegetable oils), higher activity catalysts or more stable catalysts must be developed. Moreover, there is still a need for the development of catalysts with equivalent or better performance characteristics but synthesized directly from less expensive and readily available starting materials.
[0042] As there is a continuous need in the art for improving catalyst efficiency, i.e. improving the yield of the reaction catalysed by the said catalyst component after a certain period of time under given conditions (e.g. temperature, pressure, solvent and reactant/catalyst ratio) or else, at a given reaction yield, providing milder conditions (lower temperature, pressure closer to atmospheric pressure, easier separation and purification of product from the reaction mixture) or requiring a smaller amount of catalyst (i.e. a higher reactant/catalyst ratio) and thus resulting in more economic and environment-friendly operating conditions. This need is still more stringent for use in reaction-injection molding (RIM) processes such as, but not limited to, the bulk polymerisation of endo- or exo-dicyclopentadiene, or formulations thereof.
[0043] There is also a specific need in the art, which is yet another goal of this invention, for improving reaction-injection molding (RIM) processes, resin transfer molding (RTM) processes and reactive rotational molding (RRM) processes such as, but not limited to, the bulk polymerisation of endo- or exo-dicyclopentadiene, or copolymerization thereof with other monomers, or formulations thereof. More specifically there is a need to improve such processes which are performed in the presence of multicoordinated transition metal complexes, in particular ruthenium complexes. All the above needs constitute the various goals to be achieved by the present invention; nevertheless other advantages of this invention will readily appear from the following description.
SUMMARY OF THE INVENTION
[0044] The present invention is directed to addressing one or more of the above-mentioned issues. The invention is based on the unexpected finding that improved metathesis of unsaturated compounds such as olefins and alkynes can be obtained by catalysts having a general structure of formula (I-II) and (VII) by modifying the alkylidene part of group 8 catalysts of the prior art in combination with a ditopic or multitopic ligand(s).
[0045] The present invention provides catalysts which can be easily and efficiently activated by a chemical activator (Brönsted and Lewis acids) or a photo-activator (Photo acid generator, PAG) showing exceptional activity after activation. The catalysts of present invention can also be activated by in-situ generation of a Brønsted acid by combining a Lewis acid, which at least contains one halogen atom, with any —OH or —SH containing molecule(s) (liquid or solid, organic or inorganic).
[0046] In a preferred embodiment of the invention, unsaturated carboxylic acids and/or esters of unsaturated carboxylic acids individually and/or mixtures of the unsaturated carboxylic acids or mixtures of esters of unsaturated carboxylic acids can be converted. The catalysts of this invention are preferably used in concentrations of less than or equal to 1000 ppm, in particular in the range from 1 to 1000 ppm, preferably 5 to 200 ppm. The inventive method can be carried out at temperatures between 0 to 100° C., preferably between 20 to 90° C., are carried out in particular between 40 to 80° C.
[0047] The method can be performed using conventional solvents, in which the reactant(s) and the catalyst are dissolved, e.g. hydrocarbons or alcohols. In a preferred embodiment of the invention the method may be carried out solventless.
[0048] Via this inventive method unsaturated α,ω dicarboxylic acids and unsaturated α,ω dicarboxylic acid diesters are obtained together with the corresponding unsaturated hydrocarbons. A separation of the mixture can be done, for example, by distillation, by fractionated crystallization or by extraction. These products produced by the inventive method unsaturated α,ω dicarboxylic acids and unsaturated α,ω dicarboxylic acid diester can be used in e.g. cosmetic preparations. If necessary, the products thus obtained can be subjected to hydrogenation.
[0049] The present invention is also based on the unexpected finding that the synthesis time of the organometallic compounds of formula (I-II) and (VII) can be reduced to 4 hours or less while maintaining high to excellent yields.
[0000]
[0050] The organometallic catalyst compounds of the present invention can be prepared by contacting a Group 8 metal precursor compound with at least one ditopic ligand which alternatively can bear at least an extra chelating moiety.
[0051] Wherein,
[0052] M is a Group 8 metal, preferably ruthenium or osmium;
[0053] R 1 -R 6 are identical or different and selected from H, hydrocarbyl, substituted hydrocarbyl, heteroatom containing hydrocarbyl, substituted heteroatom-containing hydrocarbyl, and functional groups, except that R 2 does not represent phenyl when R 1 ═R 3 ═R 4 ═R 5 ═R 6 ═H;
[0054] wherein alternatively in each case two directly adjacent radicals from the group of R 1 -R 6 , including the ring carbon atoms to which they are attached by a cyclic bridging group, generating one or more cyclic structures, including aromatic structures;
[0055] X 1 preferably represents an anionic ligand;
[0056] L 1 preferably represents a neutral electron donor;
[0057] L 1 and X 1 may be joined to form a multidentate monoanionic group and may form single ring of up to 30 non-hydrogen atoms or a multinuclear ring system of up to 30 non-hydrogen atoms;
[0058] A 1 -A 2 are identical or different and are selected from the group consisting of oxygen, sulphur, selenium, NR″″, PR″″, POR″″, AsR″″, AsOR″″, SbOR″″ and SbR″″;
[0059] T 1 -T 2 are identical or different and are selected from the group consisting of:
[0000]
[0060] wherein E preferably represents a donor atom selected from the group consisting of nitrogen, phosphor, oxygen, sulphur, and selenium; wherein for the group
[0000]
[0000] in case of oxygen, sulphur and selenium, R is omitted for double bonded E or R remains for a single bonded E; wherein for the group
[0000]
[0000] in case of oxygen, sulphur and selenium, the E-C bound is a single bond and the C atom contains an extra R group or the C—R′ is a double bond or the C—R is a double bond.
[0061] R, R′, R″, R′″ and R″″ are identical or different and selected from H, hydrocarbyl, substituted hydrocarbyl, heteroatom containing hydrocarbyl, substituted heteroatom-containing hydrocarbyl, and functional groups;
[0062] wherein alternatively in each case two directly adjacent radicals from the group of R, R′, R″, R′″ and R″″, including the carbon atoms to which they are attached, generating one or more cyclic structures, including aromatic structures.
[0063] C 1 -C 2 are carbon atoms linked to each other via a single or double bond wherein in case of a single bond each carbon atom bears an extra substituent R C1 and R C2 ; R C1 and R C2 are identical or different and are as defined for R′, R″, R′″ and R″″.
[0064] In an extra aspect, the invention provides a method for performing a catalytic metathesis reaction comprising contacting at least one olefin or olefinic compound with the metathesis catalyst of the invention. An olefin includes a single olefin, multi-olefin as well as a combination or mixture of two or more olefins, reference to “a substituent” encompasses a single substituent as well as two or more substituents, and the like.
[0065] In a further aspect the present invention is based on the unexpected finding that superior catalysts (I-II, VII) useful in the metathesis of unsaturated compounds such as olefins and alkynes, their activity can even be extra enhanced by bringing into contact a metal complex (I-II, VII) with an activating compound (hereinafter also referred as “activator”) selected from Brønsted acids (Brønsted acids are proton donors, which is the commonly accepted practice among chemists). The nature of the Brønsted acid can be liquid, solid, inorganic or organic. Well-know representative compounds of Brønsted acids, but not limited, are HCl, HBr, H 2 SO 4 , CH 3 COOH, sulphonic acid resins, etc.
[0066] In a further aspect the present invention is based on the unexpected finding that superior catalysts useful in the metathesis of unsaturated compounds such as olefins and alkynes can be obtained by bringing into contact a metal complex (I-II, VII) with an activating compound (hereinafter also referred as “activator”) selected from the group consisting of:
M a (I) halides. compounds represented by the formula M a X 2-y R a y (0≦y≦2).
[0069] wherein
[0070] R a is equal to R 1 -R 6 defined as herein-above,
[0071] X is atom of the halogen group and identical or different in case more then one halogen atom is present, and
[0072] M a is an atom having an atomic mass from 27 to 124 and being selected from the group consisting of groups IB, IIB, IIIA, IVB, IVA and VA of the Periodic Table of elements under conditions such that at least partial cleavage of a bond between the metal and the ditopic or multitopic ligand of said catalyst occurs.
compounds represented by the formula M a X 3-y R a y (0≦y≦3) wherein R a , X and M a defined as herein-above. compounds represented by the formula M a X 4-y R a y (0≦y≦4) wherein R a , X and M a defined as herein-above. compounds represented by the formula M a X 5-y R a y (0≦y≦5) wherein R a , X and M a defined as herein-above. compounds represented by the formula M a X 6-y R a y (0≦y≦6) wherein R a , X and M a defined as herein-above.
[0077] In yet another specific embodiment, the present invention is based on the unexpected finding that useful catalytic species can be suitably obtained by reacting an activator such as defined hereinabove, provided that said activator includes at least one halogen atom, in the presence of at least one further reactant having the formula RYH, wherein Y is selected from the group consisting of oxygen, sulphur and selenium, and R as defined hereinabove. According to this specific embodiment, a strong acid (such as a hydrogen halide) may be formed in situ by the reaction of said activator, with said further reactant having the formula RYH, and said strong acid if produced in sufficient amount may in turn be able:
in a first step, to protonate the ditopic (or multitopic) ligand and decoordinate T 1 (in case of structure (I)) or T 1 or T 2 or both (in case of structure (II)) of said ditopic (or multitopic) ligand from the complexed metal, and in a second step, to decoordinate the further heteroatom of said ditopic (or multitopic) ligand from the complexed metal.
[0080] In this specific embodiment, at least partial cleavage of a bond between the metal and the ditopic (or multitopic) ligand of said metal complex occurs like in the absence of the further reactant having the formula RYH, but coordination of T 1 or T 2 or both atoms of the ditopic (or multitopic) ligand to the activator occurs less frequently because it competes unfavourably with the protonation/decoordination mechanism resulting from the in situ generation of a strong acid (such as a hydrogen halide). This alternative mechanism is however quite effective in the catalysis of metathesis reactions of olefins and alkynes since it provides a more random distribution of the strong acid in the reaction mixture than if the same strong acid is introduced directly in the presence of catalyst (I-II,VII).
[0081] The new catalytic species of the invention may be produced extra-temporaneously, separated, purified and conditioned for separate use in organic synthesis reactions later on, or they may be produced in situ during the relevant chemical reaction (e.g. metathesis of unsaturated organic compounds) by introducing a suitable amount of the activator into the reaction mixture before, simultaneously with, or alternatively after the introduction of the starting catalyst compound. The present invention also provides catalytic systems including, in addition to said new catalytic species or reaction products, a carrier suitable for supporting said catalytic species or reaction products.
[0082] The present invention also provides methods and processes involving the use of such new catalytic species or reaction products, or any mixture of such species, or such catalytic systems, in a wide range of organic synthesis reactions including the metathesis of unsaturated compounds such as olefins and alkynes and In particular, this invention provides an improved process for the ring opening polymerization of strained cyclic olefins such as, but not limited to, dicyclopentadiene.
[0083] In the context of this invention, all the above and below mentioned, general or preferred ranges of definitions, parameters or elucidations among one another, or also between the respective ranges and preferred ranges can be combined in any manner.
[0084] In the context of this invention, related to the different types of metathesis catalysts, the term “substituted” means that a hydrogen atom or an atom is replaced by a specified group or an atom, and the valence of the atom indicated is not exceeded and the substitution leads to a stable compound.
BRIEF DESCRIPTION OF THE FIGURES
[0085] FIG. 1 is reaction progress after 1 h during the synthesis of catalyst 12.
[0086] FIG. 2 is reaction progress after 5 h during the synthesis of catalyst 12.
[0087] FIG. 3 is comparison between commercial catalyst N and 5A, 6A and 7A of this invention for the ring closing metathesis (RCM) of diethyldiallylmalonate (DEDAM) using activation.
[0088] FIG. 4 is comparison between catalyst F and 5A-7A at a 0.1 mol % loading for the RCM of DEDAM.
[0089] FIG. 5 is influence of activator amount on the catalytic performance for RCM of DEDAM.
[0090] FIG. 6 is ROMP of DCPD using catalyst 4A, 8A, 9A and 12 of this invention.
[0091] FIG. 7 is ROMP of DCPD using in-situ activation.
DETAILED DESCRIPTION
Terminology and Definitions
[0092] Unless otherwise mentioned, the invention is not limited to specific reactants, substituents, catalysts, reaction conditions, or the like, as such may vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting.
[0093] In this specification and in the claims that follow, reference will be made to a number of terms, which shall be defined to have the following meanings:
[0094] The term “alkyl” as used herein refers to a linear, branched, or cyclic saturated hydrocarbon group typically although not necessarily containing 1 to about 24 carbon atoms, preferably 1 to about 12 carbon atoms, such as methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, t-butyl, octyl, decyl, and the like, as well as cycloalkyl groups such as cyclopentyl, cyclohexyl and the like. Generally, although again not necessarily, alkyl groups herein contain 1 to about 12 carbon atoms. The term “C 1 -C 6 -alkyl” intends an alkyl group of 1 to 6 carbon atoms, and the specific term “cycloalkyl” intends a cyclic alkyl group, typically having 3 to 8 carbon atoms.
[0095] The term “substituted alkyl” refers to alkyl substituted with one or more substituent groups, and the terms “heteroatom-containing alkyl” and “heteroalkyl” refer to alkyl in which at least one carbon atom is replaced with a heteroatom. If not otherwise indicated, the term “alkyl” includes linear, branched, cyclic, unsubstituted, substituted, and/or heteroatom-containing alkyl.
[0096] The term “alkylene” as used herein refers to a difunctional linear, branched, or cyclic alkyl group, where “alkyl” is as defined above.
[0097] The term “alkenyl” as used herein refers to a linear, branched, or cyclic hydrocarbon group of 2 to about 24 carbon atoms containing at least one double bond, such as ethenyl, n-propenyl, isopropenyl, n-butenyl, isobutenyl, octenyl, decenyl, tetradecenyl, hexadecenyl, eicosenyl, and the like. Preferred alkenyl groups herein contain 2 to about 12 carbon atoms. The term “cycloalkenyl” intends a cyclic alkenyl group, preferably having 5 to 8 carbon atoms. The term “substituted alkenyl” refers to alkenyl substituted with one or more substituent groups, and the terms “heteroatom-containing alkenyl” and “heteroalkenyl” refer to alkenyl in which at least one carbon atom is replaced with a heteroatom. If not otherwise indicated, the term “alkenyl” include linear, branched, cyclic, unsubstituted, substituted, and/or heteroatom-containing alkenyl.
[0098] The term “alkenylene” as used herein refers to a difunctional linear, branched, or cyclic alkenyl group, where “alkenyl” is as defined above.
[0099] The term “alkynyl” as used herein refers to a linear or branched hydrocarbon group of 2 to about 24 carbon atoms containing at least one triple bond, such as ethynyl, n-propynyl, and the like. Preferred alkynyl groups herein contain 2 to about 12 carbon atoms. The term “substituted alkynyl” refers to alkynyl substituted with one or more substituent groups, and the terms “heteroatom-containing alkynyl” and “heteroalkynyl” refer to alkynyl in which at least one carbon atom is replaced with a heteroatom. If not otherwise indicated, the term “alkynyl” include linear, branched, unsubstituted, substituted, and/or heteroatom-containing alkynyl respectively.
[0100] The term “alkoxy” as used herein intends an alkyl group bound through a single, terminal ether linkage; that is, an “alkoxy” group may be represented as —O-alkyl where alkyl is as defined above. Analogously, “alkenyloxy” refers to an alkenyl group bound through a single, terminal ether linkage, and “alkynyloxy” refers to an alkynyl group bound through a single, terminal ether linkage.
[0101] The term “aryl” as used herein, and unless otherwise specified, refers to an aromatic substituent containing a single aromatic ring or multiple aromatic rings that are fused together, directly linked, or indirectly linked (such that the different aromatic rings are bound to a common group such as a methylene or ethylene moiety). Preferred aryl groups contain 5 to 24 carbon atoms, and particularly preferred aryl groups contain 5 to 14 carbon atoms. Exemplary aryl groups contain one aromatic ring or two fused or linked aromatic rings, e.g., phenyl, naphthyl, biphenyl, diphenylether, diphenylamine, benzophenone, and the like. “Substituted aryl” refers to an aryl moiety substituted with one or more substituent groups, and the terms “heteroatom-containing aryl” and “heteroaryl” refer to aryl substituents in which at least one carbon atom is replaced with a heteroatom, as will be described in further detail infra.
[0102] The term “aryloxy” as used herein refers to an aryl group bound through a single, terminal ether linkage, wherein “aryl” is as defined above. An “aryloxy” group may be represented as —O-aryl where aryl is as defined above. Preferred aryloxy groups contain 5 to 24 carbon atoms, and particularly preferred aryloxy groups contain 5 to 14 carbon atoms. Examples of aryloxy groups include, without limitation, phenoxy, o-halo-phenoxy, m-halo-phenoxy, p-halo-phenoxy, o-methoxyphenoxy, m-methoxy-phenoxy, p-methoxy-phenoxy, 2,4-dimethoxy-phenoxy, 3,4,5-trimethoxy-phenoxy, and the like.
[0103] The term “alkaryl” refers to an aryl group with an alkyl substituent, and the term “aralkyl” refers to an alkyl group with an aryl substituent, wherein “aryl” and “alkyl” are as defined above. Preferred alkaryl and aralkyl groups contain 6 to 24 carbon atoms. Alkaryl groups include, but not limit to, for example, p-methylphenyl, 2,4-dimethylphenyl, p-cyclohexylphenyl, 2,7-dimethylnaphthyl, 7-cyclooctylnaphthyl, 3-ethyl-cyclopenta-1,4-diene, and the like. Examples of aralkyl groups include, without limitation, benzyl, 2-phenyl-ethyl, 3-phenyl-propyl, 4-phenyl-butyl, 5-phenyl-pentyl, 4-phenylcyclohexyl, 4-benzylcyclohexyl, 4-phenylcyclohexylmethyl, 4-benzylcyclohexylmethyl, and the like. The terms “alkaryloxy” and “aralkyloxy” refer to substituents of the formula —OR wherein R is alkaryl or aralkyl, respectively, as just defined.
[0104] The term “acyl” refers to substituents having the formula —(CO)-alkyl, —(CO)-aryl, or —(CO)-aralkyl, and the term “acyloxy” refers to substituents having the formula —O(CO)-alkyl, —O(CO)aryl, or —O(CO)-aralkyl, wherein “alkyl,” “aryl, and “aralkyl” are as defined above.
[0105] The terms “cyclic” and “ring” refer to alicyclic or aromatic groups that may or may not be substituted and/or heteroatom containing, and that may be monocyclic, bicyclic, or polycyclic. The term “alicyclic” is used in the conventional sense to refer to an aliphatic cyclic moiety, as opposed to an aromatic cyclic moiety, and may be monocyclic, bicyclic, or polycyclic.
[0106] The terms “halo” and “halogen” are used in the conventional sense to refer to a chloro, bromo, fluoro, or iodo substituent.
[0107] “Hydrocarbyl” refers to univalent hydrocarbyl radicals containing 1 to about 30 carbon atoms, preferably 1 to about 24 carbon atoms, most preferably 1 to about 12 carbon atoms, including linear, branched, cyclic, saturated, and unsaturated species, such as alkyl groups, alkenyl groups, aryl groups, and the like. The term “hydrocarbylene” intends a divalent hydrocarbyl moiety containing 1 to about 30 carbon atoms, preferably 1 to about 24 carbon atoms, most preferably 1 to about 12 carbon atoms, including linear, branched, cyclic, saturated and unsaturated species. “Substituted hydrocarbyl” refers to hydrocarbyl substituted with one or more substituent groups, and the terms “heteroatom-containing hydrocarbyl” and “heterohydrocarbyl” refer to hydrocarbyl in which at least one carbon atom is replaced with a heteroatom. Similarly, “substituted hydrocarbylene” refers to hydrocarbylene substituted with one or more substituent groups, and the terms “heteroatom containing hydrocarbylene” and “heterohydrocarbylene” refer to hydrocarbylene in which at least one carbon atom is replaced with a heteroatom. Unless otherwise indicated, the term “hydrocarbyl” and “hydrocarbylene” are to be interpreted as including substituted and/or heteroatom-containing hydrocarbyl and hydrocarbylene moieties, respectively.
[0108] The term “heteroatom-containing” as in a “heteroatom-containing hydrocarbyl group” refers to a hydrocarbon molecule or a hydrocarbyl molecular fragment in which one or more carbon atoms is replaced with an atom other than carbon, e.g., nitrogen, oxygen, sulfur, phosphorus or silicon, typically nitrogen, oxygen or sulfur. Similarly, the term “heteroalkyl” refers to an alkyl substituent that is heteroatom-containing, the term “heterocyclic” refers to a cyclic substituent that is heteroatom-containing, the terms “heteroaryl” and “heteroaromatic” respectively refer to “aryl” and “aromatic” substituents that are heteroatom-containing, and the like. It should be noted that a “heterocyclic” group or compound may or may not be aromatic, and further that “heterocycles” may be monocyclic, bicyclic, or polycyclic as described above with respect to the term “aryl.” Examples of heteroalkyl groups include alkoxyalkyl, alkylsulfanyl-substituted alkyl, N-alkylated amino alkyl, and the like. Examples of heteroaryl substituents include pyrrolyl, pyrrolidinyl, pyridinyl, quinolinyl, indolyl, pyrimidinyl, imidazolyl, 1,2,4-triazolyl, 1,2,3 triazolyl, tetrazolyl, etc., and examples of heteroatom containing alicyclic groups are pyrrolidino, morpholino, piperazino, piperidino, etc.
[0109] By “substituted” as in “substituted hydrocarbyl,” “substituted alkyl,” “substituted aryl,” and the like, as alluded to in some of the aforementioned definitions, is meant that in the hydrocarbyl, alkyl, aryl, or other moiety, at least one hydrogen atom bound to a carbon (or other) atom is replaced with one or more non-hydrogen substituents. Examples of such substituents include, without limitation: functional groups such as halo, hydroxyl, sulfhydryl, C 1 -C 24 alkoxy, C 2 -C 24 alkenyloxy, C 2 -C 24 alkynyloxy, C 5 -C 24 aryloxy, C 6 -C 24 aralkyloxy, C 6 -C 24 alkaryloxy, acyl (including C 2 C 24 alkylcarbonyl (—CO-alkyl) and C 6 -C 24 arylcarbonyl (—CO-aryl)), acyloxy (—O-acyl, including C 2 C 24 alkylcarbonyloxy (—O—CO-alkyl) and C 6 -C 24 arylcarbonyloxy (—O—CO-aryl)), C 2 C 24 alkoxycarbonyl (—(CO)—O— alkyl), C 6 -C 24 aryloxycarbonyl (—(CO)—O-aryl), halocarbonyl (—CO)X where X is halo), C 2 -C 24 alkylcarbonato (—O—(CO)—O-alkyl), C 6 -C 24 arylcarbonato (—O—(CO)—O-aryl), carboxy (—COOH), carboxylato (—COO − ), carbamoyl (—(CO)—NH 2 ), mono-(C 1 -C 24 alkyl) substituted carbamoyl (—(CO)—NH(C 1 -C 24 alkyl)), di-(C 1 -C 24 alkyl)-substituted carbamoyl (—(CO)N(C 1 -C 24 alkyl) 2 ), mono-(C 5 -C 24 aryl)-substituted carbamoyl (—(CO)—NH-aryl), di-(C 5 -C 24 aryl) substituted carbamoyl (—(CO)—N(C 5 -C 24 aryl) 2 ), M(C 1 -C 24 alkyl) (C 5 -C 24 aryl))-substituted carbamoyl, thiocarbamoyl (—(CS)—NH 2 ), mono-(C 1 -C 24 alkyl)-substituted thiocarbamoyl (—(CS)NH(C 1 -C 24 alkyl)), di-(C 1 -C 24 alkyl)-substituted thiocarbamoyl (—(CS)—N(C 1 -C 24 alkyl) 2 ), mono-(C 5 -C 24 aryl)-substituted thiocarbamoyl (—(CS)—NH-aryl), di-(C 5 -C 24 aryl)-substituted thiocarbamoyl ((CS)—N(C 5 -C 24 aryl) 2 ), N—(C 1 -C 24 alkyl)N—(C 5 -C 24 aryl)-substituted thiocarbamoyl, carbamido (NH—(CO)—NH 2 ), cyano (—C═N), cyanato (—O—C═N), thiocyanato (—S—C═N), formyl (—(CO)—H), thioformyl (—(CS)—H), amino (—NH 2 ), mono-(C 1 -C 24 alkyl)-substituted amino, di-(C 1 -C 24 alkyl) substituted amino, mono-(C 5 -C 24 aryl)-substituted amino, di-(C 5 -C 24 aryl)-substituted amino, C 2 -C 24 alkylamido (—NH—(CO)-alkyl), C 6 -C 24 arylamido (—NH—(CO)-aryl), imino (—CR═NH where R=hydrogen, C 1 -C 24 alkyl, C 5 -C 24 aryl, C 6 -C 24 alkaryl, C 6 -C 24 aralkyl, etc.), C 2 -C 20 alkylimino (—CR═N(alkyl), where R=hydrogen, C 1 -C 24 alkyl, C 5 -C 24 aryl, C 6 -C 24 alkaryl, C 6 -C 24 aralkyl, etc.), arylimino (—CR═N(aryl), where R=hydrogen, C 1 -C 20 alkyl, C 5 -C 24 aryl, C 6 -C 24 alkaryl, C 6 -C 24 aralkyl, etc.), nitro (—NO 2 ), nitroso (—NO), sulfo (—SO 2 —OH), sulfonato (—SO 2 —O − ), C 1 -C 24 alkylsulfanyl (—S-alkyl; also termed “alkylthio”), C 5 -C 24 arylsulfanyl (—S-aryl; also termed “arylthio”), C 1 -C 24 alkylsulfinyl (—(SO)-alkyl), C 5 -C 24 arylsulfinyl (—(SO)-aryl), C 1 -C 24 alkylsulfonyl (—SO 2 -alkyl), C 5 -C 24 arylsulfonyl (—SO 2 -aryl), boryl (—BH 2 ), borono (—B(OH) 2 ), boronato (—B(OR) 2 where R is alkyl or other hydrocarbyl), phosphono (—P(O)(OH) 2 ), phosphonato (—P(O)(O) 2 ), phosphinato (—P(O)(O − )), phosphor (—PO 2 ), and phosphino (—PH 2 ); and the hydrocarbyl moieties C 1 -C 24 alkyl (preferably C 1 -C 12 alkyl, more preferably C 1 -C 6 alkyl), C 2 -C 24 alkenyl (preferably C 2 -C 12 alkenyl, more preferably C 2 -C 6 alkenyl), C 2 -C 24 alkynyl (preferably C 2 -C 12 alkynyl, more preferably C 2 -C 6 alkynyl), C 5 -C 24 aryl (preferably C 5 -C 24 aryl), C 6 -C 24 alkaryl (preferably C 6 -C 16 alkaryl), and C 6 -C 24 aralkyl (preferably C 6 -C 16 aralkyl).
[0110] By “functionalized” as in “functionalized hydrocarbyl”, “functionalized alkyl”, “functionalized olefin”, “functionalized cyclic olefin”, and the like, is meant that in the hydrocarbyl, alkyl, olefin, cyclic olefin, or other moiety, at least one hydrogen atom bound to a carbon (or other) atom is replaced with one or more functional groups such as those described hereinabove.
[0111] In addition, the aforementioned functional groups may, if a particular group permits, be further substituted with one or more additional functional groups or with one or more hydrocarbyl moieties such as those specifically enumerated above. Analogously, the above-mentioned hydrocarbyl moieties may be further substituted with one or more functional groups or additional hydrocarbyl moieties such as those specifically enumerated.
[0112] The present invention comprises a novel family of metathesis catalyst compounds useful for the different types of olefin and alkyne metathesis reactions, including but not limited to Ring closing metathesis (RCM), Cross metathesis (CM), Ring opening metathesis (ROM), Ring opening metathesis polymerization (ROMP), acyclic diene metathesis (ADMET), self-metathesis, conversion of olefins with alkynes (enyne metathesis), polymerization of alkynes, ethylene cross-metathesis and so on.
[0000]
[0113] M is a Group 8 metal, preferably ruthenium or osmium,
[0114] R 1 -R 6 are identical or different and represents hydrogen, halogen, hydroxyl, aldehyde, keto, thiol, CF 3 , nitro, nitroso, cyano, thiocyano, isocyanates, carbodiimide, carbamate, thiocarbamate, dithiocarbamate, amino, amido, imino, ammonium, silyl, sulphonate (—SO 3 − ), —OSO 3 − , —PO 3 − or —OPO 3 − , acyl, acyloxy or represents alkyl, cycloalkyl, alkenyl, cycloalkenyl, substituted alkenyl, heteroalkenyl, heteroatom-containing alkynyl, alkenylene, alkynyl, substituted alkynyl, aryl, substituted aryl, heteroaryl, carboxylate, alkoxy, alkenyloxy, alkynyloxy, aryloxy, alkaryl, aralkyl, alkaryloxy, aralkyloxy, alkoxycarbonyl, alkylamino-, alkylthio-, arylthio, alkyl sulfonyl, alkylsulfinyl, dialkylamino, alkylammonium, alkyl silyl or alkoxysilyl, where these radicals may each optionally all be substituted by one or more aforementioned groups defined for R 1 -R 6 , and except that R 2 does not represent phenyl when R 1 ═R 3 ═R 4 ═R 5 =R 6 ═H;
[0115] or alternatively in each case two directly adjacent radicals from the group of R 1 -R 6 , including the ring carbon atoms to which they are attached by a cyclic bridging group, generating one or more cyclic structures, including aromatic structures.
[0116] C 1 -C 6 alkyl is, but not limited to, for example methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl, tert-butyl, n-pentyl, 1-methylbutyl, 2-methylbutyl, 3-methylbutyl, neo-pentyl, 1-ethyl-propyl and n-hexyl.
[0117] C 3 -C 8 cycloalkyl includes, but not limited to, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl and cyclooctyl.
[0118] C 6 -C 24 aryl includes an aromatic radical having 6 to 24 skeletal carbon atoms. Preferred mono-, bi- or tricyclic carbocyclic aromatic radicals have 6 to 10 skeletal carbon atoms, for example but not limited to, phenyl, biphenyl, naphthyl, phenanthrenyl or anthracenyl.
[0119] X 1 preferably represents an anionic ligand.
[0120] In the general formulas X 1 can be for example, hydrogen, halogen, pseudohalogen, straight-chain or branched C 1 -C 30 alkyl, C 6 -C 24 aryl, C 1 -C 20 alkoxy, C 6 -C 24 aryloxy, C 3 -C 20 alkyl diketonate, C 6 -C 24 aryl diketonate, C 1 -C 20 carboxylate, C 1 -C 20 alkylsulfonate, C 6 -C 24 aryl sulfonate, C 1 -C 20 alkyl thiol, C 6 -C 24 aryl thiol, C 1 -C 20 alkyl sulfonyl or C 1 -C 20 alkylsulfinyl-radicals.
[0121] The abovementioned radical X 1 may further be substituted by one or more additional residues, for example by halogen, preferably fluorine, C 1 -C 20 alkyl, C 1 -C 20 -alkoxy or C 6 -C 24 aryl, where these groups may optionally be in turn be substituted by one or more substituents from the group comprising halogen, preferable fluorine, C 1 -C 5 alkyl, C 1 -C 5 alkoxy, and phenyl.
[0122] L 1 and X 1 may be joined to form a multidentate monoanionic group and may form a single ring of up to 30 non-hydrogen atoms or a multinuclear ring system of up to 30 non-hydrogen atoms;
[0123] In a preferred embodiment, X 1 denote halogen, in particular, fluorine, chlorine, bromine or iodine, benzoate, nitrate, C 1 -C 5 carboxylate, C 1 -C 5 alkyl, phenoxy, C 1 -C 5 alkoxy, C 1 -C 5 alkyl thiol, C 6 -C 24 arylthiol, C 6 -C 24 aryl or C 1 -C 5 alkyl sulfonate.
[0124] In a particularly preferred embodiment, X 1 is chlorine, CF 3 COO, CH 3 COO, CFH 2 COO, (CH 3 ) 3 CO, nitrate, (CF 3 ) 2 (CH 3 )CO, (CF 3 )(CH 3 ) 2 CO, PhO (phenoxy), C 6 F 5 O (pentafluorophenoxy), MeO (methoxy), EtO (ethoxy), tosylate (p-CH 3 —C 6 H 4 —SO 3 ), mesylate (2,4,6-trimethylphenyl) or CF 3 SO 3 (trifluoromethanesulfonate).
[0125] A 1 -A 2 are identical or different and are selected from the group consisting of oxygen, sulphur, selenium, NR″″, PR″″, POR″″, AsR″″, AsOR″″, SbOR″″ and SbR″″.
[0126] T 1 -T 2 are identical or different and selected from the group consisting of
[0000]
[0127] Wherein E preferably represents a donor atom selected from the group consisting of nitrogen, phosphor, oxygen, sulphur, and selenium; wherein for the group
[0000]
[0000] in case of oxygen, sulphur and selenium, R is omitted for double bonded E or R remains for a single bonded E; wherein for the group
[0000]
[0000] in case of oxygen, sulphur and selenium, the E-C bound is a single bond and the C atom contains an extra R group or the C—R′ is a double bond or the C—R is a double bond.
[0128] R, R′, R″, R′″ and R″″ are identical or different and represents hydrogen, halogen, hydroxyl, aldehyde, keto, thiol, CF 3 , nitro, nitroso, cyano, thiocyano, isocyanates, carbodiimide, carbamate, thiocarbamate, dithiocarbamate, amino, amido, imino, ammonium, silyl, sulphonate (—SO 3 − ), —OSO 3 − , —PO 3 − or —OPO 3 − , acyl, acyloxy or represents alkyl, cycloalkyl, alkenyl, cycloalkenyl, substituted alkenyl, heteroalkenyl, heteroatom-containing alkynyl, alkenylene, alkynyl, substituted alkynyl, aryl, substituted aryl, heteroaryl, carboxylate, alkoxy, alkenyloxy, alkynyloxy, aryloxy, alkaryl, aralkyl, alkaryloxy, aralkyloxy, alkoxycarbonyl, alkylamino-, alkylthio-, arylthio, alkyl sulfonyl, alkylsulfinyl, dialkylamino, alkylammonium, alkyl silyl or alkoxysilyl, where these radicals may each optionally all be substituted by one or more aforementioned groups defined for R, R′, R″, R′″ and R″″, wherein alternatively in each case two directly adjacent radicals from the group of R, R′, R″, R′″ and R″″, including the atoms to which they are attached, generating one or more cyclic structures, including aromatic structures.
[0129] C 1 -C 6 alkyl is, but not limited to, for example methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl, tert-butyl, n-pentyl, 1-methylbutyl, 2-methylbutyl, 3-methylbutyl, neopentyl, 1-ethyl-propyl and n-hexyl.
[0130] C 3 -C 8 cycloalkyl includes, but not limited to, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl and cyclooctyl.
[0131] C 6 -C 24 aryl includes an aromatic radical having 6 to 24 skeletal carbon atoms. Preferred mono-, bi- or tricyclic carbocyclic aromatic radicals have 6 to 10 skeletal carbon atoms, for example but not limited to, phenyl, biphenyl, naphthyl, phenanthrenyl or anthracenyl.
[0132] Alternatively R is optionally substituted with a neutral donor ligand (L 2 ) as defined by L 1 .
[0133] C 1 -C 2 are carbon atoms linked to each other via a single or double bond wherein in case of a single bond each carbon atom bears an extra substituent R C1 and R C2 .
[0134] R C1 and R C2 are identical or different and are as defined for R′, R″, R′″ and R″″.
[0135] L 1 preferably represent neutral electron donor.
[0136] The ligand L 1 may, for example, represent a phosphine, sulphonated phosphine, phosphate, phosphinite, phosphonite, phosphite, arsine, stibine, ether, amine, amide, sulfoxide, carboxyl, nitrosyl, pyridine, substituted pyridine, pyrazine, thiocarbonyl, thioether, triazole carbene, mesionic carbene (MIC), N-Heterocyclic carbene (“NHC”), substituted NHC, or cyclic alkyl amino carbene (CAAC) or substituted CAAC.
[0137] Preferably, ligand L 1 represents a phosphine ligand having the formula P(Q 1 ) 3 with Q 1 are identical or different and are alkyl, preferably C 1 -C 10 alkyl, more preferably C 1 -C 5 -alkyl, cycloalkyl-, preferably C 3 -C 20 cycloalkyl, more preferably C 3 -C 8 cycloalkyl, preferably cyclopentyl, cyclohexyl, and neopentyl, aryl, preferably C 6 -C 24 aryl, more preferably phenyl or toluyl, C 1 -C 10 alkyl-phosphabicyclononane, C 3 -C 20 cycloalkyl phospha-bicyclononane, a sulfonated phosphine ligand of formula P(Q 2 ) 3 wherein Q 2 represents a mono- or poly-sulfonated Q 1 -ligand; C 6 -C 24 aryl or C 1 -C 10 alkyl-phosphinite ligand, a C 6 -C 24 aryl or C 1 -C 10 alkyl phosphonite ligand, a C 6 -C 24 aryl or C 1 -C 10 alkyl phosphite-ligand, a C 6 -C 24 aryl C 1 -C 10 alkyl arsine ligand, a C 6 -C 24 aryl or C 1 -C 10 alkyl amine ligands, a pyridine ligand, a C 6 -C 24 aryl or C 1 -C 10 alkyl-sulfoxide ligand, a C 6 -C 24 aryl or C 1 -C 10 alkyl ether ligand or a C 6 -C 24 aryl or C 1 -C 10 alkyl amide ligands which all can be multiply substituted, for example by a phenyl group, wherein these substituents are in turn optionally substituted by one or more halogen, C 1 -C 5 alkyl or C 1 -C 5 alkoxy radicals.
[0138] The term “phosphine” includes, for example, PPh 3 , P(p-Tol) 3 , P(o-Tol), PPh(CH 3 ) 2 , P(CF 3 ) 3 , P(p-FC 6 H 4 ) 3 , P(p-CF 3 C 6 H 4 ) 3 , P(C 6 H 4 —SO 3 Na) 3 , P(CH 2 C 6 H 4 —SO 3 Na) 3 , P(iso-Propyl) 3 , P(CHCH 3 (CH 2 CH 3 )) 3 , P(cyclopentyl) 3 , P(cyclohexyl) 3 , P(Neopentyl) 3 and cyclohexyl-phosphabicyclononane.
[0139] The term “phosphinite” includes for example triphenylphosphinite, tricyclohexylphosphinite, triisopropylphosphinite and methyldiphenylphosphinite.
[0140] The term “phosphite” includes, for example, triphenyl phosphite, tricyclohexyl phosphite, tri-tert-butyl phosphite, triisopropyl phosphite and methyldiphenylphosphite.
[0141] The term “stibine” includes, for example triphenylstibine, tricyclohexylstibine and Trimethylstibene.
[0142] The term “sulfonate” includes, for example, trifluoromethanesulfonate, tosylate and mesylate.
[0143] The term “sulfoxide” includes, for example, CH 3 S(═O)CH 3 and (C 6 H 5 ) 2 SO.
[0144] The term “thioether” includes, for example CH 3 SCH 3 , C 6 H 5 SCH 3 , CH 3 OCH 2 CH 2 SCH 3 and tetra-hydrothiophene.
[0145] The term “pyridine” in this application is a generic term and includes all the unsubstituted and substituted nitrogen-containing ligands described in WO-A-03/011455 and U.S. Pat. No. 6,759,537 B2. Examples are: pyridine, picolines (α-, β-, and γ-picoline), lutidines (2,3-, 2,4-, 2,5-, 2,6-, 3,4- and 3,5-lutidine), collidine (2,4,6-trimethylpyridine), trifluoromethylpyridine, phenylpyridine, 4-(dimethylamino) pyridine, chloropyridines (2-, 3- and 4-chloropyridine), bromopyridines (2-, 3- and 4-bromopyridine), nitropyridines (2-, 3- and 4-nitropyridine), bipyridine, picolylimine, gamma-pyran, phenanthroline, pyrimidine, bipyrimide, pyrazine, indole, coumarine, carbazole, pyrazole, pyrrole, imidazole, oxazole, thiazole, dithiazole, isoxazole, isothiazole, quinoline, bisquinoline, isoquinoline, bisisoquinoline, acridine, chromene, phenazine, phenoxazine, phenothiazine, triazine, thianthrene, purine benzimidazole, bisimidazole, bisoxazole, pyrrole, imidazole and phenylimidazole.
[0146] In other useful embodiment ligand L 1 represents a N-Heterocyclic carbene (NHC) usually having a structure of the formulas (IIIa) or (IIIb):
[0000]
[0147] by which
[0148] R 7 -R 14 , R 11′ , R 12′ are identical or different and are hydrogen, halogen, hydroxyl, aldehyde, keto, thiol, CF 3 , nitro, nitroso, cyano, thiocyano, isocyanates, carbodiimide, carbamate, thiocarbamate, dithiocarbamate, amino, amido, imino, ammonium, silyl, sulphonate (—SO 3 − ), —OSO 3 − , —PO 3 − or —OPO 3 − , acyl, acyloxy or represents alkyl, cycloalkyl, alkenyl, cycloalkenyl, substituted alkenyl, heteroalkenyl, heteroatom-containing alkynyl, alkenylene, alkynyl, substituted alkynyl, aryl, substituted aryl, heteroaryl, carboxylate, alkoxy, alkenyloxy, alkynyloxy, aryloxy, alkaryl, aralkyl, alkaryloxy, aralkyloxy, alkoxycarbonyl, alkylammonium, alkylamino-, alkylthio-, arylthio, alkylsulfonyl, alkylsulfinyl, dialkylamino, alkylsilyl or alkoxysilyl, where these radicals may each optionally all be substituted by one or more aforementioned groups defined for R 1 -R 6 .
[0149] Optionally, one or more of the radicals R 7 -R 14 , R 11′ , R 12′ independently of one another can be substituted by one or more substituents, preferably straight or branched C 1 -C 10 alkyl, C 3 -C 8 cycloalkyl, C 1 -C 10 alkoxy or C 6 -C 24 aryl, where these aforementioned substituents may in turn be substituted by one or more radicals, preferably selected from the group comprising halogen, especially chlorine or bromine, C 1 -C 5 alkyl, C 1 -C 5 alkoxy and phenyl.
[0150] Just for clarification, the depicted structures of the N-Heterocyclic carbene in the general formulas (IIIa) and (IIIb) are equal with the N-Heterocyclic carbenes described in the literature, where frequently the structures (IIIa′) and (IIIb′) are used, which highlighting the carbene character of N-Heterocyclic carbene. This also applies to the corresponding preferred, structures shown below (IVa)-(IVf)
[0000]
[0151] In a preferred embodiment of the catalysts the general formulas (IIIa) and (IIIb) R 7 , R 8 , R 11 , R 11′ R 12 and R 12′ are independently of one another denote hydrogen, C 6 -C 24 -aryl, particularly preferably phenyl, straight or branched C 1 -C 10 alkyl, particularly preferably propyl or butyl, or together with the inclusion of the carbon atoms to which they are attached form a cycloalkyl or aryl radical, where all the abovementioned radicals are optionally substituted may be substituted by one or more further radicals selected from the group comprising straight or branched C 1 -C 10 alkyl, C 1 -C 10 alkoxy, C 6 -C 24 aryl, and a functional group selected from the group consisting of hydroxy, thiol, thioether, ketone, aldehyde, ester, ether, amine, imine, amide, nitro, carboxylic acid, disulfide, carbonate, isocyanate, carbodiimide, carboalkoxy, carbamate, and halogen.
[0152] In a particularly preferred embodiment, the catalysts of the general formulas (I-II) have one N-Heterocyclic carbene (NHC) as ligand L 1 , where the radicals R 9 , R 10 , R 13 and R 14 are identical or different and are straight or branched C 1 -C 10 alkyl, particularly preferably i-propyl or neopentyl, C 3 -C 10 cycloalkyl, preferably adamantyl, C 6 -C 24 aryl, particularly preferably phenyl, C 1 -C 10 alkylsulfonate, particularly preferably methanesulphonate, C 1 -C 10 aryl sulphonate, particularly preferably p-toluenesulfonate.
[0153] If necessary, the above-mentioned residues are substituted as the meanings of R 9 , R 10 , R 13 and R 14 by one or more further radicals selected from the group comprising straight or branched C 1 -C 5 alkyl, especially methyl, C 1 -C 5 alkoxy, aryl and a functional group selected from the group consisting of hydroxy, thiol, thioether, ketone, aldehyde, ester, ether, amine imine, amide, nitro, carboxylic acid, disulfide, carbonate, isocyanate, carbodiimide, carboalkoxy, carbamate, and halogen.
[0154] In particular, the radicals R 9 , R 10 , R 13 and R 14 can be identical or different and denote i-propyl, neopentyl, adamantyl, mesityl or 2,6-diisopropylphenyl.
[0155] Particularly preferred N-Heterocyclic carbenes (NHC) have the following structure (IVa)-(IVf), in which Mes stands for a 2,4,6-trimethylphenyl radical or alternatively, in all cases, for a 2,6-diisopropylphenyl radical.
[0000]
[0156] In alternative embodiment, the neutral ligand L may be selected from a ligand of any of the formulas (Va-Vc):
[0000]
[0157] R 8 , R 9 , R 10 , R 11 , R 11′ , R 12 , R 13 , R 14 are identical or different and are equal to R 3 -R 6 defined as herein-above. Any adjacent group of R 11 , R 11′ and R 12 in structure (Vb) and (Vc) may form a 3, 4, 5, 6, or 7 membered cycloalkyl, alkylene bridge, or aryl.
[0158] In other useful embodiments, one of the N groups bound to the carbene in Formula (IIIa) or (IIIb) is replaced with another heteroatom, preferably S, O or P, preferably an S heteroatom. Other useful N-heterocyclic carbenes include the compounds described in Chem. Eur. J 1996, 2, 772 and 1627 ; Angew. Chem. Int. Ed. 1995, 34, 1021 ; Angew. Chem. Int. Ed. 1996, 35, 1121; and Chem. Rev. 2000, 100, 39.
[0159] For purposes of this invention and claims thereto, “cyclic alkyl amino carbenes” (CAACs) are represented by the Formula (VI):
[0000]
[0160] Wherein the ring A is a 4-, 5-, 6-, or 7-membered ring, and Z is a linking group comprising from one to four linked vertex atoms selected from the group comprising C, O, N, B, Al, P, S and Si with available valences optionally occupied by hydrogen, oxo or R-substituents, wherein R is independently selected from the group comprising C 1 to C 12 hydrocarbyl groups, substituted C 1 to C 12 hydrocarbyl groups, and halides, and each R 15 is independently a hydrocarbyl group or substituted hydrocarbyl group having 1 to 40 carbon atoms, preferably methyl, ethyl, propyl, butyl (including isobutyl and n-butyl), pentyl, cyclopentyl, hexyl, cyclohexyl, octyl, cyclooctyl, nonyl, decyl, cyclodecyl, dodecyl, cyclododecyl, mesityl, adamantyl, phenyl, benzyl, toluyl, chlorophenyl, phenol, or substituted phenol.
[0161] Some particularly useful CAACs include:
[0000]
[0162] Other useful CAACs include the compounds described in U.S. Pat. No. 7,312,331 and in Angew. Chem. Int. Ed. 2005, 44, 7236-7239.
[0163] For the case that the R group present in T 1 or T 2 of the inventive catalysts with the general formula (I) is further substituted with a neutral donor ligand, the following examples can be generated with the structures of the general formula (VII).
[0000]
[0164] Wherein the ring G is a 4-, 5-, 6-, 7-, 8-, 9- or 10-membered ring, and Z is a linking group comprising from one to seven linked vertex atoms selected from the group comprising C, O, N, P, S and Si with available valences optionally occupied by hydrogen, halogen, hydroxyl, aldehyde, keto, thiol, CF 3 , nitro, nitroso, cyano, thiocyano, isocyanates, carbodiimide, carbamate, thiocarbamate, dithiocarbamate, amino, amido, imino, ammonium, silyl, sulphonate (—SO 3 − ), —OSO 3 − , —PO 3 − or —OPO 3 − , acyl, acyloxy or represents alkyl, cycloalkyl, alkenyl, cycloalkenyl, substituted alkenyl, heteroalkenyl, heteroatom-containing alkynyl, alkenylene, alkynyl, substituted alkynyl, aryl, substituted aryl, heteroaryl, carboxylate, alkoxy, alkenyloxy, alkynyloxy, aryloxy, alkaryl, aralkyl, alkaryloxy, aralkyloxy, alkoxycarbonyl, alkylamino-, alkylthio-, arylthio, alkyl sulfonyl, alkylsulfinyl, dialkylamino, alkylammonium, alkylsilyl or alkoxysilyl, where these vertex atoms may each optionally all be substituted by one or more aforementioned groups defined for R, R″, R′″ and R″″,
[0165] or alternatively in each case two directly adjacent vertex atoms from Z generate one or more cyclic structures, including aromatic structures.
[0166] L 1 and L 2 are identical or different ligands, preferably represent neutral electron donors, and L 2 has the same meaning as L 1 as defined in structures (I-II)
[0167] wherein M, X 1 , A 1 , T 1 , L 1 , R 1 -R 6 and R′, R″, R′″ and R″″ have the same meanings as defined in the general structures (I-II).
[0168] As examples of the catalysts of the invention, the following structures may be mentioned:
[0000]
[0169] In certain embodiments, the catalyst compound employed in the olefin metathesis processes may be bound to or deposited on a solid catalyst support. The solid catalyst support will make the catalyst compound heterogeneous, which will simplify catalyst recovery. In addition, the catalyst support may increase catalyst strength and attrition resistance. Suitable catalyst supports include, without limitation, silica's, alumina's, silica-alumina's, aluminosilicates, including zeolites and other crystalline porous aluminosilicates; as well as titania's, zirconia, magnesium oxide, carbon, carbon nanotubes, graphene, Metal organic frameworks and cross-linked, reticular polymeric resins, such as functionalized cross-linked polystyrenes, e.g., chloromethyl-functionalized cross-linked polystyrenes.
[0170] The catalyst compound may be deposited onto the support by any method known to those skilled in the art, including, for example, impregnation, ion-exchange, deposition-precipitation, II-II interactions and vapor deposition. Alternatively, the catalyst compound may be chemically bound to the support via one or more covalent chemical bonds, for example, the catalyst compound may be immobilized by one or more covalent bonds with one or more of substituents of the indenylidene ligand or directly immobilized via one or more chemical bounds on the Group 8 metal by substituting one or more anionic ligands or immobilized via one or more chemical bounds between the ligand and the support.
[0171] If a catalyst support is used, the catalyst compound may be loaded onto the catalyst support in any amount, provided that the metathesis process proceeds to the desired metathesis products. Generally, the catalyst compound is loaded onto the support in an amount that is greater than about 0.01 wt % of the Group 8 metal, based on the total weight of the catalyst compound plus support. Generally, the catalyst compound is loaded onto the support in an amount that is less than about 20 wt % of the Group 8 metal, based on the total weight of the catalyst compound and support.
[0172] In general, acetylenic compounds useful in this invention may contain a chelating moiety of the formula (VIII)
[0000]
[0173] wherein,
[0174] D is a leaving group;
[0175] R 16 to R 17 are as defined below;
[0176] R 16 is selected from hydrogen, halogen, alkyl, alkenyl, alkynyl, aryl, heteroalkyl, heteroatom containing alkenyl, heteroalkenyl, heteroaryl, alkoxy, alkenyloxy, aryloxy, alkoxycarbonyl, carbonyl, alkylamino, alkylthio, aminosulfonyl, monoalkylaminosulfonyl, dialkylaminosulfonyl, alkyl sulfonyl, nitrile, nitro, alkylsulfinyl, trihaloalkyl, perfluoroalkyl, carboxylic acid, ketone, aldehyde, nitrate, cyano, isocyanate, hydroxyl, ester, ether, amine, imine, amide, halogen-substituted amide, trifluoroamide, sulfide, disulfide, sulfonate, carbamate, silane, siloxane, phosphine, phosphate, or borate, and wherein when R 16 is aryl, polyaryl, or heteroaryl, R 16 may be substituted with any combination of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 and can be linked with any of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 to form one or more cyclic aromatic or non-aromatic groups.
[0177] R 17 is selected from annulenes, having the general formula C n H n (when n is an even number) or C n H n+1 (when n is an odd number). Well-know representative compounds of annulenes, but not limited, are cyclobutadiene, benzene, and cyclooctatetraene. Annulenes can be aromatic or anti-aromatic. Every H-atom from the annulene fragment can be substituted by halogen, alkyl, alkenyl, alkynyl, aryl, heteroalkyl, heteroatom containing alkenyl, heteroalkenyl, heteroaryl, alkoxy, alkenyloxy, aryloxy, alkoxycarbonyl, carbonyl, alkylamino, alkylthio, aminosulfonyl, monoalkylaminosulfonyl, dialkylaminosulfonyl, alkyl sulfonyl, nitrile, nitro, alkylsulfinyl, trihaloalkyl, perfluoroalkyl, carboxylic acid, ketone, aldehyde, nitrate, cyano, isocyanate, hydroxyl, ester, ether, amine, imine, amide, halogen-substituted amide, trifluoroamide, sulfide, disulfide, sulfonate, carbamate, silane, siloxane, phosphine, phosphate, or borate, and wherein when R 17 is aryl, polyaryl, or heteroaryl, R 17 may be substituted with any combination of R 1 , R 2 , R 3 , R 4 , R 5 , and can be linked with any of R 1 , R 2 , R 3 , R 4 , R 5 and R 6 to form one or more cyclic aromatic or non-aromatic groups.
[0178] Examples of suitable leaving groups include, but are not limited to, hydroxyl, halide, ester, perhalogenated phenyl, acetate, benzoate, C 2 -C 6 acyl, C 2 -C 6 alkoxycarbonyl, C 1 -C 6 alkyl, phenoxy, C 1 -C 6 alkoxy, C 1 -C 6 alkylsulfanyl, aryl, or C 1 -C 6 alkylsulfonyl. In even more preferred embodiments, D is selected from hydroxyl, halide, CF 3 CO 2 , CH 3 CO 2 , CFH 2 CO 2 , (CH 3 ) 3 CO 3 (CF 3 ) 2 (CH 3 )CO, (CF 3 )(CH 3 ) 2 CO, PhO, MeO, EtO, tosylate, mesylate, or trifluoromethane-sulfonate. In particular embodiments, D is advantageously hydroxyl (OH).
[0179] Preferred organic acetylenic compounds are of the formula (IX),
[0000]
[0180] Wherein
[0181] m* is an integer from 1 to 5;
[0182] R* is selected from R 1 , R 2 , R 3 , R 4 , R 5 and R 6 , or combinations thereof, as defined above.
[0183] D and R 16 are as defined above.
[0184] Preferred organic acetylenic compounds include:
[0000]
[0185] Synthesis of Metathesis Catalyst Compounds
[0186] The catalyst compounds described in this invention may be synthesized by any methods known to those skilled in the art.
[0187] Representative methods of synthesizing the Group 8 catalyst compound of the type described herein include, for example, treating a solution of the acetylenic compound in a suitable solvent, such as dioxane, with a reactant complex of a Group 8 metal, such as dichlorobis-(triphenylphosphine)ruthenium(II) and hydrogen chloride (in dioxane). The reaction mixture may be heated, for a time period appropriate to yield the desired modified indenylidene catalyst compound. Typically, removal of the volatiles and washed with hexane affords the Group 8 modified indenylidene 1 st generation compound (Scheme 4) in high yields (>80%).
[0188] A phosphine ligand, such as tricyclohexylphosphine, cyclohexyl-phosphabicyclononane, a phosphinite or a phosphinite may be added thereafter, if desired. The reaction conditions typically include mixing the Group 8 reactant compound and the preferred phosphine ligand in a suitable solvent, e.g. dichloromethane, for a time sufficient to effectuate the phosphine ligand exchange, at a suitable temperature typically ambient, yield (>90%).
[0189] A N-Heterocyclic carbenes (NHC), such as 1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene, 1,3-bis(2,6-diisopropylphenyl)-2-imidazolidinylidene or a CAAC may be added 1 st generation compound (Scheme 4), if desired. The reaction conditions typically include mixing the Group 8 reactant 1 st generation compound (Scheme 4) and the preferred NHC, CAAC ligand in a suitable solvent, e.g. toluene, for a time sufficient to effectuate the phosphine ligand exchange, at a suitable temperature typically between ambient and 80° C. Addition of isopropanol followed by filtration and washing, the desired 2 nd generation compound (Scheme 4) is obtained in high yield (>85%).
[0190] A pyridine ligand, such as pyridine, 3-Br pyridine may be added 2 nd generation compound (Scheme 4), if desired. The reaction conditions typically include mixing the Group 8 reactant 2 nd generation compound (Scheme 4) and the preferred pyridine ligand in as solvent, for a time sufficient to effectuate the phosphine ligand exchange, at a suitable temperature typically between ambient and 80° C. Filtration and washing gives the desired 3 rd generation compound (Scheme 4) in high yield (>85%).
[0000]
[0191] Scheme 4: different generations of non-chelating modified indenylidene catalysts.
[0192] Treating a solution of the ditopic (or multitopic) ligand, e.g. O,N-bidentate ligands, in a suitable solvent, such as THF, with a 1 st or 2 nd or 3 rd generation non-chelating modified indenylidene complex (see scheme 4), e.g. (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene in a 1:1 ratio and adding a required amount of silver (e.g. AgO 2 ) for a time sufficient to effectuate the ligand exchange, at a suitable temperature typically between ambient and 80° C. to yield the desired modified indenylidene catalyst compound. The reaction temperature was then lowered to room temperature, the white precipitate of PCy 3 AgCl (byproduct) and excess of Ag 2 O was removed by filtration and the filtrate was concentrated under reduced pressure. The isolated solid residue provides the desired product (type I) in high yield (>85%).
[0193] Treating a solution of the ditopic (or multitopic) ligand, e.g. O,N-bidentate ligands, in a suitable solvent, such as THF, with a 1 st or 2 nd or 3 rd generation non-chelating modified indenylidene complex (see scheme 4), e.g. (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene in a 2:1 ratio and adding an equivalent amount of silver (e.g. AgO 2 ) for a time sufficient to effectuate the ligand exchange, at a suitable temperature typically between ambient and 80° C. to yield the desired modified indenylidene catalyst compound. The reaction temperature was then lowered to room temperature, the white precipitate of PCy 3 AgCl (byproduct) and excess of Ag 2 O was removed by filtration and the filtrate was concentrated under reduced pressure. The isolated solid residue provides the desired product (type II) in high yield (>85%).
[0194] Treating a solution of the ditopic (or multitopic) ligand, e.g. O,N-bidentate ligands, in a suitable solvent, such as THF, with a catalyst of type I in a 1:1 ratio and adding a required amount of silver (e.g. AgO 2 ) for a time sufficient to effectuate the ligand exchange, at a suitable temperature typically between ambient and 80° C. to yield the desired modified indenylidene catalyst compound. The reaction temperature was then lowered to room temperature, the white precipitate of PCy 3 AgCl (byproduct) and excess of Ag 2 O was removed by filtration and the filtrate was concentrated under reduced pressure. The isolated solid residue provides the desired product (type II) in high yield.
[0195] The exchange of the ditopic (or multitopic) ligands can also be performed by generating first the salt of the ligand (Sodium, Potassium, Magnesium, Thallium salts, . . . ) as is well-know by persons skilled in the art.
[0196] Examples, but not limited, of ditopic or multitopic ligands are described in WO2005035121, European patent 1 468 004, EP 08 290 747.
[0197] While the present invention describes a variety of transition metal complexes useful in catalyzing metathesis reactions, it should be noted that such complexes may be formed in situ. Accordingly, additional ligands may be added to a reaction solution as separate compounds, or may be complexed to the metal center to form a metal-ligand complex prior to introduction to the reaction.
[0198] Synthetic protocols for representative 1,1-substituted prop-2-yn-1-ol ligands, ditopic, multitopic ligands and the corresponding ruthenium alkylidene complexes are as follows. Other substituted prop-2-yn-1-ol, ditopic, multitopic ligands and their respective metal complexes may be derived analogously.
Example 1: 2-[(4-bromo-2,6-dimethylphenylimino)methyl]-4-nitrophenoxy (PCy 3 )(3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (1F)
Synthesis of (PPh 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methylinden-1-ylidene) (1D)
[0199]
Step 1: Bis(2-methylphenyl)methanone (1A)
[0200] To a solution of 2-bromotoluene (2 eq., 2.6 ml, 21.79 mmol,) in 26 ml diethyl ether at −90° C., t-BuLi (1.9 M in pentane) (3 eq., 32.7 mmol, 17.2 ml.) was added drop wise. The solution was stirred for 30 min. at room temperature, followed by drop wise addition of N,N-dimethylcarbamoyl chloride (1 eq., 1 ml, 10.9 mmol), the reaction mixture was stirred for another 3 hours. The crude reaction mixture was quenched using 35 ml 1N HCl and diluted with diethyl ether. The organic phase was washed with water and the aqueous phase was extracted twice with diethyl ether, thereafter the ether fractions were combined and dried with anhydrous MgSO 4 . Removal of MgSO 4 by filtration followed by purification using flash column chromatography (silica gel, hexane as solvent) and finally evaporation of the solvent and a white solid was obtained 0.93 g (40.6%).
[0201] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 7.38 (td, 2H), 7.29 (td, 4H), 7.20 (td, 2H), 2.44 (s, 6H).
[0202] 13 C NMR (75 MHz, CDCl 3 ): δ 200.79, 139.01, 138.17, 131.43, 131.07, 130.31, 125.42, 20.67.
Step 2: 1,1-bis-methylphenyl-3-(trimethylsilyl)prop-2-yn-1-ol (1B)
[0203] n-BuLi (2.5 M in hexanes) (1.5 eq., 5.7 ml, 14.28 mmol,) was added drop wise to stirred solution of trimethylsilylacetylene (1.5 eq., 2 ml, 14.28 mmol) in anhydrous THF (17 ml) at −90° C. under an argon atmosphere. After addition, the resulting solution was stirred for another 5 min in a cold bath followed by stirring for 30 minutes at room temperature. Thereafter, bis(2-methylphenyl)methanone (9.52 mmol, 2 g) in 17 ml dry THF was added slowly to the solution at −90° C. and the resulting mixture was allowed to heat up and refluxed for 30 min. The crude reaction mixture was quenched using 15 ml 1N HCl and diluted with diethyl ether. The organic phase was washed with water and the aqueous phase were combined and extracted twice with ether, thereafter the ether fractions were combined and dried with anhydrous MgSO 4 . After removal of MgSO 4 by filtration, and evaporation of the solvent a yellow liquid was obtained in quantitative yield. The obtained product was used without further purification.
[0204] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 7.95 (dd, 2H), 7.27 (dd, 4H), 7.15 (dd, 2H) 2.75 (s, 1H) 2.14 (s, 6H), 0.27 (d, 9H).
[0205] 13 C NMR (75 MHz, CDCl 3 ): δ 141.01, 136.76, 132.37, 128.13, 127.45, 125.58, 107.10, 92.44, 75.01, 21.40, 0.00.
Step 3: 1,1-bis-2-methylphenyl-prop-2-yn-1-ol (1C)
[0206] A solution of 1,1-bis-methylphenyl-3-(trimethylsilyl)prop-2-yn-1-ol was obtained from previous step and K 2 CO 3 (1 eq, 1.3 g 9.52 mmol) in dry methanol (10 ml) was stirred at room temperature for 3 h. The crude reaction mixture was quenched using 20 ml 1N HCl and diluted with diethyl ether. The organic phase was washed with water and the aqueous phase was extracted twice with diethyl ether, thereafter the ether fractions were combined and dried on anhydrous MgSO 4 . Removal of MgSO 4 by filtration followed by purification using flash column chromatography (silica gel, Hexane/EtOAc=30/1) and finally evaporation of the solvent a yellowish solid (2.06 g, 92% yield for step 2+3) was obtained.
[0207] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 7.95 (m, 2H), 7.23 (m, 4H), 7.09 (m, 2H) 2.89 (s, 1H) 2.67 (s, 1H), 2.02 (s, 6H).
[0208] 13 C NMR (75 MHz, CDCl 3 ): δ 140.60, 136.33, 132.30, 128.19, 127.24, 125.58, 85.52, 76.80, 74.75, 21.16.
[0209] ESI[M-OH]: 219.1, calculated: 219.1.
Step 4: (PPh 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene) (1D)
[0210] (PPh 3 ) 3 RuCl 2 (1 eq., 0.575 g, 0.6 mmol) and 1,1-bis-2-methylphenyl-prop-2-yn-1-ol (compound C, 1.5 eq., 0.213 g, 0.9 mmol) were added in 4 ml HCl/dioxane solution (0.15 mol/1). The solution was heated to 90° C. for 3 hour, after which the solvent was removed under vacuum. Hexane (20 ml) was added to the flask and the solid was ultrasonically removed from the wall. The resulting suspension was filtered and washed two times using hexane (5 ml). The remaining solvent was evaporated affording a red-brown powder; 0.52 g (Yield: 95%). The product was characterized by NMR spectra 1 H and 31 P.
[0211] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 7.56 (dd, 11H), 7.37 (t, 6H), 7.21-7.31 (m, 13H), 7.09 (tetra, 3H), 6.95 (t, 3H), 6.47 (t, 1H), 6.14 (s, 1H), 2.20 (s, 3H), 1.66 (s, 3H).
[0212] 31 P NMR (121.49 MHz, CDCl 3 ): δ 29.33.
Step 5: Synthesis of (PCy 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (1E)
[0213]
[0214] A 25 ml vial was charged with (PPh 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene) (1 eq., 0.4574 g, 0.5 mmol), tricyclohexylphosphine (3 eq., 0.42 g, 1.5 mmol) and dichloromethane (10 ml). After completion of the reaction (1 h) the resulting slurry was dried under vacuum and 20 ml isopropanol was added. Filtration afforded a red-brown powder, which after washing with 5 ml isopropanol (2×) and drying under vacuum afforded 0.44 g of catalyst (Yield: 93%). The product was characterized by NMR spectra 1 H and 31 P.
[0215] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 8.54 (d, 1H), 7.24-7.29 (m, 1H), 7.10-7.17 (m, 4H), 7.07 (s, 1H), 7.02 (d, 1H), 2.61 (d, 6H), 2.22 (s, 3H), 1.18-1.96 (m, 63H).
[0216] 31 P NMR (121.49 MHz, CDCl 3 ): δ 31.75, 31.56.
[0217] Characteristic values of 1 H and 31 P: H—C8: 8.54 ppm (d, 1H) and P: 31.75 and 31.56 ppm.
Step 6: Synthesis of 2-[(4-bromo-2,6-dimethylphenylimino)methyl]-4-nitrophenoxy (PCy 3 )(3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (1F)
[0218]
[0219] (PCy 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.53 mmol) and 2-[(4-bromo-2,6-dimethylphenylimino)methyl]-4-nitrophenol (0.53 mmol) (synthesized according the literature), silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0220] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 1F.
[0221] Characteristic values of 1 H and 31 P: H—C8: 6.75 ppm (d, 1H) and P: 39.65 ppm.
[0222] The isolated solid residue was recrystallized from pentane to provide the catalyst. Yield after recrystallization: 75%.
Example 2: Synthesis of (S-IMes)(2-[(2-methylphenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (2B)
Step 1: Synthesis of (S-IMes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene) (2A)
[0223]
S-IMes=saturated 1,3-bis(mesityl)-imidazolidine-2-ylidene (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)
[0224] A 10 mL vial was charged with (PCy 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene) (1 eq., 0.3804 g, 0.4 mmol) and 5-IMes (1.1 eq., 0.134 g, 0.44 mmol). Dry toluene (3 ml) was added under inert atmosphere. The mixture was vigorously stirred at 50° C. for 30 minutes and dried under vacuum followed by addition of 10 ml isopropanol. After filtration and washing (two times 5 ml isopropanol), an orange powder was obtained; 0.33 g (Yield: 84%). The product was characterized by NMR spectra 1 H, 13 C, and 31 P.
[0225] 1 H NMR (300 MHz, CDCl 3 , TMS): δ 8.47 (d, 1H), 7.44 (dd, 1H), 7.20-7.28 (m, 2H), 7.04-7.11 (m, 3H), 6.99 (d, 1H), 6.93 (s, 1H), 6.88 (d, 1H), 6.81 (s, 1H), 6.05 (s, 1H), 3.70-4.07 (m, 4H), 2.74 (s, 3H), 2.68 (s, 3H), 2.38 (s, 3H), 2.33 (s, 3H), 2.14 (s, 3H), 2.02 (s, 3H), 1.87 (s, 3H), 0.86-1.83 (m, 36H).
[0226] 13 C NMR (75 MHz, CDCl 3 ): δ 294.06, 293.96, 217.16, 216.19, 143.91, 140.11, 139.79, 139.52, 139.39, 138.77, 138.29, 136.94, 136.85, 136.27, 135.69, 134.04, 130.70, 130.01, 129.88, 129.57, 128.94, 128.58, 128.14, 127.25, 127.13, 126.27, 125.30, 125.05, 52.68, 52.64, 52.29, 52.26, 33.09, 32.87, 29.47, 29.24, 27.70, 27.57, 26.20, 21.18, 20.91, 20.32, 20.15, 19.36, 18.97, 18.92, 18.44.
[0227] 31 P NMR (121.49 MHz, CDCl 3 ): δ 26.75.
Step 2: Synthesis of (S-IMes)(2-[(2-methylphenylimino)methyl]-4-nitrophenoxy)(3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (2B)
[0228]
[0229] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene)(0.51 mmol) and 2-[(2-methylphenylimino)methyl]-4-nitrophenol (0.51 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0230] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 2B.
[0231] Characteristic values of 1 H: H—C8: 8.39 ppm (d, 1H). (no 31 P NMR peak present in the complex)
[0232] The isolated solid residue provided the catalyst in 85% yield.
Example 3: (S-IMes)(2-[(2-chlorophenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (3A)
[0233]
[0234] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene) (0.51 mmol) and 2-[(2-chlorophenylimino)methyl]-4-nitrophenol (0.51 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0235] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 3A.
[0236] Characteristic values of 1 H: H—C8: 8.33 ppm (d, 1H). (no 31 P NMR peak present in the complex)
[0237] The isolated solid residue provided the catalyst in 87% yield.
Example 4: Synthesis of (S-IMes)(2-[(4-bromo-2,6-dimethylphenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (4A)
[0238]
[0239] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[(4-bromo-2,6-dimethylphenylimino)methyl]-4-nitrophenol (0.53 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0240] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 4A.
[0241] Characteristic values of 1 H: H—C8: 8.45 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0242] The isolated solid residue provided the catalyst in 89% yield.
Example 5: Synthesis of (S-IMes)(2-[(2,6-dimethylphenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (5A)
[0243]
[0244] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[(2,6-dimethylphenylimino)methyl]-4-nitrophenol (0.53 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0245] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex 5A.
[0246] Characteristic values of 1 H: H—C8: 8.87 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0247] The isolated solid residue provided the catalyst in 91% yield.
Example 6: Synthesis of (S-IMes)(2-[(2,6-dimethylphenylimino)methyl]phenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (6A)
[0248]
[0249] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[(2,6-dimethylphenylimino)methyl]-phenol (0.53 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0250] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex X6A.
[0251] Characteristic values of 1 H: H—C8: 9.10 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0252] The isolated solid residue provided the catalyst in 91% yield.
Example 7: Synthesis of (S-IMes)(2-[(2,6-dimethylphenylimino)methyl]-4-methoxyphenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (7A)
[0253]
[0254] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[(2,6-dimethylphenylimino)methyl]-4-methoxyphenol (0.53 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0255] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex 7A.
[0256] Characteristic values of 1 H: H—C8: 9.15 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0257] The isolated solid residue provided the catalyst in 87% yield.
Example 8: Synthesis of (S-IMes)(2-[(pentafluorophenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (8A)
[0258]
[0259] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[pentafluorophenylimino)methyl]-4-nitrophenol (0.53 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0260] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex 8A.
[0261] Characteristic values of 1 H: H—C8: 8.25 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0262] The isolated solid residue provided the catalyst in 82% yield.
Example 9: Synthesis of (S-IMes)(2-[(3s,5s,7s)-adamantan-1-ylimino methyl]-4-nitrophenoxy)(3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (9A)
[0263]
[0264] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.51 mmol) and 2-[(3s,5s,7s)-adamantan-1-yliminomethyl]-4-nitrophenol (0.51 mmol) and silver(I) oxide (0.31 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0265] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 9A.
[0266] Characteristic values of 1 H: H—C8: 8.39 ppm (d, 1H). (no 31 P NMR peak present in the complex)
[0267] The isolated solid residue provided the catalyst in 84% yield.
Example 10: Synthesis of (2-[(2-methylphenylimino)methyl]-4-nitrophenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (10D)
Synthesis of (PPh 3 ) 2 Cl 2 Ru(3-i-propyl-inden-1-ylidene) (10B)
[0268]
Step 1: 1-i-propyl-1-phenyl-prop-2-yn-1-ol (10A)
[0269] Ethynylmagnesium bromide (1.2 eq, 12.7 mmol, 25.4 ml) (0.5M in THF) was added to (i-propyl)(phenyl)methanone (1 eq., 10.6 mmol, 1.57 g) in dry THF (7 ml). The resulting solution was allowed to heat up under reflux overnight. The crude mixture was quenched by addition of 1N HCl (15 ml) and diluted with diethyl ether. The organic layer was separated; the aqueous layer was extracted twice with diethyl ether. The organic layers were combined dried on anhydrous MgSO 4 , filtered, and concentrated under vacuum. The product obtained after column chromatography (Hexane: EtOAc 20:1) is a yellow liquid 1.75 g yield 95%.
[0270] 1 H NMR (300 MHz, CDCl 3 ): δ 7.61 (dt, 2H), 7.22-7.36 (m, 3H), 2.66 (s, 1H), 2.50 (s, 1H), 2.09 (sept, 1H), 1.06 (d, 3H), 0.81 (d, 3H).
[0271] 13 C NMR (75 MHz, CDCl 3 ): δ 143.42, 127.95, 127.74, 126.14, 85.03, 77.07, 74.99, 40.16, 17.90, 17.38.
Step 2: (PPh 3 ) 2 Cl 2 Ru(3-i-propyl-inden-1-ylidene) (10B)
[0272] (PPh 3 ) 3 RuCl 2 (1 eq., 0.575 g, 0.6 mmol) and 1-(i-propyl)-1-phenylprop-2-yn-1-ol (compound 18A, 1.5 eq., 0.144 g, 0.9 mmol) were added in 4 ml HCl/dioxane solution (0.15 mol/1). The solution was heated to 90° C. for 3 hour, after which the solvent was removed under vacuum. Hexane (20 ml) was added to the flask and the solid was ultrasonically removed from the wall. The resulting suspension was filtered and washed two times using hexane (5 ml). The remaining solvent was evaporated affording a red-brown powder; 0.48 g (Yield: 93%). The product was characterized by NMR spectra 31 P.
[0273] 31 P NMR (121.49 MHz, CDCl 3 ): δ 29.55.
Step 3: Synthesis of (PCy 3 ) 2 Cl 2 Ru(3-i-isopropyl-inden-1-ylidene) (10C)
[0274]
[0275] A 25 ml vial was charged with (PPh 3 ) 2 Cl 2 Ru(3-i-propyl-inden-1-ylidene) (1 eq., 0.4260 g, 0.5 mmol), tricyclohexylphosphine (3 eq., 0.42 g, 1.5 mmol) and dichloromethane (10 ml). After completion of the reaction (1 h) the resulting slurry was dried under vacuum and 20 ml isopropanol was added. Filtration afforded a red brown powder, which after washing with 5 ml isopropanol (2×) and drying under vacuum afforded 0.40 g of catalyst (Yield: 90%). The product was characterized by NMR spectra 1 H and 31 P.
[0276] Characteristic values of 1 H and 31 P: H—C8: 8.57 ppm (d, 1H) and P: 31.44 ppm.
Step 4: Synthesis of (2-[(2-methylphenylimino)methyl]-4-nitrophenoxy)(3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (10D)
[0277]
[0278] (Simes)(PCy 3 )Cl 2 Ru(3-isopropyl-inden-1-ylidene) (0.50 g, 0.55 mmol) and 2-[(2-methylphenylimino)methyl]-4-nitrophenol (0.14 g, 0.55 mmol), and silver(I) oxide (0.33 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0279] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex 10D.
[0280] Characteristic values of 1 H: H—C8: 8.29 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0281] The isolated solid residue provided the catalyst in 84% yield.
Example 11: Synthesis of (PCy 3 )(2-[(1-imidazole-3-propylimino)methyl]-phenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (11B)
Step 1: Synthesis of (1-imidazole-3-propylimino)methyl-phenol (11A)
[0282] Salicylaldehyde (37.54 mmol, 4.00 mL), 1-(3-aminopropyl)imidazole (37.54 mmol, 4.50 mL) and 15 ml ethyl alcohol were added to a 100 ml flask and refluxed for 4 hours. The resulting yellow solution was cooled overnight, filtered and washed with cold ethanol (3×1 mL). Bright yellow crystals were isolated in 90% yield.
[0283] 1 H NMR (300 MHz, CDCl 3 ) δ 13.09 (s, 1H), 8.25 (s, 1H), 7.39 35 (s, 1H), 7.26 (t, J=7.8 Hz, 1H), 7.18 (d, J=8.2 Hz, 1H), 7.01 (s, 1H), 6.93-6.79 (m, 3H), 4.00 (t, J=6.9 Hz, 2H), 3.48 (t, J=6.5 Hz, 2H), 2.12 (p, J=6.7 Hz, 2H). 13 C NMR (75 MHz, CDCl 3 ) δ 166.10, 160.90, 137.11, 132.57, 131.42, 129.79, 118.99, 116.98, 40 77.48, 76.64, 55.86, 44.30, 31.78 MS (EI, 70 eV, rel. intensity): 229 (100, M + ).
Step 2: Synthesis of Synthesis of (PCy 3 )(2-[(1-imidazole-3-propylimino)methyl]-phenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (11B)
[0284]
[0285] (PCy 3 ) 2 Cl 2 Ru(3-2-methylphenyl-5-methyl-inden-1-ylidene (0.53 mmol) and (1-imidazole-3-propylimino)methyl-phenol (0.53 mmol), silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (50° C.) and stirred for a period of 4 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure.
[0286] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 11B.
[0287] Characteristic values of 1 H and 31 P: H—C8: 7.25 ppm (d, 1H) and P: 36.95 ppm.
[0288] The isolated solid residue provided the catalyst in 75% yield.
Example 12: Synthesis of (S-IMes)(2-[(2-methylphenylimino)methyl]phenoxy) 2 (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II) (12)
Route A: Starting from (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene) (2A)
[0289]
[0290] (Simes)(PCy 3 )Cl 2 Ru(3-2-methylphenyl-5-methylphenyl-inden-1-ylidene) (0.51 mmol) and 2-[(2-methylphenylimino)methyl]phenol (1.1 mmol) and silver(I) oxide (0.65 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 5 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure. Addition of 2 mL CH 2 Cl 2 and an excess of cold pentane precipitate the catalyst as a deep red powder, Yield: 85%.
[0291] The reaction mixture was investigated on 1 H and 31 P NMR, which revealed quantitative transformation to complex 12.
[0292] Characteristic values of 1 H: H—C8: 8.11 ppm (d, 1H). (no 31 P NMR peak present in the complex)
[0293] The reaction progress has been monitored using H-NMR, in FIG. 1 the reaction progress after 1 h is displayed. It is clear that this is still a mixture of the starting Ru-precursor, the ditopic O,N-ligand, the mono O,N-ruthenium complex and the bis O,N-ruthenium complex. FIG. 2 is Reaction progress after 5 h confirming completion of the reaction.
Route B: starting from (SIMes)(2-[(2-methylphenylimino)methyl]phenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl
[0294]
[0295] (SIMes)(2-[(2-methylphenylimino)methyl]phenoxy) (3-2-methylphenyl-5-methyl-inden-1-ylidene)Ru(II)Cl (0.51 mmol) and 2-[(2-methylphenylimino)methyl]phenol (0.52 mmol) and silver(I) oxide (0.32 mmol) were added to a Schlenk flask under argon. Dry THF (20 mL) was transferred to the Schlenk flask and then heated (40° C.) and stirred for a period of 5 h followed by cooling to room temperature. The white precipitate of PCy 3 AgCl (byproduct) and excess of AgO 2 was removed by filtration. The filtrate was collected in a Schlenk flask and the solvent was removed by evaporation under reduced pressure. Addition of 2 mL CH 2 Cl 2 and an excess of cold pentane precipitate the catalyst as a deep red powder, Yield: 85%.
[0296] The reaction mixture was investigated on 1 H and 31 P-NMR, which revealed quantitative transformation to complex 12.
[0297] Characteristic values of 1 H: H—C8: 8.11 ppm (d, 1H). (no 31 P-NMR peak present in the complex)
[0298] Performance of the Catalysts of Present Invention
Example 13: Comparison of Commercial Available Catalyst (N) with Catalyst of this Invention 5A, 6A and 7A for RCM of DEDAM Using Activation a
[0299] FIG. 3 is comparison between commercial catalysts N and 5A, 6A and 7A for the ring-closing metathesis of diethyldiallylmalonate (DEDAM) using activation ( a using catalyst N and chemically activated 5A, 6A and 7A at 0.5 mol %, 20 eq of PhSiCl 3 , substrate loading: 0.41 mmol DEDAM, temperature: 20° C., solvent: 0.60 mL CDCl 3 , conversion determined by 1 H NMR).
[0300] Upon chemical activation, complexes 6A and 7A significantly outperform the commercial complex N at ambient temperature.
Example 14: Effect of Catalyst Loading, Comparison of Commercial Available Catalyst (N) with Newly Developed Catalyst 5A, 6A and 7A for RCM of DEDAM after Activation
[0301] FIG. 4 is comparison between catalysts F and 5A-7A at a 0.1 mol % loading for the RCM of DEDAM ( a using catalyst F and chemically activated 5A-7A at 0.1 mol %, 10 eq of PhSiCl 3 , substrate loading: 0.41 mmol DEDAM, temperature: 20° C., solvent: 0.60 mL CDCl 3 , conversion determined by 1 H NMR).
[0302] At lower catalyst loadings, catalyst lifetime becomes increasingly important. All of the Schiff base-containing catalysts described herein, upon activation by PhSiCl 3 , yield quantitative RCM of DEDAM at a catalyst loading of 0.1 mol % in CDCl 3 , at room temperature with the exception of 5A which requires 60° C. In all cases, the performance of the salicylaldimine systems 5A-7A is superior to that of the commercial available complex F.
Example 15: Comparison of Commercial Available Catalysts (N) with Newly Developed Catalyst for RCM of DEDAM in Protic Solvent MeOH at 50° C.
[0303]
[0000]
TABLE 1
Comparison of TON (Turn Over Number) of reported catalysts and catalyst of this invention
Catalyst
TON a
Ref
8
Grubbs R. et al. Tetrahedron Letters 2005, 46, 2577-2580.
7
Blechert S. et al. Bioorganic & Medicinal Chemistry Letters 2002, 12, 1873-1876.
14
Blechert S. et al. Bioorganic & Medicinal Chemistry Letters 2002, 12, 1873-1876.
19
Raines R. et al. Advanced Synthesis & Catalysis 2007, 349, 395-404.
60
This invention
189
This invention
190
This invention
a TON = Turn over Number; RCM of DEDAM using 0.5 mol % catalyst in MeOH-d 4 at 50° C.
Example 16: Comparison of Commercial Available Catalysts Catalyst of this Invention for RCM of DEDAM-2
[0304]
[0305] It is well known that DEDAM-2 is a difficult substrate to ring-close since it bears a methyl group on each double bond which introduce severe sterical hindering for the catalyst.
[0000]
TABLE 2
Comparison of the catalysts for the reluctance substrate DEDAM-2
Loading
T
Catalyst
(mol %)
(° C.)
TON a,b
0.5
100
44
4A
0.5
100
136
13*
0.5
100
110
14**
0.5
100
37
8A
5
100
7
5
30
3 c
2.5
60
38 d
Mod. H2
a Conversion obtained by 1 H NMR.
b Performed in toluene.
c Performed in CD 2 Cl 2 , data from ref. ( Organometallics 2006, 25, 5740).
d Performed in C 6 D 6 , data from ref. ( Org. Lett. 2007, 9, 1589).
*The catalyst has been prepared according to the description of 4A except that 2-[(2,6-
diisopropylphenylimino)methyl]-4-nitrophenol was applied as ditopic ligand.
**The catalyst has been prepared according to the description of 4A except that
2-[(2,4,6-trimethylphenylimino)methyl]-phenol was applied as ditopic ligand.
[0306] The catalysts of this invention show 100% conversion at a 5 mol % loading. Decreasing the catalyst loading to 0.5 mol % leads to a TON of 136 for 13 and 110 for 14. These results outperform the previous highest TON of 38 for Mod. 112 (modified Hoveyda catalyst) and represent a 20-fold increase compared with the standard Grubbs 2 nd generation catalyst. Therefore, 13 and 14 represent an excellent answer to ‘a major challenge for the design of new more efficient catalysts’.
Example 17: Influence of the Amount of Activator on the Performance of Catalyst 6A of this Invention for RCM of DEDAM
[0307]
[0308] Conditions: 0.5 mol % catalyst, variable eq of PhSiCl 3 , substrate loading: 0.41 mmol DEDAM, temperature: 20° C., solvent: 0.60 mL CDCl 3 , conversion determined by 1 H NMR.
[0309] FIG. 5 is influence of activator amount (from top to bottom the amount decreases from 50 eq. to 0.5 eq PhSiCl 3 ) on the catalytic performance for RCM of DEDAM.
[0310] It is clear that no longer an excess of activator is required to activate the catalysts of this invention and clearly outperforms the systems described in EP 1 577 282; EP 1 757 613. Moreover, an excess of activator is not immediately decomposing the catalyst demonstrating the robustness of the systems.
Example 18: Monitoring Ring Opening Metathesis Polymerization (ROMP) of Dicyclopentadiene (DCPD)
[0311] The required amount was of catalyst was dissolved in a minimum amount of dichloromethane (CH 2 Cl 2 ), and thereafter added to 80 g of DCPD which contains the required amount of activator (here PhSiCl 3 was used). The mixture was stirred and the polymerization reaction was monitored as a function of time starting at 20° C. by a thermocouple which was placed inside the reaction mixture to collect the temperature data. catalyst/DCPD: 1/60000.
[0312] The catalysts used are 4A, 8A, 9A and 12. For catalyst 4A and 8A the catalyst/activator=1/5 while for the 9A and 12 the catalyst/activator=1/0.5.
[0313] FIG. 6 is ROMP of DCPD using catalyst 4A, 8A, 9A and 12 of this invention.
[0314] A ruthenium catalysts Verpoort (WO 03/062253) and Telene (WO 2011/009721 A1) comprising one and two bidentate Schiff base ligand respectively have been used as a reference catalyst; see table 3.
[0000]
[0315] It is clear that the catalysts of this invention outperform the catalysts described in WO 2011009721 and (WO 03/062253; Tetrahedron Lett., 2002, 43, 9101-9104; (b) J. Mol. Catal. A: Chern., 2006, 260, 221-226; (c) J. Organomet. Chem., 2006, 691, 5482-5486).
[0316] Introducing extra groups, substituents on the indenylidene part of the catalysts result in more steric strain in the molecule which promotes the initiation of the catalyst once it is activated.
[0000]
TABLE 3
Comparison between existing catalyst (T and VP) and catalysts
of this invention (4A, 8A, 9A and 12) for the ROMP of DCPD
DCPD/
T max
Tg 1
Tg 2
Catalyst
Latency
Cocatalyst
Cl/Ru
Ru
(° C.)
(° C.)
(° C.)
9A
fair
PhSiCl 3
0.5
50000
230
170
179
8A
Good
PhSiCl 3
5
50000
223
168
175
4A
Good
PhSiCl 3
5
50000
195
160
169
12
Good
PhSiCl 3
0.5
50000
223
171
179
T*
Good
PhSiCl 3
2
30000
217
171
178
VP*
Good
PhSiCl 3
45
30000
215
156
169
*for reference only
[0317] All catalysts of this invention show an excellent latency towards DCPD (with 9A a fair latency), they are inactive at room temperature. All catalysts of this invention show an improved stability and are superior to other catalysts used as a reference (T and VP), see table 3.
[0318] Upon chemical activation, the catalyst of type I-I, e.g. 12 and 9A, according to the present invention, demonstrate an increased initiation compared to the reference catalyst (T and VP) because it requires only less than 1 equivalent of PhSiCI 3 to generate a highly active system. When the ROMP of DCPD is catalysed by the chemically activated VP complex (reference), under the same conditions (less than 1 equivalent of PhSiCI 3 ) a low catalytic activity was observed.
[0319] Moreover the ratio catalyst/monomer is increased with 66% compared to the reference catalysts (T and VP) which clearly stress out their superior performance of the catalysts of the present invention
Example 19: Monitoring Ring Opening Metathesis Polymerization (ROMP) of Cyclo-Octadiene (COD)
[0320]
[0321] After charging an NMR tube with the appropriate amount of catalyst dissolved in deuterated solvent (CDCl 3 ), COD was added. The polymerization reaction was monitored as a function of time at 20° C. by integrating olefinic 1 H-signals of the formed polymer (5.38-4.44 ppm) and the consumed monomer (5.58 ppm).
[0322] catalyst/COD: 1/3000, catalyst concentration: 0.452 mM.
[0000]
TABLE 4
ROMP of COD (3000 equiv).
Catalyst/
T
PhSiCl 3 (equiv) a
[° C.]
time [min]
Conv. [%]
cis [%] b
TOF (h −1 )
G2 [c] /0
RT
30
100
13
6 000
F/0
RT
45
100
60
600 [d]
N/0
RT
300
100
70
600
VP/20
RT
10
100
9
18 000
6A/5
RT
5
100
5
36 000
7A/5
RT
5
100
20
36 000
a Conditions: Catalyst concentration: 0.453 mM, solvent: CDCl 3 , temperature: 20° C., conversion determined by 1 H NMR.
b Percent olefin with cis configuration in the polymer backbone; ratio based on data from 1 H and 13 C NMR spectra ( 13 C NMR spectroscopy: δ = 32.9 ppm allylic carbon trans; δ = 27.6 ppm allylic carbon cis).
[c] see Nature 2007, 450, 243-251.].
[d] monomer/catalyst = 300.
[0323] The catalysts of this invention are superior compared with other catalysts, the obtained TON is at least 2 times higher compared with catalyst VP and even 6 times higher or more compared with the other catalysts.
Example 20: In-Situ Activation Using TiCl 4 /iPrOH of Catalyst 4A for the ROMP of Dicyclopentadiene (DCPD)
[0324] This example demonstrates the possibility of in-situ activation of the catalysts of this invention. Here 40 g of DCPD in which TiCl 4 is present is mixed with 40 g of DCPD in which iPrOH and the catalyst are present. In the total DCPD mixture (80 g) a thermocouple is place to follow the temperature increase during the polymerization. From the plot it follows that all monomers are converted since a high temperature of 200° C. is reached. The ratio DCPD/catalyst/Lewis acid-alcohol=30000/1/10-10 and 30000/1/5-5.
[0325] FIG. 7 is ROMP of DCPD using in-situ activation of catalyst 4A.
[0326] This excellent results confirms that all kinds of combinations between Lewis acids and RYH molecules can be used for in-situ activation of the catalysts of this invention as described in the description
Example 21: Removal of the Residual Ruthenium (11B) from the Reaction Mixture
[0327] Subsequent to the RCM or cross-metathesis applications, in order to remove the residual ruthenium in final metathesis products, the reaction mixtures were passed through silica gel (3 g per 0.006 mmol of catalyst 11B) with different eluents (see Table 5). The silica gel can also be introduced directly into the reaction mixture. Complete decolorization was observed within 10 minutes of intense stirring. The ruthenium content of some selected metathesis products were determined by ICP-MS analysis. Using a basic filtration through silica gel, the ruthenium content of the products with an initial ruthenium content of 500 ppm were reduced to 1 ppm.
[0000]
TABLE 5
Residual ruthenium from reaction mixtures after column chromatography.
Ru content
Entry
Product
Eluent
(ppm)
1
CH 2 Cl 2 Toluene
1 1
2
Self-metathesis product of
CH 2 Cl 2
1
methy-10-undecenoate
Toluene
3
Example 22: Cross Metathesis of FAME (Fatty Acid Methyl Esters) Using Catalyst 4A
[0328] 50 ml of a methyl ester mixture (consisting of 92.0% methyl oleate and 2.9% Methyl linoleate, percentages are based on a calibrated GC-Method) in the presence of 150 ppm of the catalyst (4A) is heated at 50° C. for 1 hour. After completion of the reaction 27% dimethyldiesters and 24% of 9-octadecene is obtained.
|
Metal catalyst compounds are disclosed. The catalyst compound are represented by the formula (I-II and VII): wherein M is a Group 8 metal; X is an anionic ligand; L is a neutral two electron donor ligand; K 2 (A-E) is a ditopic or multitopic ligand. Also disclosed is an easy applicable catalyst synthesis and the application in different olefin metathesis processes, e.g. Reaction Injection Molding (RIM), rotational molding, vacuum infusion, vacuum forming, process for conversion of fatty acids and fatty acid esters or mixtures thereof, in -olefins, dicarboxylic acids or dicarboxylic esters, etc.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a ferroelectric liquid crystal material. More particularly it relates to a ferroelectric liquid crystal composition comprising smectic liquid crystal compound(s) and optically active compound(s) and having high-speed response properties and a light switching element using the same.
2. Description of the Related Art
Liquid crystal compounds have been broadly used as a material for liquid crystal elements, but most of such liquid crystal display elements are of TN display mode, and as liquid crystal materials, those belonging to nematic phase have been used.
Since TN display mode is non-emissive, it has specific features that eyes are not tired and power consumption is small, but on the other hand, it has drawbacks that the response is slow and the display is not seen depending on the angle of view. Thus, the mode has recently been being turned toward a direction of making the best use of its characteristics as flat display, and in particular, high-speed response properties and a broad angle of view have been required.
Various improvements in liquid crystal materials in response to such requirements have been attempted. However, as compared with other emissive displays such as electroluminescence display, plasma display, etc., TN display mode is considerably inferior in the aspect of the response time and the breadth of angle of view.
In order to make the best use of the specific features of liquid crystal display elements such as non-emissive mode and low power consumption and also secure response properties matching emissive display, development of a novel liquid crystal display mode in place of TN display mode has been indispensable. As one of such attempts, a display mode utilizing the light switching phenomenon of ferroelectric liquid crystals has been proposed by N. A. Clark et al (see Appl. Phys. Lett., vol. 36, p. 899 (1980)).
The presence of ferroelectric liquid crystals has been announced by R. B. Meyer et al for the first time (see J. Phys. vol. 36, p. 69 (1975)), and the phases of the crystals include chiral smectic C phase, chiral smectic I phase, chiral smectic F phase, chiral smectic G phase and chiral smectic H phase (hereinafter abbreviated to Sc* phase, S I * phase, S F * phase, S * G phase and S * H phase, respectively in the aspect of liquid crystal structure.
Various specific features are required for ferroelectric liquid crystal materials used for practically usable ferroelectric liquid crystal display elements, but at present, there is no single compound which satisfies all the specific features; hence it is necessary to use ferroelectric liquid crystal compositions obtained by mixing some liquid crystal compounds or liquid crystal compounds with non-liquid-crystal compounds.
Further, the ferroelectric liquid crystal compositions are not limited to those consisting only of ferroelectric liquid crystal compounds, but it has been reported that using compound(s) or composition(s) each exhibiting achiral smectic C, F, G, H, I phase or the like phase (hereinafter abbreviated to Sc phase or the like) as base substance(s), at least one compound exhibiting ferroelectric liquid crystal phases is mixed with the above compound(s) or composition(s) to constitute a ferroelectric liquid crystal composition as a whole (see Japanese patent application laid-open No. Sho 61-195187/1986). Further, it has also been reported that using compound(s) or composition(s) each exhibiting S c phase or the like as base substance(s), at least one compound which is optically active but exhibits no ferroelectric liquid crystal phase is mixed with the above compound(s) or composition(s) to constitute a ferroelectric liquid crystal composition as a whole (see Mol. Cryst. Liq. Cryst., 89, 327 (1982)).
In a brief summary of these facts, it is seen that when at least one optically active compound, irrespective of whether or not the compound exhibits ferroelectric liquid crystal phase, is mixed with a base compound, it is possible to constitute a ferroelectric liquid crystal composition.
A smectic liquid crystal mixture comprising the above-mentioned base substance exhibiting at least one of achiral S c phase or the like and having at least one of S c phase or the like will hereinafter referred to as "smectic base mixture".
As such smectic base mixture, liquid crystal mixtures exhibiting S c phase within a broad temperature range including room temperature are practically preferred. As a component of the smectic base mixture, some compounds selected from among liquid crystal compounds of e.g. phenylbenzols, Schiff's bases, phenylpyrimidines, 5-alkyl-2-(4-alkoxyphenyl)pyrimidines, etc. have been used.
For example, Japanese patent application laid-open No. Sho 61-291679/1986 and PCT International publication No. WO 86/06401 disclose a ferroelectric liquid crystal obtained by mixing a 5-alkyl-2-(4-alkoxyphenyl)pyrimidine with an optically active compound, and the former publication discloses that use of a ferroelectric smectic liquid crystal material using the above pyrimidine derivative as a smectic base mixture makes it possible to shorten the response time of light switching elements. Further the above former publication also discloses that a ferroelectric liquid crystal material consisting of a 5-alkyl-2-(4'-alkylbiphenylyl-4)pyrimidine, the above 5-alkyl-2-(4-alkyloxyphenyl)pyrimidine and an optically active compound is also effective for improving response properties.
However, as compared with liquid crystal displays of other modes such as emissive display, a further improvement in the response properties has been desired for the above liquid crystal display.
On the other hand, one more problem desired to solve, together with the improvement in the response properties is to reduce the temperature-dependency of the response time. Current ferroelectric liquid crystal materials have a large temperature-dependency of the response time so that a cross talk phenomenon often occurs due to environmental temperature change to notably reduce the display quality of the display.
Thus, a ferroelectric liquid crystal material having a small temperature-dependency of the response time together with high-speed response properties has been earnestly desired.
SUMMARY OF THE INVENTION
As apparent from the foregoing, a first object of the present invention is to provide a ferroelectric liquid crystal composition having high-speed response properties and also a small temperature-dependency of the response time, and a second object thereof is to provide a light-switching element using the above liquid crystal composition and having high-speed response properties.
The present inventors have made extensive research in order to further improve the invention disclosed in the above Japanese patent application laid-open No. Sho 61-291679/1986. As a result, we have found that when liquid crystal compounds are combined together as shown below, a ferroelectric liquid crystal composition having high-speed response properties and also a small temperature-dependency of the response time is obtained, and have completed the present invention.
The present invention in the first aspect resides in (1) a ferroelectric liquid crystal composition comprising the following three liquid crystal components A, B and C, the respective proportions of the components A, B and C being 10 to 70% by weight, 10 to 50% by weight and 10 to 40% by weight based on the total weight of these components, respectively:
liquid crystal component A:
at least one compound selected from compounds expressed by the formula ##STR6## wherein R 1 and R 2 represent the same or different alkyl group of 1 to 18 carbon atoms and compounds expressed by the formula ##STR7## wherein R 3 and R 4 represent the same or different alkyl group or alkoxy group each of 1 to 18 carbon atoms;
liquid crystal component B:
at least one compound selected from compounds expressed by the formula ##STR8## wherein R 5 represents an alkyl group of 1 to 18 carbon atoms; n represents an integer of 0 to 10; and * indicates an asymmetric carbon atom; and
liquid crystal component C:
at least one compound selected from compounds expressed by the formula ##STR9## wherein R 6 represents an alkyl group or an alkoxy group each of 1 to 18 carbon atoms and * indicates an asymmetric carbon atom and compounds expressed by the formula ##STR10## wherein R 7 represents an alkyl group or an alkoxy group each of 1 to 18 carbon atoms and * indicates an asymmetric carbon atom.
The present invention in the second aspect resides in
a light switching element containing
a ferroelectric liquid crystal composition comprising the following three liquid crystal components A, B and C, the respective proportions of the components A, B and C being 10 to 70% by weight, 10 to 50% by weight and 10 to 40% by weight based on the total weight of these components, respectively:
liquid crystal component A:
at least one compound selected from compounds expressed by the formula ##STR11## wherein R 1 and R 2 represent the same or different alkyl group of 1 to 18 carbon atoms and compounds expressed by the formula ##STR12## wherein R 3 and R 4 represent the same or different alkyl group or alkoxy group each of 1 to 18 carbon atoms;
liquid crystal component B:
at least one compound selected from compounds expressed by the formula ##STR13## wherein R 5 represents an alkyl group of 1 to 18 carbon atoms; n represents an integer of 0 to 10; and * indicates an asymmetric carbon atom; and
liquid crystal component C:
at least one compound selected from compounds expressed by the formula ##STR14## wherein R 6 represents an alkyl group or an alkoxy group each of 1 to 18 carbon atoms and * indicates an asymmetric carbon atom and compounds expressed by the formula ##STR15## wherein R 7 represents an alkyl group or an alkoxy group each of 1 to 18 carbon atoms and * indicates an asymmetric carbon atom.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a chart illustrating the concentration dependencies of the response time of the respective mixture systems of a ferroelectric liquid crystal composition A of the present invention with a smectic base composition B, the proportions of A to B being varied.
FIG. 2 shows a chart illustrating the respective temperature dependencies of the response time of ferroelectric liquid crystal compositions C and D.
FIG. 3 shows a chart illustrating the respective temperature dependencies of the response time of ferroelectric liquid crystal compositions C and E.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The compounds of the formulas (I) and (II) constituting the above component (A) used in the present invention are achiral compounds, but have S c phase or the like and also have a very low viscosity; hence they are very useful as a smectic base mixture. The usefulness of the compounds has already been described by the present inventors in Japanese patent application laid-open No. Sho 61-291679/1986, and the compounds are also very effective as a component of the ferroelectric liquid crystal composition aimed in the present invention.
Similarly, the compound of the formula (III) costituting the component (B) is a halogen-containing heterocyclic compound previously applied for patent, the invention having been made by the present inventors (Japanese patent application No. Sho 61-10578/1986). The spontaneous polarization value of the compound is not so large, but the compound has Sc* phase within a very low temperature range; hence it is useful as a base liquid crystal compound for low temperatures. Further, as will be described later, it has been found by the present inventors for the first time that the compound also has an effect of reducing the temperature dependency of the response time of ferroelectric liquid crystal compositions.
Similarly, the compounds of the formulas (IV) and (V) constituting the above component (C) are halogen-containing optically active liquid crystal compounds previously applied for patent, the invention having been made by the present inventors, and already laid open (Japanese patent applica&ion laid-open No. Sho 61-210056/1986) and has a very large spontaneous polarization value. Compounds having among the spontaneous polarization value (abbreviated to Ps), the viscosity (abbreviated to η) and the response time (abbreviated to τ) of ferroelectric liquid crystal materials, a relationship of ##EQU1## wherein E represents an intensity of electric field impressed to a liquid crystal cell, and having a low viscosity and also a large spontaneous polarization value have been desired. The compounds of the formulas (IV) and (V) constituting the component (C) play such a role in the ferroelectric liquid crystal composition. Further, it has also been found by the present inventors that these compounds also have an effect of reducing the temperature dependency of the response time of ferroelectric liquid crystal compositions.
The present inventors have examined the respective proportions of the components A, B and C in which proportions a liquid crystal composition having aimed superior specific features is obtained by making the best use of the respective specific features of the components A, B and C. As a result, as described above, the proportion of the component A is in the range of 10 to 70% by weight, that of the component B is in the range of 10 to 50% by weight and that of the component C is in the range of 10 to 40% by weight.
The present invention is based on a combination of the respective superior specific features of the liquid crystal compounds of the above formulas (I) to (V). The superior specific features of the respective liquid crystal components will be described below in more detail.
The compounds of the formulas (I) and (II) constituting the liquid crystal component A are both achiral compounds, but the compound of the formula (I) has Sc phase within a low temperature region (e.g. Cr 28 Sc 47 S A 58 N 66 I so in the case of the formula (I) wherein R 1 =C 6 H 13 -- and R 2 =C 8 H 17 --), whereas the compound of the formula (II) has Sc phase within a high temperature region (e.g. Cr 58 Sc 134 S A 144 N 157 I so in the case of the formula (II) wherein R 3 =C 7 H 15 -- and R 4 =C 8 H 17 --). Thus, by combining the compound of the formula (I) with that of the formula (II), a smectic base mixture having Sc phase over from a low temperature region to a high temperature region is obtained.
The superior specific features of the compound having this skeleton have already been described by the present inventors in Japanese patent application laid-open No. Sho 61-291679/1986, and since it has a very low viscosity, it also plays an important role as a smectic base mixture in the ferroelectric liquid crystal composition aimed in the present invention.
FIG. 1 shows the concentration dependency of the response time of a mixture system of a ferroelectric liquid crystal composition A (phase transition points: ˜Sc* 55 S A 69N* 76 I so ) composed of chiral smectic liquid crystal compounds with a smectic base composition B (phase transition points: Cr 4 Sc 65 S A 79 N 90 I so ) composed of achiral liquid crystal compounds. The measured temperature is 25° C., the intensity of electric field is 5 V/μm and the proportions of the respective compositions are as follows: ##STR16##
As seen from FIG. 1, as the composition B is added to the composition A, the response becomes faster, and the effectiveness of addition of the composition B is observed as far as 60% by weight in terms of the concentration of the composition B. However, beyond this concentration, the response time becomes slow; hence such higher concentrations are not practical. In view of the fact that the use object of the compounds of the component A consists in use as a smectic base compound, the concentration of the liquid crystal component A is preferred to be in the range of 70% by weight or less.
The compound of the formula (III) constituting the liquid crystal component B is a chiral compound and its spontaneous polarization value is not so large, but the compound has Sc* phase within a very low temperature region (e.g. Cr 7 Sc* 31 S A 33 I so in the case of the formula (III) wherein R 5 =C 6 H 13 -- and n =5); hence the component B also plays an important role as a liquid crystal base compound like the liquid crystal base component A in the ferroelectric liquid crystal composition position aimed in the present invention.
The compound having this skeleton is a compound previously applied for patent, the inventors of the application being the present inventors (Japanese patent application No. Sho 61-10578/1986). As a result of various examinations made later, a surprising effect of the compound has been found by the present inventors for the first time.
FIG. 2 shows the respective temperature dependencies of the response time of the following ferroelectric liquid crystal compositions C and D:
Composition C consists of the above-mentioned smectic base composition B and a chiral smectic liquid crystal compound A shown below (phase transition points of the C: ˜Sc* 62 Sc 74 N* 87 I so ).
Composition D consists of the smectic base composition position B, a chiral smectic liquid crystal compound A shown below and chiral smectic liquid crystal compounds B and C each of the formula (III) and shown below (phase transition points of the D: ˜Sc* 53 S A 70 N* 75 I so ).
The intensity of electric field is 5 V/μm and the respective proportions of the compositions C and D are as follows: ##STR17##
As seen from FIG. 2, when the composition C is compared with the composition D, there is a tendency that the response times of the two compositions are to a similar extent within a temperature region of 20° C. to 40° C. i.e. the vicinity of room temperature to higher temperatures, whereas the response time of the composition D is faster than that of the composition C within a lower temperature region of 0° to 20° C. The ratio of the response time at 0° C. to that at 40° C. is about 10 in the case of the composition C, while it is about 6.9 in the case of the composition D, that is, the temperature dependency of the composition C is very small. The difference between the composition C and the composition D consists only in that a moiety (40% by weight) of the smectic base composition B (80% by weight) in the composition C is replaced by the compound B and the compound C each of the formula (III) in the composition D. Thus, the fact that the temperature dependency of the response time of the composition D is better than that of the composition C is considered to be affected by the compound B and the compound C. Namely, it is seen that use of the compound of the formula (III) affords a ferroelectric liquid crystal composition having a small temperature-dependency of the response time. Since the component B compound has Sc* phase within a very low temperature region, the upper limit temperature of Sc* phase lowers when the compound is used too much (for example, comparison of the upper limit temperature of Sc* of composition C with that of composition D); hence such excess quantity is undesirable. Thus, the concentration range of the liquid crystal component B in the ferroelectric liquid crystal composition aimed in the present invention is preferably 50% by weight or less.
The compounds of the formulas (IV) and (V) as the liquid crystal component C are chiral compounds previously applied for patent in Japan by the present applicants and already laid open (Japanese patent application laid-open No. Sho 61-210056/1986), which compounds exhibit Sc* phase within a high temperature region and also have a very large spontaneous polarization value (for example, in the case of a compound of the formula (IV) wherein R 6 =C 8 H 17 O--, the phase transition points: Cr 52 Sc* 104 N* 109 `I so , Ps: 132 nC/cm 2 (T-Tc=-30° C.), and in the case of a compound of the formula (V) wherein R 7 =C 7 H 15 O--, the phase transition points: Cr 69 Sc* 95 S A 106 I so , Ps: 93 nC/cm 2 (T-Tc=-30° C.). Thus, the above compounds are important ones playing a role of developing high-speed response properties and also improving the upper limit temperature of Sc* phase of the composition in the ferroelectric liquid crystal composition aimed in the present invention. Further it has been found by the present inventors for the first time that these compounds have a surprising effect of reducing the temperature-dependency of the response time of ferroelectric liquid crystal compositions as in the case of the compound of the formula (III) as the liquid crystal component B. FIG. 3 shows a chart illustrating the respective temperature-dependencies of the response time in the above-mentioned ferroelectric liquid crystal composition C and a ferroelectric liquid crystal composition E (phase transition points: ˜Sc* 65 S A 74 N* 86 I so ) consisting of the above-mentioned smectic base composition B and a chiral smectic liquid crystal compound D which is a compound of the formula (IV). The intensity of the electric field is 5 V/μm. The proportions of the composition E are as follows: ##STR18## Further, the spontaneous polarization value at 25° C. of the composition C was 2 nC/cm 2 and that of the composition E was 5 nC/cm 2 . As apparent from FIG. 3, the response time of the composition E is faster than that of the composition C and the temperature-dependency of the composition E is also less than that of the composition C (the ratio of the response times at 0° C. and 40° C. is about 10 in the case of the composition C and about 7.3 in the case of the composition E). The difference between the composition C and the composition E corresponds to the difference between the chiral smectic compound A and the chiral smectic compound D, and it has been found that by using the compound of the formula (IV), a ferroelectric liquid crystal composition having high-speed response properties and yet a small temperature-dependency of response time is obtained. Further, as apparent from Example 7 mentioned later, the compound of the formula (V) also has the same effectiveness as that of the compound of the formula (IV); hence it is anticipated that by using the compounds of the formula (IV) and the formula (V), a ferroelectric liquid crystal composition having a small temperature-dependency of response time may be obtained. Taking into account the respective concentration ranges of the liquid crystal component A and the liquid crystal component B, and also in view of the usefulness of the liquid crystal component C, the concentration range of the liquid crystal component C in the ferroelectric liquid crystal composition aimed in the present invention is preferred to be 40% by weight or less.
The respective proportions of the liquid crystal components A, B and C in which proportions a ferroelectric liquid crystal composition having superior specific features, aimed in the present invention is obtained making the best use of the respective specific features of these components as described above are as follows:
liquid crystal component A: 10 to 70% by weight,
liquid crystal component B: 10 to 50% by weight, and
liquid crystal component C: 10 to 40% by weight.
Next, the foregoing will be described by way of examples.
A ferroelectric liquid crystal composition F consisting of Sc compounds as the liquid crystal component A of the present invention and known chiral smectic liquid crystal compounds and having the following proportions was prepared: ##STR19##
The phase transition points of this composition were as follows: ##STR20##
The Ps at 25° C. was 4.7 nC/cm 2 , the tilt angle was 21° and the length of the helical pitch of Sc* phase was 5 μm.
This liquid crystal composition F was filled in a cell of 2 μm thick provided with electrodes subjected to aligning treatment and a square wave of peak to peak (hereinafter abbreviated to V pp ) of 20 V and 100 Hz was impressed to measure the response time. As a result, the time was 350μ sec at 25° C. Further, the response time at 0° C. and 40° C. were 2m sec and 200μ sec, respectively, and the ratio of the response times at 0° C. and 40° C. was 10.
Further, a ferroelectric liquid crystal composition G consisting of Sc compounds as the liquid crystal component A and known chiral smectic liquid crystal compounds and having the following proportions was prepared: ##STR21##
The phase transition points of this composition G were as follows: ##STR22##
The Ps at 25° C. was 5.9 nC/cm 2 , the tilt angle was 24° and the length of the helical pitch of Sc* phase was 3 μm.
This liquid crystal composition G was filled in the same cell as in the case of the composition F and the response time was measured to give 230 μ at 25° C. Further, the response times at 0° C. and 40° C. were 1.9μsec and 130μ sec, respectively and the ratio of the response times at 0° C. and 40° C. was 14.6.
On the other hand, a ferroelectric liquid crystal composition H comprising the liquid crystal components A, B and C of the present invention as shown below was prepared: ##STR23##
The phase transition points of this composition H were as follows: ##STR24##
The Ps at 25° C. was 8 nC/cm 2 , the tilt angle was 24° and the length of the helical pitch of Sc* phase was 3 μm.
This liquid crystal composition H was filled in the same cell as in the case of the above composition F and the response time was measured to give 150μ sec at 25° C. Further, the response times at 0° C. and 40° C. were 600μ sec and 80μ sec, respectively, and the ratio of the response times at 0° C. and 40° C. was 7.5.
As apparent from the foregoing, the ferroelectric liquid crystal composition comprising the liquid crystal components A, B and C of the present invention has far superior high-speed response properties and a small temperature-dependency of response time.
Examples 1 to 11
The present invention will be described in more detail by way of Examples, but it should not be construed to be limited thereto.
In addition, the spontaneous polarization value (Ps) was measured according to Sawyer-Tower method, and the helical pitch (P) was sought by using a cell of about 200 μm thick subjected to homogeneous alignment and directly measuring the distance between dechiralization lines corresponding to the helical pitch under a polarizing microscope. The tilt angle (θ) was sought by impressing a sufficiently high electric field higher than the critical electric field to a cell subjected to homogeneous alingment to make the helical structure extinct, followed by inverting its polarity and observing the angle (corresponding to 2θ) at which the extinction position was transferred, under crossed nicols.
The response time was sought by filling the respective compositions in a cell subjected to aligning treatment and having a distance between electrodes of 2 μm, impressing a square wave of V pp of 20 V and 100 Hz and observing the change in the intensity of transmitted light at that time.
In addition, the compositions of Examples include those containing a chiral compound for extending the pitch of Sc* phase besides the above-mentioned respective components A, B and C, but such chiral compound does not damage the specific features of the ferroelectric liquid crystal composition aimed in the present invention; hence no problem is raised.
Table 1 shows the component proportions of the ferroelectric liquid crystal compositions of the present invention in Examples 1 to 11 and Table 2 shows the values of their specific features. Further, the respective proportions in Table 1 are of percentage by weight.
TABLE 1 Example No. Component Formula Compound 1 2 3 4 5 6 7 8 9 10 11 A I ##STR25## 18 17.5 17.5 19.3 19.3 17.5 17.5 18 18 15 I ##STR26## 12 12 15 12 10 I ##STR27## 5 5 5.5 5.5 5 5 I ##STR28## 6 10 10 11 11 10 10 6 6 5 I ##STR29## 6 6 6 5 II ##STR30## 10 10 11 11 10 10 10 10 II ##STR31## 12 5 12 15 12 10 II ##STR32## 7.5 7.5 8.2 8.2 7.5 7.5 II ##STR33## 6 6 6 5 B III ##STR34## 5 10 20 10 15 III ##STR35## 5 10 10 10 5 10 5 5 III ##STR36## 10 15 15 15 15 15 20 5 5 III ##STR37## 20 5 C IV ##STR38## 20 15 15 20 20 20 5 20 IV ##STR39## 5 20 IV ##STR40## 10 20 15 V ##STR41## 15 Others ##STR42## 5 5 5 ##STR43## 5 5
TABLE 2__________________________________________________________________________ Example No.Specific features 1 2 3 4 5 6 7 8 9 10 11__________________________________________________________________________Phase transition points (°C.)C.sub.r → S.sub.C * -6 -22 -17 -18 -20 -21 -20 -5 -10 -7 -9S.sub.C * → S.sub.A 56 54 57 55 58 56 55 53 55 51 55S.sub.A → N* 70 67 70 67 69 68 64 65 72 67 72N* → I.sub.SO 74 72 77 74 76 73 68 71 75 74 78Ps* (μm) 8 12 8 9 8 9 9 7 9 9 4Tilt angle* (°) 25 24 25 25 25 24 26 21 25 21 21Helical pitch* (μm) 2 3 3 2 4 5 2 2 3 2 2Response time (μsec)40° C. 100 100 100 125 100 100 130 125 130 130 20025° C. 160 150 175 170 150 150 170 175 220 200 350 0° C. 750 700 750 900 750 700 900 900 800 900 1400Temp. dependency of 7.5 7 7.5 7.2 7.5 7 6.9 7.2 6.2 6.9 7response time40˜0° C.__________________________________________________________________________ (Note) *value at 25° C.
|
A ferroelectric liquid crystal composition comprising smectic liquid crystal compound(s) and optically active compound(s) and having high-speed response properties and a light switching element containing the same are provided, which composition comprises the following three liquid crystal components A, B and C, the respective proportions thereof being 10 to 70%, 10 to 50% and 10 to 40% each by weight based on the total weight of these components, respectively:
liquid crystal component A:
at least one compound selected from compounds of the formula ##STR1## wherein R 1 and R 2 each are 1-18C alkyl, and compounds of the formula ##STR2## wherein R 3 and R 4 each are 1-18C alkyl or alkoxy; liquid crystal compound B:
at least one compound of the formula ##STR3## wherein R 5 is a 1-18C alkyl, n is an integer of 0 to 10 and * indicates asymmetric carbon; and
liquid crystal component C:
at least one compound selected from compounds of the formula ##STR4## wherein R 6 is 1-18C alkyl or alkoxy and * is as defined above; and compounds of the formula ##STR5## wherein R 7 is 1-18 alkyl or alkoxy and * is as defined above.
| 2
|
REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional Patent Application Ser. No. 62/201,861, filed Aug. 6, 2015 and U.S. Provisional Patent Application Ser. No. 62/265,073, filed Dec. 9, 2015, the entire content of both of which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates generally to the Internet, including the mobile Internet. In particular, techniques and methods are disclosed that enable a search engine app on a mobile device to display true three-dimensional results, allowing the user of the search engine to navigate in a three dimensional site or circumnavigate a three dimensional object and interact with the same.
BACKGROUND OF THE INVENTION
[0003] According to Wikipedia, “Competition for the . . . mobile search market promises to be fierce, thanks to the large . . . online ad market and strong pushes by portals.” In addition to native search engines, such as the Safari for the iOS systems, major search engines such as Google and Baidu in China have introduced downloadable applications to extend their search engine businesses. Currently all mobile search engine Apps (“2D Search Apps”) present results in two dimensions, which may include text, images or video. There is a need, however, to present certain results in three-dimensions, for example, a building, a store or a three dimensional object such as a 3D car model.
[0004] It is believed that having this capability will increase the attractiveness of search results to users, as they can have a three-dimensional experience, either in viewing an object or in entering and interacting with a scene. For the same reason, it is believed that owners of conventional two-dimensional websites may also want to convert their websites from two to three dimensional, so that when presented to the users, their websites will be more attractive.
SUMMARY OF THE INVENTION
[0005] This invention resides in a method transforming an existing two-dimensional search engine app (“2D Search App”), into a search engine that can present three-dimensional results (“3D Search App”), as well as a system for the production of the three-dimensional contents. The conversion process rapid, the 3D Search App adds no more than 10 MB to existing 2D Search Apps, and can be released as a normal version upgrade.
[0006] The technology, which allows the presentation of 3D sites and objects on a mobile device, comprises a client in the form of a mobile App in communication with a central server. The client is capable of performing 3D rendering in accordance with the instructions received from the server. The client also interacts with the server to send and retrieve other data, including requests, instructions and text, images or video.
[0007] The server is capable of converting 3D models into instructions which can be sent to the client, thereby allowing the client to reproduce the 3D model in the mobile device for viewing. These 3D models may be imported from model building applications such as 3D Max or Sketch Up, or by way of a proprietary template-based customization backroom.
[0008] The invention finds application in a wide range of fields. As one example, a fashion brand which currently has an online store may wish to present its search result in a 3D store which the user can enter and view products which are available. In this case, the fashion brand may select the standard 3D Option. A 3D Backroom will automatically create the 3D store (size of store to be selected by the brand) and populate the store with products of the brand in synchronization with its online store.
[0009] As another example, a restaurant may wish to present its search result in 3D which highlights its environment and settings. In this case, it may wish to modify certain standard models to display logo, decoration or images not contained in its 2D website. This can mostly be accomplished in the customer version of the 3D Backroom. Or a hotel may wish to present its search result in 3D to highlight the various facilities it has, and permits the user to view its various rooms. In this case, the hotel may need to utilize expert 3D model construction services to construct a customized 3D model for the various areas that the hotel wishes to exhibit.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a diagram that illustrates the flow of information enabling a 3D search result according the invention; and
[0011] FIG. 2 are flowcharts that illustrate site registration (right flowchart) and search engine operations (left flowchart).
DETAILED DESCRIPTION OF THE INVENTION
[0012] This invention has two primary components: A first part that enables a 2D Search App to Display 3D results, and a second part involving the production of the 3D results.
Part 1—Enabling a 2D Search App to Display 3D Results
[0013] The elements involved in this aspect of the enabling process are as follows, wherein the numerical references may be found primarily in FIG. 1 :
[0014] 1) A downloadable App 101 capable of displaying 3D results (the “Client”), either as a 3D object 105 at which users can view from different angles, or as a 3D site 106 in which users can move about freely. In both cases, users can further interact with the 3D object or 3D site to obtain additional 2D or 3D information.
[0015] 2) Server 200 connected to the Client 101 can send instructions in real time to construct or erect the various 3D objects or 3D sites, as well as transmitting rules for further interactions and receiving requests or reports from the Client.
[0016] 3) A Software Application or Development Kit (“SDK”) 101 which allows the Client to be attached to, and to interact with, any 2D Search App (“Host App” 100 ). Once the Client 101 is attached to Host App 100 , the Host App can define the circumstances under which the Client is invoked by the user, and conditions for the user to return to the Host App. The 2D Search App can then introduce a version upgrade with the Client as an attachment.
[0017] 4) A Backroom residing on the Server 200 receives information or instructions from potential customers for the construction of 3D models or sites, so that such 3D models or sites can be displayed in 3D with the correct information to search engine users. Due to the potential variety of needs from customers, certain level of customization may require manual assistance or participation by expert Backroom operators.
[0018] 5) An Application Programming Interface 202 (“API”) which connects the Backroom with the backroom of the 2D Search App (or Host App), allowing the exchange of information, including whether or not a particular website contains 3D results which could be displayed by invoking the Client, and whether or not a customer desires to construct a 3D website (in which case, the backroom of the 2D Search App will refer the customer to the 3D Backroom.
[0019] In order to transform a 2D Search App into a 3D Search App, all that is required is for the 2D Search App to utilize the SDK to attach the Client to its 2D Search App (which becomes the Host App), modify the 2D Search App to set the conditions for invoking the Client, and publish the new hybrid App as an update version to its current 2D Search App.
Part 2—The Production of 3D Results
[0020] The elements involved in the process relating to the production of 3D results to be displayed in the 3D Search App are as follows:
[0021] 1) Backroom 203 (“Host Backroom”) for the 2D Search App (or Host App) which is used for interacting with potential customers 302 interested in placing advertising or performing various search engine optimization functions.
[0022] 2) 3D Backroom 201 , which receives information or instructions from potential customers 301 for the construction of 3D models or sites, so that the 3D models or sites can be displayed in 3D with the correct information to search engine users.
[0023] 3) An Application Programming Interface (“API”) 202 which connects the 3D Backroom with the Host Backroom, allowing the exchange of information, including but not limited to whether or not a particular website contains 3D results 103 which could be displayed by invoking the Client, and whether or not a customer desires to construct a 3D website. If this is the case, the Host Backroom will refer the customer to the 3D Backroom; and if the customer indeed constructs 3D results, the 3D Backroom will so notify the Host Backroom. Where applicable, the 3D Backroom may complete a payment process (if any), or provide necessary information for the Host Backroom to complete part or all of the payment process.
[0024] The production of 3D results can be accomplished in one or more steps, as follows:
[0000] 1) Converting a 2D website 401 into a standard 3D Website 106 containing some or all of the information in the website:
[0025] a) The customer utilizes a website or a mobile App, or a combination of both, which are connected to the 3D Backroom, to select the 3D structure he/she wishes to present based upon a number of different selections.
[0026] b) On each selectable structure, special locations or spots will be marked with identifications. Such locations or spots can display text, images or video information otherwise contained in the one or more 2D websites.
[0027] c) Certain special tokens 402 (including hypertext symbols or text) will be made available to the customer. The customer inserts the tokens (associated with particular spots locations or spots in the 3D structure) in the hypertext markup language used to power their 2D website(s) in accordance with instructions to indicate which information is to be displayed on which location or spots.
[0028] d) The 3D Backroom notifies the Server, which sends out a web spider 403 to the website(s), finds the special tokens, and retrieves the information identified by the special tokens.
[0029] e) The retrieved information, together with special tokens which identifies the locations or spots on which it is to be displayed, are then incorporated into the 3D rendering instructions 104 to be communicated to the Client to construct the 3D website containing the desired information. In the event that the information selected exceeds the permitted space within the 3D site, excess information will be made available as additional pages (which can be scrolled or turned or otherwise) viewable by the user.
[0030] f) Upon review and approval of the customer (optional), the 3D Website will reside on the Server.
[0031] g) The Server will notify the Host Server that the customer (identified by their 2D website or websites) has successfully produced a corresponding 3D Website, so that when a search event occurs and the customer's website or websites are to be displayed, a special symbol 103 will be inserted in the search result display 102 to indicate that this customer has a 3D Website.
[0032] h) If the search engine user taps on the special symbol, the 3D Search App will call up the Client connected by the SDK, and the user will enter into a 3D site where he will be able to navigate, view and interact with the information presented in a real 3D experience.
[0033] i) There are default modes for the selection of structure and the placement of information so that the customer need not make all selection decisions.
[0034] j) The 3D Backroom can further streamline and simplify the token placement process for customers who utilize some of the major Content Management Systems (such as Joolma), as the process will be integrated into such systems.
[0000] 2) Converting a 2D website into a customized 3D Website containing some or all of the information in the website:
[0035] a) In cases where the customer desires customization beyond the selection of 3D structure and placement of information, including the insertion of information other than on the 2D websites, the customer can utilize the customer version of the 3D Backroom.
[0036] b) In this version of the 3D Backroom, the customer can have a greater range of selection including, but not limited to, additional building styles, 2D decorations, 3D decorative objects, wall and floor textures and styles for text.
[0037] c) If further customization is needed, including the creation of 3D sites not within the selection, the customer can utilize expert services.
[0000] 3) Inserting custom 3D objects:
[0038] a) In some cases, the customer may wish to display custom 3D objects instead of or in addition to 3D sites, for example, an automotive brand displaying its new model car.
[0039] b) The 3D Backroom can accept standard 3D models from a number of major 3D rendering software tools and convert them into a 3D format for display.
[0040] c) In some cases, the customer can utilize expert services to construct these 3D models.
[0041] d) When constructed, the 3D models can be placed into the 3D sites, or individually called up to be displayed in the 3D Search App.
[0042] e) The 3D objects can move within 3D sites, for example, a 3D car model can rotate on a pedestal to simulate a showroom, or even drive through a 3D virtual city to simulate a test drive.
[0000] 4) 3D Websites with user-user interaction:
[0043] a) If, at a given time, more than one search engine user is viewing the same 3D site, then symbols (or avatars) representing these users can be made visible to other users with the placements of these symbols representing the actual location of these users as they navigate about within the 3D site, simulating a real-life encounter in a 3D environment.
[0044] b) These users can communicate with one another by tapping the symbol of the target, utilizing text, graphics (expressions) or voice.
[0045] c) If these users are registered, thereby having identifications, friends' lists or fans' lists can be created so that users can socialize further.
[0046] Typically, when a search result contains a 3D object or site, a symbol will appear on the screen of the user's mobile device. When the user taps that symbol or icon, the Client will be activated, and the user will be able to navigate or circumnavigate in the 3D site or object and interact with it. When the user is done with the 3D activities, they will be returned to the point where they first activated the 3D technology. Other possible User Interface arrangements can also be utilized.
[0047] The flowcharts shown in FIG. 2 provide an example of processes that occur on both Client side and the Server side. The flowcharts are provided solely to facilitate the understanding of the processes, with the understanding that the sequence of events depicted in the flowcharts is only one of the many ways the processes may occur.
[0048] The right-side flowchart of FIG. 2 illustrates how 3D scenes are constructed. When a Potential Customer 302 visits Search Engine Server Backroom 203 to register a website, the user may select to make the website a 3D Website. This intent is communicated from the Search Engine Server to a Server 200 through API 202.
[0049] Utilizing a website or a mobile app connected to the 3D Backroom 201 , the Potential Customer 302 can insert tokens 402 to identify which 3D structure is to be displayed on which location or spot. The Backroom 201 then notifies the Server 200, which will then send out Web Spider 403 to crawl the Customer website to find the tokens and retrieve the information identified by the tokens. The crawled data, including the retrieved information along with the tokens which identified the locations or spots on which the information is to be displayed, will then be stored in the Server as 3D Rendering Instructions 104.
[0050] The left-side flowchart illustrates how a Client 101 communicates with a Server 200 to display 3D search results. When a user runs a search using Host App 100 available on a website or a mobile phone, Search Engine is queried by the Host App 100 to generate and return a list of search results. For each returned search result item, API 202 located on Server 200 is consulted to see whether there is 3D version available. If API 202 indicated there is an available 3D version, a 3D Symbol 103 is shown next to the item in the list results. The user can then click on the 3D Symbol 103 to access a hyperlink associated with the 3D Symbol. The hyperlink refers to a medium that displays a 3D scene. The 3D scene may be a 3D Object 105 or a 3D site 106. The 3D scene resides on Server 200. Only a Host App attached with an 3D-capable Client 101 can view the 3D scene. Upon receiving a request from the user to display the 3D scene, the Client 101 will construct the 3D scene on the locations or spots according to its interpretation of the 3D rendering instructions 104.
|
An existing two-dimensional search engine app (“2D Search App”) is transformed into a search engine that can present three-dimensional results (“3D Search App”), allowing the presentation of 3D sites and objects on a mobile device through a mobile App in communication with a central server. The client is capable of performing 3D rendering in accordance with the instructions received from the server. The client also interacts with the server to send and retrieve other data, including requests, instructions and text, images or video. The server is capable of converting 3D models into instructions which can be sent to the client, thereby allowing the client to reproduce the 3D model in the mobile device for viewing. The invention finds application in a wide range of fields, including fashion, retail outlets, and product demonstration and sales.
| 6
|
FIELD OF THE INVENTION
[0001] This invention relates to single-pole recording heads for disk drives and in particular to a structure and method for reducing cross-talk and improving the signal-to noise ratio in a head used for perpendicular recording on a magnetic disk.
BACKGROUND
[0002] In perpendicular magnetic recording the data is recorded on a magnetic disk in which the easy axis of magnetization is aligned perpendicular to the surface of the disk. The recording head, viewed from the air bearing surface, contains a relatively small main pole and a relatively large auxiliary pole.
[0003] The recording head is normally mounted on a rotary arm which pivots about a stationary axis to move the head to various radial positions on the disk. This generates a skew angle θ between the main axis of the rotary arm and the tangential direction of the data tracks on the disk. This is illustrated schematically in FIGS. 1A-1C . In FIG. 1A the skew angle θ is equal to zero, i.e., the main axis of rotary arm 2 is exactly parallel to the data track on disk 4 that underlies the recording head 3 at the end of rotary arm 2 . In FIG. 1B , where the recording had 3 is located nearer to the center of disk 4 , the skew angle is equal to θ 1 . In FIG. 1C , where recording head 3 is located nearer to the edge of disk 4 , the skew angle is equal to θ 2 (which would have a sign opposite to that of θ 1 ).
[0004] The existence of a skew angle creates the problem illustrated in FIG. 2A , which is a schematic top view of the main pole 5 over two data tracks T 1 and T 2 . The skew angle is θ 3 . Although recording head 5 is writing to track T 2 , it is evident that a corner of head 5 overlies track T 1 . A solution to this problem is to fabricate the recording head with a trapezoidal shape, as shown in FIG. 2B . As shown, recording head 6 does not extend over track T 1 when the skew angle is equal to θ 3 because the sides of head 6 are canted by an angle α, giving head 6 a trapezoidal shape.
[0005] FIG. 3 is general schematic view of a perpendicular recording head 10 taken from the air-bearing surface (ABS), showing a main pole 11 , an auxiliary pole 12 , a reading element 13 and a lower shield 14 . For clarity, the components shown in FIG. 3 are not drawn to scale. The sides of main pole 11 are beveled by an angle α. It should be noted that this invention does not involve the structure of the auxiliary pole, reading element or lower shield. These components are well known and can be fabricated in accordance with known techniques.
[0006] FIG. 4 is a view of recording head 10 taken through a cross section that is perpendicular to the ABS. Shown are the main pole 11 and the auxiliary pole 12 . Also shown are a yoke 15 , a back gap 16 and a coil 17 . The main pole 11 , auxiliary pole 12 , yoke 15 and back gap 16 are made of a magnetic metal such as NiFe. The coil 16 is made of an electrically conductive metal such as Cu. The supporting layers separating these components are made of a hard nonconductive material such as alumina (Al 2 O 3 ). In operation, an electrical signal through coil 17 generates a magnetic flux that flows through yoke 15 and main pole 11 in the direction of the ABS and from the head to a magnetic recording disk (not shown).
[0007] FIGS. 5A and 5B are views of main pole 11 from the ABS and show how the trapezoidal shape is normally fabricated. Initially, main pole 11 has a rectangular shape, as shown in FIG. 5A . An ion milling process is normally used to bevel the sides of main pole 11 . As indicated by the arrows, the ion beam is directed to main pole 11 at an oblique angle so as to erode more material near the bottom of main pole 11 . To erode both sides of the main pole, the ion beam can be programmed to change the angle of incidence in sequence.
[0008] FIG. 6 is a close-up view of the area designated A in FIG. 4 , which is where most of the discussion herein is directed. The interface between the yoke 15 and the main pole 11 is shown, as well as the underlying and overlying alumina layers. The arrows denote the magnetic flux flowing from the yoke 15 to the main pole 11 and to the ABS.
[0009] One of the difficulties that has been encountered is to get a large enough bevel angle α in the main pole to avoid the problems of cross talk and signal-to-noise (STN) degradation described above. Conventionally, the layer directly below the main pole is made of alumina, which is a very hard material. The presence of this underlying alumina layer acts as a hard mask from below and makes it difficult to get a large bevel angle with the ion milling process. This can happen in two ways. First, the alumina layer retards the material of the main pole from being removed without over-milling. Second, during the milling process the alumina may redeposit onto the surfaces of the main pole, slowing down the removal process even more.
SUMMARY
[0010] According to this invention, a bevel angle promotion layer is formed beneath the layer of magnetic material that is to form the main pole. The main pole is not formed on a hard material such as Al 2 O 3 . The bevel angle promotion layer is formed of a non-magnetic material such as NiP, Rh, Ta, NiCr or Cd that is softer than Al 2 O 3 , (i.e., a material that is eroded more easily by ion milling than Al 2 O 3 ). With the main pole formed on this softer material, it is much easier to obtain the required bevel angle with an ion milling process, without the formation of the “fences” that result when the main pole rests on a hard material such as Al 2 O 3 .
[0011] There are several embodiments within the scope of the invention. In a first embodiment, the bevel angle promotion layer is formed between an end of the yoke and the air bearing surface (ABS). A top surface of the bevel angle promotion layer is coplanar with a top surface of the yoke, and the bevel angle promotion layer has the same thickness as the yoke. The main pole overlaps the yoke, and the magnetic flux flows across an interface between the yoke and the main pole.
[0012] In an second embodiment, the bevel angle promotion layer is integrated with a leading edge tape layer to broaden the path through which the magnetic flux may flow between the yoke and the main pole.
[0013] The invention also includes methods of fabricating the embodiments of this invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIGS. 1A-1C illustrate how a skew angle is produced as a recording head mounted to a rotary arm sweeps across a magnetic disk.
[0015] FIGS. 2A and 2B illustrate how cross talk can be reduced and the signal-to-noise ratio improved by forming the main pole of a recording head in a trapezoidal shape.
[0016] FIG. 3 is a schematic view from the ABS of a single pole type recording head having a trapezoidal main pole.
[0017] FIG. 4 is view of the recording head of FIG. 3 taken at a cross section perpendicular to the ABS.
[0018] FIGS. 5A and 5B illustrate conceptually the use of an ion milling process to form the beveled sides of a trapezoidal main pole.
[0019] FIG. 6 is a cross-sectional view of a prior art recording head with no bevel angle promotion layer.
[0020] FIG. 7 is a cross-sectional view of a single pole recording head with a promotion layer that overlaps the yoke.
[0021] FIGS. 8A-8C illustrate a process of fabricating the recording head shown in FIG. 7 .
[0022] FIGS. 9A and 9B illustrate the formation of a “fence” in a head wherein the main pole directly overlies an Al 2 O 3 layer.
[0023] FIG. 10 is a cross-sectional view of a single pole recording head with a bevel angle promotion layer that does not overlap the yoke so as to constrict the magnetic flux path.
[0024] FIGS. 11A-11L illustrate a process of fabricating the recording head shown in FIG. 10 .
[0025] FIG. 12 is a cross-sectional view of a recording head wherein a bevel angle promotion layer is integrated with a leading edge taper layer to broaden the magnetic flux path.
[0026] FIGS. 13A-13G illustrate a process of fabricating the recording head shown in FIG. 12 .
DETAILED DESCRIPTION
[0027] As described above, the presence of a hard alumina level directly beneath the main pole impedes the fabrication of a large bevel angle α using an ion milling process. One technique of overcoming this problem is to fabricate a relatively soft layer, which can be referred to as a “bevel angle promotion layer” or simply “promotion layer,” immediately below the main pole. FIG. 7 illustrates a view similar to that of FIG. 6 but with a promotion layer 20 underneath main pole 11 .
[0028] The promotion layer 11 may be fabricated by the process illustrated in FIGS. 8A-8C . Initially, the yoke 15 and underlying alumina layer are fabricated using known processes. Then, as shown in FIG. 8A , a “lift off” photoresist layer 22 is deposited and patterned with an aperture overlying a portion of yoke 15 . A “lift” off photoresist layer is actually two photoresist layers which are patterned to produce the overhang shown in FIG. 8A .
[0029] Next, as shown in FIG. 8B , promotion layer 20 is deposited on the structure. Promotion layer 20 could include NiP, Rh, Ta, NiCr or Cd, for example. Lift off photoresist layer 22 is then removed (along with the overlying portion of promotion layer 20 ), and main pole 11 is deposited. Main pole 11 could be made of NiFe. Afterward, the overlying alumina layer is deposited, and the structure is lapped or polished to the location of the ABS (shown in FIGS. 8B and 8C ), producing the head shown in FIG. 7 .
[0030] One possible problem with this structure is illustrated in FIG. 7 . Because the promotion layer 20 is made of a soft non-magnetic material, the overlap between promotion layer 20 and yoke 15 tends to reduce the area through which the magnetic flux must flow at the interface between yoke 15 and main pole 11 .
[0031] Another possible problem is illustrated in FIG. 9A . With a relatively thin promotion layer 20 the ion beam may still strike the alumina layer, causing atoms of alumina to become dislodged and forming “fences” 24 that extend upwards along the sides of main pole 11 . As the ion milling process continues, this can lead to a seriously deformed main pole, as shown in FIG. 9B .
[0032] These problems are overcome in the structure shown in FIG. 10 . In this structure a thick promotion layer 26 is formed, having a top surface that is substantially coplanar with the top surface of the yoke 15 . Thus, promotion layer 26 does not overlap yoke 15 , and the flux flow across the interface between yoke 15 and main pole 11 is not restricted.
[0033] FIGS. 11A-11J illustrate a process that can be used to fabricate the structure of FIG. 10 .
[0034] The process to be described begins at the stage of the overall head fabrication process after the back gap 16 and an adjacent Al 2 O 3 layer 28 have been formed. This is shown in FIG. 11A . The back gap 16 may be made of NiFe. The preceding stages of the process (e.g., the fabrication of the auxiliary pole and the coil) are conventional and will not be described here.
[0035] Referring to FIG. 11B , a NiP seed layer 30 is deposited on Al 2 O 3 layer 28 by chemical vapor deposition, sputtering or some other deposition technique to a thickness of 1000 Å, for example. If desired, the seed layer can be removing from the back gap 16 by ion milling.
[0036] Next, as shown in FIG. 11C , yoke 15 , typically made of NiFe, is plated onto back gap 16 and seed layer 30 , with an opening in the area where the ABS is to be formed. A photoresist layer (not shown) is deposited in the opening area to prevent NiFe from being plated in that area. After yoke 15 has been plated, the photoresist layer is removed. Yoke 15 merges with back gap 16 to form a path for the magnetic flux.
[0037] As shown in FIG. 11D , a photoresist layer 34 is deposited on yoke 15 and photoresist layer 34 is patterned to form an opening 36 , which overlies opening 32 and a portion of yoke 15 .
[0038] As shown in FIG. 11E , a NiP layer 38 is plated in opening 36 and on NiP seed layer. NiP layer 38 may be 5-7 μm thick, for example. Photoresist layer 34 is removed, as shown in FIG. 11F .
[0039] An Al 2 O 3 layer 40 is then deposited over the entire surface of the structure to fill areas not shown in the drawings, as shown in FIG. 11G . The top surface of the structure is then polished by chemical-mechanical polishing (CMP) to a level below the top surface of yoke 15 , leaving the structure shown in FIG. 11H .
[0040] Next, as shown in FIG. 11I , a NiFe layer 40 is deposited to form a structure which will become main pole 20 . NiFe layer 40 is then patterned to form a specified area of contact with yoke 15 , as shown in FIG. 11J .
[0041] FIGS. 11K and 11L are views taken at the cross section labeled ABS in FIG. 11I . FIG. 11K shows how NiFe layer 40 is initially patterned to the width of main pole 20 , and FIG. 11L shows how the sides of main pole 20 are beveled to a desired angle, using an ion milling process. Because layer 38 underneath main pole 20 is made of NiP, a relatively soft material as compared with Al 2 O 3 , a large angle can be formed, and there are no “fences” along the sides of main pole 20 .
[0042] After the deposition of an Al 2 O 3 layer over and around main pole 20 , the structure is diced and polished along the cross section ABS to form the pole structure shown in FIG. 10 .
[0043] As described above, it is helpful to maximize the area of contact between the yoke and the main pole because this provides a broader path for the magnetic flux to flow between these elements. According to another aspect of this invention, the bevel angle promotion layer is integrated with a leading edge taper layer to increase the area of contact between the yoke and the main pole.
[0044] A cross-sectional view of a main pole structure in accordance with this aspect of the invention is shown in FIG. 12 . Main pole 20 overlies both a bevel angle promotion layer 50 and a leading edge taper layer 52 . Promotion layer 50 is formed of a relatively soft non-magnetic material such as NiP, Rh, Ta, NiCr or Cd. Leading edge taper layer 52 is formed of a magnetic material such as NiFe. The interface between promotion layer 50 and leading edge taper layer 52 is located between the end of yoke 15 and the ABS. As a result, the magnetic flux can flow through the portion of leading edge taper layer 52 that is located between the end of yoke 15 and the ABS.
[0045] FIGS. 13A-13G illustrate the steps of a process for fabricating the structure shown in FIG. 12 . Initially, the main pole, coil, yoke and intervening Al 2 O 3 layers are formed in a conventional manner to arrive at the structure shown in FIG. 13A . The top surface of yoke 15 and Al 2 O 3 layer 54 are coplanar.
[0046] As shown in FIG. 13B , promotion layer 50 is deposited by chemical vapor deposition, sputtering, or another full film deposition method to a thickness of 10-300 nm, for example, on top of yoke 15 and Al 2 O 3 layer 54 . Promotion layer 50 can be formed of Rh, for example.
[0047] As shown in FIG. 13C , a lift off photoresist layer 56 is deposited and patterned such that an edge of photoresist layer 56 is located over Al 2 O 3 layer 54 between the edge of yoke 15 and the plane of the ABS that is later to be formed.
[0048] As shown in FIG. 13D , the portion of promotion layer 50 that is left exposed by photoresist layer 56 is removed by ion milling, leaving an angled edge that overlies Al 2 O 3 layer 54 . The ion beam can be programmed to transition through a desired sequence of angles.
[0049] Next, as shown in FIG. 13E , the leading edge taper layer 52 is deposited. Leading edge taper layer 52 may be formed of NiFe. Because photoresist layer 56 is used as a mask both for the removal of a portion of promotion layer 50 and for the deposition of leading edge taper layer 52 , the edges of promotion layer 50 and lead edge taper layer 52 abut each other at a location above Al 2 O 3 layer 54 . The lateral location of the edge of photoresist layer 56 determines the location of the interface between leading edge taper layer 52 and promotion layer 50 and hence the amount of leading edge taper layer 52 that will be available as a path for the magnetic flux flowing from yoke 15 .
[0050] Photoresist layer 56 is then removed by a lift-off process, yielding the structure shown in FIG. 13F . The NiFe layer that will form the main pole 20 is deposited on top of leading edge taper layer 52 and promotion layer 50 . The main pole 20 is patterned and shaped by ion milling as described above in connection with FIGS. 11K and 11L . The presence of the relatively soft promotion layer 50 in the area of the ABS allows the bevel angle α to be made larger than if the main pole 20 were located over a harder material such as Al 2 O 3 , for example. Thereafter an Al 2 O 3 layer is deposited over the main pole 20 and the structure is diced at the ABS (denoted by the dashed line in FIG. 13G ) to produce the structure shown in FIG. 12 . This unique structure allows two desirable objectives to be satisfied simultaneously: namely, the fabrication of a main pole having a trapezoidal shape with a large bevel angle and the creation of a broad path for the magnetic flux to flow between the yoke and the main pole.
[0051] Although the present invention is illustrated in connection with specific embodiments for instructional purposes, the present invention is not limited thereto. Various adaptations and modifications may be made without departing from the scope of the invention. Therefore, the spirit and scope of the appended claims should not be limited to the foregoing description.
|
A single-pole perpendicular magnetic recording head contains a bevel angle promotion layer that facilitates the fabrication of the bevel angle in a trapezoidal main pole. The bevel angle promotion layer is made of a non-magnetic material that is softer than the material (e.g., Al 2 O 3 ) that normally underlies the main pole. In one embodiment, the bevel angle promotion layer is formed between an end of the yoke and the air bearing surface (ABS), with the top surface of the bevel angle promotion layer being substantially coplanar wit the top surface of the yoke. In other embodiment the bevel angle promotion layer is integrated with a leading edge taper material, which is formed of a magnetic material, to broaden the magnetic flux path between the yoke and the main pole.
| 8
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from U.S. Provisional Patent Application Serial No. 60/317,883 filed Sep. 7, 2001; the disclosures of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Technical Field
[0003] The present invention generally relates to the technical field of heating, ventilation, and air conditioning equipment. More particularly, the present invention relates to equipment for mounting ventilation ducts in heating, ventilation, and air conditioning systems. Specifically, the present invention relates to a register boot frame that is first used to cover the register openings in new construction and is then used to help install the register boots.
[0004] 2. Background Information
[0005] Duct systems for ventilation systems include register boots where the ducts extend through register openings in floors. Floors are installed in new construction before the duct systems are installed. The register openings are also cut into the floors before the ventilation ducts are installed. In new house construction, the register openings allow debris to fall through the floor into the basement. Such falling debris is undesirable in generally but is especially undesirable when the new concrete floor is poured in the basement. Covers for the register openings are thus desired in the art.
[0006] Register openings also create a safety hazard because people can accidently step through the openings and injure a foot, an ankle, or a leg. Any cover provided for the register openings would ideally provide a warning to those walking near the openings and would support the weight of a person who accidently steps on the cover.
[0007] Another problem with register openings and register boots is that they are somewhat difficult and time consuming to install. The worker installing a register boot must first position the boot from below and have second worker connect the boot to the floor from above. This process is undesirable because it requires two workers. Another drawback is that the resulting connection between the register boot and the floor can be rather leaky.
BRIEF SUMMARY OF THE INVENTION
[0008] The present invention provides a register opening cover that may be used to cover register openings until the register boot is installed in the register opening. During the installation of the register boot, the invention may be used to hold the register boot in place until the register boot is securely connected to the floor. After the register boot is installed, the cover forms an insulator around the register boot.
[0009] One embodiment of the invention provides a register opening cover and register boot frame that can be configured to fit register boots of different sizes. Another embodiment of the invention provides a register opening cover that will support some of the weight of a worker who may step on the covered register opening.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0010] [0010]FIG. 1 is a top plan view of the first embodiment of the register boot frame of the present invention.
[0011] [0011]FIG. 2 is a side view of the frame of FIG. 1.
[0012] [0012]FIG. 3 is a top plan view of the second embodiment of the register boot frame of the present invention.
[0013] [0013]FIG. 3A is a top plan view of the third embodiment of the register boot frame of the present invention.
[0014] [0014]FIG. 4 is a perspective view of a floor section having a register opening with the register boot frame of the invention aligned with the opening before it is installed.
[0015] [0015]FIG. 5 is a view similar to FIG. 4 showing the register boot frame installed over the opening.
[0016] [0016]FIG. 6 is a section view taken along line 6 - 6 of FIG. 5.
[0017] [0017]FIG. 7 is a view similar to FIG. 6 showing the register boot frame with the center section removed and a register boot being aligned with the register opening.
[0018] [0018]FIG. 8 is a view similar to FIG. 6 showing the register boot installed in the register opening.
[0019] [0019]FIG. 9 is a perspective view of the register boot installed in the register opening with the register boot frame of the invention.
[0020] [0020]FIG. 10 is a perspective view of an alternative embodiment installed adjacent a wall with the longitudinal edge of the frame folded up.
[0021] [0021]FIG. 11 is a series of views showing the installations processes for the invention.
[0022] Similar numbers refer to similar elements throughout the specification.
DETAILED DESCRIPTION OF THE INVENTION
[0023] The first embodiment of the register boot frame of the invention is indicated generally by the numeral 2 in the accompanying drawings. Frame 2 may be configured to be used with ten, twelve, or fourteen inch register boots by selectively removing the middle portion 3 of the body 4 of frame 2 . In the first embodiment, body 4 includes a center portion 6 and two end portions 8 that are separated from center portion 6 with a perforation line 10 . Perforation lines 10 allows both end portions 8 to be removed to size frame 2 to fit the ten inch register boot. One end portion 8 may be removed to size frame 2 to fit the twelve inch register boot. When a fourteen inch register boot is used, both end portions 8 remain in place. In another embodiment of the invention, markings are used instead of perforation lines 10 and the worker cuts end portions 8 away with a knife or scissors.
[0024] Center portion 6 of frame 2 defines noncontinuous slits 12 in the form of a ten inch rectangle. Slits 12 are noncontinuous so that middle portion 3 does not fall out of center portion 6 until the worker intends to remove it. Noncontinuous slits 12 also allow middle portion 3 to support weight when frame 2 is initially installed. This allows frame 2 to support a worker who accidently steps on frame 2 when it is installed over a register opening.
[0025] When frame 2 will be used with a ten inch register boot, the worker removes both end portions 8 and cuts away middle portion 3 with a suitable knife. This configuration is depicted in FIG. 4. In another embodiment of the invention, the ten inch rectangle may be marked on center portion 6 and the worker would cut out middle portion 3 with a knife.
[0026] Each end portion 8 defines a noncontinuous, C-shaped slit 14 positioned with the open end of the C facing center portion 6 . When frame 2 is used with a twelve inch register boot, one C-shaped slit 14 is cut away such that the overall opening in frame 2 is twelve inches. In the twelve inch configuration, only one end portion 8 is cut away. When frame 2 is used with a fourteen inch register boot, two C-shaped slits 14 are cut away such that the overall opening in frame 2 is fourteen inches. In the fourteen inch configuration, both end portions 8 are used with frame 2 .
[0027] In the first embodiment of the invention, frame 2 is designed to be used with register boots that are four inches width and ten, twelve, or fourteen inches long. In the second embodiment of the invention, frame 20 (FIG. 3) is designed to work with register boots that are 2¼ inches wide. In the second embodiment, frame 22 includes a plurality of openings 22 separated by bars 24 . Bars 24 are cut away in order to form the openings for the register boots. In this embodiment, bars 24 are used to support weight when frame 20 is initially installed. Frame 20 may also be configured with noncontinuous slits.
[0028] A third embodiment of the invention is depicted in FIG. 3A and is indicated generally by the numeral 30 . Frame 30 has two end portions 8 disposed at the same end of center portion 6 . Frame 30 may include noncontinuous slits or the openings and bars depicted in the drawing.
[0029] Each of these embodiments may include corner slits 40 that allow the sidewalls of body 4 to flex when a register boot is forced up through the opening of body 4 . As will be described below in more detail, the openings in body 4 is sized to frictionally engage the outer surface of the register boot. Corner slits 40 allow body 4 to frictionally engage the register boot without tearing.
[0030] Body 4 of each embodiment may be fabricated from a corrugated plastic material. The corrugations may be disposed to run across the width of frame 2 to increase the strength of the material. The corrugations may also run the length of frame 2 . When the corrugations run along the longitudinal direction of frame 2 , the longitudinal edge of frame 2 may be folded up as described below with respect to fold line 80 . The material may be opaque and colored brightly to draw attention to the frame when it is initially positioned over a register opening. This material also allows some light to pass through into the lower level. Each frame may also be clearly marked with a warning that the frame is “NOT A STEP” so that workers will not fall through the frame and register opening.
[0031] Body 4 may also define corner fold lines 50 that allow the inner corners 52 to be folded down to help the worker position frame 2 with respect to the register opening.
[0032] Frame 2 is used in the manner depicted in FIGS. 4 - 9 . One frame 2 may be used as a template to mark opening 60 on floor 62 . The width of frame 2 may be used to space opening 60 from the wall. The user then cuts floor 62 along the marked lines to form opening 60 . An unused frame 2 is then selected to match opening 60 . In the example, frame 2 is being used with a 10×4 inch opening 60 . When inner corners 52 are not used, frame 2 is aligned with opening 60 . If corners 52 are available, the worker may fold down inner corners 52 before placing frame 2 over opening 60 . Inner corners 52 allow frame 2 to be easily positioned over opening 60 as depicted in FIGS. 5 and 6. Once positioned, frame 2 is connected to floor 62 with appropriate connectors 64 such as staples, screws, nails, or glue. Frame 2 then remains in place covering opening 60 for safety and preventing debris from falling though opening 60 .
[0033] When register boot 70 is to be installed, the worker removes middle portion 3 and slides register boot 70 up through frame 2 from below. Frame 2 frictionally engages the outer surface of register boot 70 so that frame 2 will hold register boot 70 in place while the worker walks upstairs and connects register boot 70 to floor 62 with appropriate connectors 72 . Duct tape may be used between frame 2 and boot 70 to prevent air from flowing between the two members. The invention thus allows a register boot to be installed by a single worker instead of the two workers in the past.
[0034] The flooring material may be positioned over frame 2 around the protruding portion of register boot 70 . Frame 2 then functions to seal opening 60 and to provide some insulation properties.
[0035] In alternative embodiments, frames 2 , 20 , or 30 may include a fold line 80 that allows one of the longitudinal edges of frame 2 , 20 , or 30 to be folded up to abut a wall adjacent opening 60 as shown in FIG. 10. Fold line 80 may be a mark that shows the user where to fold the frame. Fold line 80 may also be a perforated line or a score line that allows the user to easily make the fold. This configuration is designed specifically for a baseboard boot frame application.
[0036] In the foregoing description, certain terms have been used for brevity, clearness, and understanding. No unnecessary limitations are to be implied therefrom beyond the requirement of the prior art because such terms are used for descriptive purposes and are intended to be broadly construed.
[0037] Moreover, the description and illustration of the invention is an example and the invention is not limited to the exact details shown or described.
|
A register opening cover may be used to cover register openings until the register boot is installed in the register opening. During the installation of the register boot, the invention may be used to hold the register boot in place until the register boot is securely connected to the floor. After the register boot is installed, the cover forms an insulator around the register boot. One embodiment of the invention provides a register opening cover and register boot frame that can be configured to fit register boots of different sizes. Another embodiment of the invention provides a register opening cover that will support some of the weight of a worker who may step on the covered register opening.
| 5
|
CROSS REFERENCE TO RELATED APPLICATION
[0001] This is a continuation of U.S. application Ser. No. 11/782,274, filed Jul. 24, 2007, which is a continuation of U.S. application Ser. No. 09/986,577, filed Nov. 9, 2001 (U.S. Pat. No. 7,266,235), which is a divisional of U.S. application Ser. No. 09/986,299, filed Nov. 8, 2001 (U.S. Pat. No. 7,133,550). This application relates to and claims priority from Japanese Patent Application No. 2000-347443, filed on Nov. 9, 2000. The entirety of the contents and subject matter of all of the above is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a method and apparatus for fabricating substrates having circuit patterns, such as semiconductor devices and liquid crystal display devices, and, more particularly, to a technique for inspecting substrate patterns in a fabrication process.
[0003] Conventional optical or electron-beam pattern inspection apparatuses have been proposed in JP-A Nos. H5(1993)-258703, H11(1999)-160247, S61(1986)-278706, H7(1995)-5116, H2(1990)-146682, H9(1997)-312318, and H3(1991)-85742, for example.
[0004] FIG. 1 shows an example of an electron-beam pattern inspection apparatus of the type disclosed in JP-A No. H5(1993)-258703. In this conventional electron-beam pattern inspection apparatus, an electron beam 2 emitted from an electron source 1 is deflected in the X direction by a deflector 3 , and the electron beam 2 thus deflected impinges on an object substrate 5 under test after passing through an objective lens 4 . Simultaneously, while a stage 6 is moved continuously in the Y direction, secondary electrons 7 or the like produced from the object substrate 5 are detected by a detector 8 . Thus, a detected analog signal is output from the detector 8 . Then, through an A/D converter 9 , the detected analog signal is converted into a digital image. In an image processor circuit 10 , the digital image thus produced is compared with a reference digital image which is expected to be identical thereto. If any difference is found, the difference is judged to be a pattern defect 11 , and the location thereof is determined.
[0005] FIG. 2 shows an example of an optical pattern inspection apparatus of the type in JP-A No. H11(1999)-160247. In this conventional optical inspection apparatus, a light beam emitted from a light source 21 is applied to an object substrate 5 under test through an objective lens 22 , and light reflected from the object substrate 5 is detected by an image sensor 23 . While a stage 6 is moved at a constant speed, detection of reflected light is repeated to produce a detected image 24 . The detected image 24 thus produced is stored into a memory 25 . In an image processing circuit 10 , the detected image 24 is compared with a previously memorized reference image 27 , which is expected to have a pattern identical to that of the detected image 24 . If the pattern of the detected image is identical to that of the reference image 27 , it is judged that there is no defect, on the object substrate 5 . If these patterns are not identical to each other, a pattern defect 11 is recognized, and the location thereof is determined.
[0006] As an example, FIG. 3 shows a layout of a wafer 31 corresponding to the object substrate 5 . On the wafer 31 , there are formed dies 32 which are to be separated eventually as individual identical products. The stage 6 is moved along a scanning line 33 to detect images in a stripe region 34 . In a situation where a detection position A 35 is currently taken, a pattern image attained at the detection position A 35 is compared with a pattern image attained at a detection position B 36 (reference pattern image 27 ), which has been stored in the memory 25 . Thus, each pattern image is compared with a reference pattern image which is expected to be identical thereto. In this arrangement, the memory 25 has a storage capacity sufficient for retaining reference pattern image data to be used for comparison, and the circuit structure of the memory 25 is designed to perform a circular-shift memory operation.
[0007] In the following two examples, a defect check is conducted using a binary image of an object under test. In synchronization with pattern detection, a judgment is formed on whether a pattern of the object is defective or not while ignoring a possible defect in a particular mask region.
[0008] In JP-A No. S61(1986)-278706, there is disclosed an example of a technique for inspecting through-holes on a printed circuit board. In this inspection technique, a printed circuit board having through-holes only in a non-inspection region thereof is prepared beforehand, and an image of the printed circuit board is taken prior to inspection. A binary image indicating the presence/absence of through-holes is thus attained for masking, and it is stored as image data in a masking data storage. At the time of inspection, if a difference found in binary image comparison is located at a position included in a mask region stored in the masking data storage, the difference is ignored for non-inspection.
[0009] In JP-A No. H7(1995)-5116, there is disclosed an example of a technique for printed circuit board inspection. In this inspection technique, a pattern is detected to provide binary image data, and using the binary image data, a judgment is formed on whether the detected pattern is normal or not; more specifically, it is checked to determine whether the detected pattern meets any specified regular pattern or not. If not, the detected pattern is judged to be defective.
[0010] In the following two examples, using pattern data, a dead zone is provided for the purpose of allowing an error at a pattern boundary in inspection.
[0011] In JP-A No. H2(1990)-146682, there is disclosed an example of an inspection technique in which a mask pattern is compared with design data. Through calculation of design data, a pattern is reduced by a predetermined width to attain a reduced image, and also the pattern, is enlarged by a predetermined width to attain an enlarged image. Then, a part common to the reduced image and the enlarged image is extracted to provide a dead zone having a certain width. Thus, using the design data, a mask region is provided so that an error at a pattern boundary having a certain width will be ignored during inspection.
[0012] In JP-A No. H9(1997)-312318, there is disclosed an example of a technique for inspecting patterns using a scanning electron microscope (hereinafter referred to just as a “SEM”). Using a reference image acquired in advance, a vicinal area of a pattern edge is set up as a region where no critical defect occurs, since a minuscule deviation of a pattern edge is not regarded as a defect. Thus, an image of the region where no critical defect occurs is ignored. If any difference is found between the reference image and an image of a pattern under test, excluding the region where no critical defect occurs, the difference is judged to be a pattern defect.
[0013] In JP-A. No. H3(1991)-85742, there is disclosed an example of a system for carrying out comparative inspection of printed circuit patterns. An image of a candidate defect attained in comparative inspection, is stored in memory. Then, not simultaneously with the comparative inspection, the memorized image is examined to judge whether a difference is actually a defect or not.
[0014] On an object under test, there is an area where a considerable difference is found in comparative inspection of patterns, even if the difference is not actually a defect. For example, on an ion-implanted region for formation of a transistor, a non-defective difference may be found in comparative inspection of patterns. Although a difference between a part where ions have been implanted and a part where ions have not been implanted is important at a location of a transistor element, the characteristics of wiring areas, other than transistor element locations, are not affected by the presence/absence of implanted ions. Therefore, in an ion implantation process, rough masking is used to determine where ions are to be implanted. However, in electron-beam inspection of wiring areas, a considerable difference attributable to whether implanted ions are present or not may be detected, resulting in a wrong judgment indicating that the difference represents a defect.
[0015] Further, for example, in a power line layer where redundant wiring is provided, even if a part of the wiring is not connected, circuit normality can be ensured by providing a connection at another point. Therefore, in some cases, rough patterning is provided for a power wiring arrangement, so that no-connection on pattern elements are left. In comparative inspection of detected images, a difference attributable to whether a connection is provided or not nay be found, resulting in a wrong judgment indicating that the difference represents a defect.
[0016] Still further, for example, on a pattern edge, a detected signal level varies depending on the thickness/inclination of a film thereof. Although up to a certain degree of variation in detected signal output may be ignored, a considerable difference in detected signal output is likely to be taken as a defect mistakenly. A degree of false defect detection is however applicable as an index representing product quality. It is desirable to examine the degree of false defect detection and preclude false defects before carrying out defect inspection.
[0017] In the conventional optical/electron-beam pattern inspection apparatuses disclosed in JP-A Nos. H5(1993)-258703 and H11(1999)-160247, it is not allowed to set up a non-inspection region.
[0018] In the inspection techniques disclosed in JP-A Nos. S61(1986)-278706 and H7(1995)-5116, there is provided a non-inspection region. However, according to an example presented in JP-A No. S61(1986)-278706, it is required to specify a non-inspection region covering a very large area by using a bit pattern. In application to wafer inspection, a wafer surface area 300 mm in diameter has to be inspected using pixels each having a size of 0.1 μm. This requires an impractically large number of pixels, i.e., seven tera-pixels (seven terabits). According to the inspection technique disclosed in JP-A No. H7(1995)-5116, any areas other than regular pattern areas are treated as non-inspection regions. Since very complex patterns are formed on a wafer, a non-inspection region cannot be set up just by means of simple pattern regularity.
[0019] In the inspection techniques disclosed in JP-A Nos. H2(1990)-146682 and H9(1997)-312318, the use of a non-inspection region is limited to a pattern edge, and therefore it is not allowed to set up a non-inspection region at an arbitrary desired location.
[0020] In the inspection system disclosed in JP-A No. H3(1991)-85742, image data of a candidate defect is stored, and then detail inspection is carried out using the stored image data to check whether a difference is actually a defect or not. This approach is applicable to inspection of complex pattern geometries. However, based on predetermined criteria, a judgment is formed on whether a difference is actually a defect or not. Any part may be judged to be normal if requirements based on predetermined criteria are satisfied. That is to say, once a part is judged to be normal, data regarding the part will be lost.
[0021] As described above, in the conventional pattern inspection techniques, it is not allowed for a user to set up a non-inspection region effective for a device having a complex, large pattern area to be inspected, such as a wafer. Further, in cases where a considerable difference is found in comparative inspection of detected images even if the difference is not actually a defect, it is likely to be misjudged that the difference represents a defect. In addition to these disadvantages, the conventional pattern inspection techniques are also unsatisfactory as regards stability in detection of minuscule defects.
SUMMARY OF THE INVENTION
[0022] It is therefore an object of the present invention to overcome the above-mentioned disadvantages of the prior art by providing a pattern inspection method and apparatus for enabling a user to easily set up a non-inspection region effective for a device having a complex, large pattern area to be inspected.
[0023] In accomplishing this object of the present invention, and according to one aspect thereof, there is provided a pattern inspection apparatus such as shown in FIG. 4 . While an exemplary configuration of an electron-beam pattern inspection apparatus is presented here, an optical pattern inspection apparatus can be configured in the same fashion in principle. The electron-beam pattern inspection apparatus shown in FIG. 4 comprises an electron source 1 for emitting an electron beam 2 , a deflector 3 for deflecting the electron beam 2 , an objective lens 4 for converging the electron beam 2 onto an object substrate 5 under test, a stage 6 for holding the object substrate 5 and for scanning/positioning the object substrate 5 , and a detector 8 for detecting secondary electrons 7 or the like produced from the object substrate 5 to output a detected analog signal. An A/D converter 9 converts the detected analog signal into a digital image, and an image processor circuit 10 compares the converted digital image with a reference digital image expected to be identical thereto and identifies a difference found in comparison as a candidate defect 40 . A candidate defect memory part 41 is provided for storing feature quantity data of each candidate defect 40 , such as coordinate data, projection length data and shape data, and a mask setting part 44 examines pattern defects 11 stored in the candidate defect memory part 41 and flags a candidate defect located in a mask region 42 (shown in FIG. 5 ), prespecified with coordinates, as a masked defect 43 (shown in FIG. 5 ). An operation display 45 is provided on which data of pattern defects 11 received from the mask setting part 44 is displayed, an image of a selected pattern defect 11 is displayed, and the mask region 42 is displayed or edited.
[0024] The operations in the electron-beam pattern inspection apparatus, configured as mentioned above, will be described. Referring now to FIG. 5 , the mask region 42 will be described first.
[0025] On the object, substrate 5 , there is an area where a considerable difference is found in comparative inspection of patterns, even if the difference is not actually a defect, such as a region 50 where ions have been implanted. In actual practice, during ion implantation, ions are likely to be implanted in a deviated fashion, i.e., a deviated ion-implanted part 52 is formed in addition to normal ion-implanted pattern parts 51 . The deviated ion-implanted part 52 has no adverse effect on device characteristics, i.e., the deviated ion-implanted part 52 should be judged to be non-defective. However, the deviated ion-implanted part 52 is detected as a pattern defect 11 . Therefore, an area including the ion-implanted region 50 is set up as a mask region 42 , and a possible defect in the mask region 42 is treated as a masked defect 43 . Since the same die pattern is formed repetitively on the wafer 31 shown in FIG. 3 , on-die coordinates are used in region recognition. Parts, having the sane coordinates on different dies are regarded as identical, and if in-die coordinates of a part are included in a specified region, it is regarded that the part is included in the specified region. For the wafer 31 , beam shots are also characterized by repetitiveness besides dies. Each shot is a unit of beam exposure in a pattern exposure system used for semiconductor device fabrication. For identifying some kinds of false defects to be precluded in pattern inspection, the use of shots may be more suitable than that of dies with respect to pattern repetitiveness. Although the following description handles dies, it will be obvious to those skilled in the art that shots are applicable in lieu of dies and that an arrangement may be provided for allowing a changeover between shots and dies.
[0026] Operations in the electron-beam pattern inspection apparatus according to the present invention include a conditioning operation in which the mask region 42 is defined and an inspection operation in which any candidate defect 40 detected in other than the mask region 42 is judged to be a pattern defect.
[0027] In the conditioning operation, the mask region 42 is cleared, the electron beam 2 emitted from the electron source 1 is deflected in the X direction by the deflector 3 , and the electron beam 2 thus deflected is applied to the object substrate 5 through the objective lens 4 . Simultaneously, while the stage 6 is moved continuously in the Y direction, secondary electrons 7 or the like produced from the object substrate 5 are detected by the detector 8 . Thus, a detected analog signal is output from the detector 8 . Then, through the A/D converter 9 , the detected analog signal is converted into a digital image. In the image processor circuit 10 , the digital image thus produced is compared with a reference digital image which is expected to be identical thereto. If any difference is found in comparison, the difference is indicated as a candidate defect 40 . Feature quantity data of each candidate defect 40 , such as coordinate data, projection length data and shape data (image data), is stored into the candidate defect memory part 41 . In the mask setting part 44 , pattern defects 11 are set using feature quantity data of respective candidate defects 40 . The pattern defects 11 are superimposed on an image of the object substrate 5 , and the resultant image is presented on a map display part 55 of an operation display 45 (screen), as shown in FIG. 6 . The user can select any one of the pattern defects 11 (including true defects 57 and, false defects 58 not to be detected, in FIG. 6 ) on the map display part 55 of the operation display 45 . An image of a pattern defect 11 selected on the map display part 55 is presented on an image display part 56 of the operation display 45 . By checking the image of each of the pattern defects 11 on the image display part 56 , the user classifies the pattern defects 11 into true defects 57 and false defects 58 not to be detected. The results of this classification are indicated as particular symbols on the map display part 55 .
[0028] After completion of the defect classification mentioned above, the user selects an operation display screen shown in FIG. 7 , which comprises a map display part 55 for presenting an enlarged map including true defects 57 , false defects 58 not to be detected and a current position indicator 59 , and an image display part 56 for presenting an image corresponding to the current position indicator 59 . On the map display part 55 , the user can specify a mask region 42 and check a position of each pattern defect 11 . With reference to classification information on each pattern defect 11 and the image corresponding to the current position indicator 59 , the user sets up coordinates of a mask region 42 so that the false defects 58 will not be detected. As required, the user carries out the conditioning operation again to set up the coordinates of the mask region 42 more accurately.
[0029] In the inspection operation, the electron beam 2 emitted from the electron source 1 is deflected in the X direction by the deflector 3 , and the electron beam 2 thus deflected is applied to the object substrate 5 through the objective lens 4 . Simultaneously, while the stage 6 is moved continuously in the Y direction, secondary electrons 7 or the like produced from the object substrate 5 are detected by the detector 8 . Thus, a detected analog signal is output from the detector 8 . Then, through the A/D converter 9 , the detected analog signal is converted into a digital image. In the image processor circuit 10 , the digital image thus produced is compared with a reference digital image which is expected to be identical thereto. If any difference is found in comparison, the difference is indicated as a candidate defect 40 . Feature quantity data of each candidate defect 40 , such as coordinate data, projection length data and shape data (image data), is stored into the candidate defect memory part 41 . The feature quantity data of each candidate defect 40 is examined to judge whether the candidate defect 40 is located in the specified mask region 42 or not. If it is determined that the candidate defect 40 is not located in the specified mask region 42 , the candidate defect 40 is defined as a pattern defect 11 . Then, the pattern defect 11 is superimposed on an image of the object substrate 5 , and the resultant image is presented on the map display part 55 . Even if the candidate defect 40 is not defined as a pattern defect 1 , the feature quantity data thereof is retained so that it can be displayed again. This makes it possible for the user to avoid forming a wrong judgment that a considerable non-defective difference is a defect.
[0030] In the above-mentioned arrangement of the present invention, the mask setting part 44 is used for determining a false defect not to be detected. While coordinates are used in the mask setting part 44 as exemplified above, any other pattern data or feature quantity data of each candidate defect image is also applicable for identification. On a pattern edge, a degree of variation in detected signal out put dues not depend on, coordinates, and therefore pattern-edge feature quantity data is used for identification instead of coordinate data.
[0031] Further, while masking is made for non-inspection of candidate defects, as exemplified above, another inspection means, or a method of inspection based on another criterion is also applicable to examination of an area corresponding to a mask region. In this case, according to conditions specified by the user after inspection, a defect judgment can be formed again regarding candidate defects 40 stored in the candidate defect memory part 41 .
[0032] As described above, and according to the present invention, the user can set up a non-inspection region which is effective for a device having a complex, large pattern area to be inspected, such as a wafer. Further, in cases where a considerable difference is found in comparative inspection of detected images, even if the difference is not actually a defect, the present invention makes it possible to avoid false defect detection while carrying out detection of minuscule defects.
[0033] These and other objects, features and advantages of the invention will be apparent from the following mere particular description of preferred embodiments of the invention, as illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 is a schematic diagram of a conventional electron-beam pattern inspection apparatus;
[0035] FIG. 2 is a schematic diagram of a conventional optical pattern inspection apparatus;
[0036] FIG. 3 is a plan view showing a layout of a wafer;
[0037] FIG. 4 is a schematic diagram of an electron-beam pattern inspection apparatus, showing an arrangement of first problem-solving means according to the present invention;
[0038] FIG. 5 is a diagrammatic plan view illustrating operation of the first problem-solving means according to the present invention;
[0039] FIG. 6 is a diagram showing the layout of a defect check screen;
[0040] FIG. 7 is a diagram showing the layout of a mask region setting screen;
[0041] FIG. 8 is a schematic diagram showing the configuration of an electron-beam pattern inspection apparatus in a first preferred embodiment of the present invention;
[0042] FIG. 9 is a diagram showing a startup screen in the first preferred embodiment of the present invention;
[0043] FIG. 10 is a diagram showing a contrast adjustment screen for recipe creation in the first preferred embodiment of the present invention;
[0044] FIG. 11 is a diagram showing a trial inspection initial screen for recipe creation in the first preferred embodiment of the present invention;
[0045] FIG. 12 is a plan view of a wafer, showing a scanning sequence in the first preferred embodiment of the present invention;
[0046] FIG. 13 is a diagram showing a trial inspection defect check screen for recipe creation in the first preferred embodiment of the present invention;
[0047] FIG. 14 is a diagram showing a mask region setting screen for recipe creation in the first preferred embodiment of the present invention;
[0048] FIG. 15 is a diagram showing an inspection defect check screen in the first preferred embodiment of the present invention;
[0049] FIG. 16 is a schematic diagram showing the configuration of an electron-beam pattern inspection apparatus in a second preferred embodiment of the present invention;
[0050] FIG. 17 is a diagram showing an image processing region setting screen for recipe creation in the second preferred embodiment of the present invention;
[0051] FIG. 18 is a schematic diagram showing the configuration of an electron-beam pattern inspection apparatus in a third preferred embodiment of the present invention;
[0052] FIG. 19 is a diagram showing a defect check screen for recipe creation in the third preferred embodiment of the present invention; and
[0053] FIG. 20 is a diagram showing an image processing feature quantity data setup screen for recipe creation in the third preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0054] The present invention will now be described in detail by way of example with reference to the accompanying drawings.
Embodiment 1
[0055] A first preferred embodiment of the present invention will be described. FIG. 8 shows the configuration of an electron-beam pattern inspection apparatus according to the first preferred embodiment of the present invention. The electron-beam pattern inspection apparatus comprises an electron optical system 106 , including: an electron source 1 for emitting an electron beam 2 from an electron gun in which the electron beam 2 from the electron source 1 is extracted and accelerated by an electrode to produce a virtual electron source at a predetermined point through an electrostatic or magnetic field superimposing lens; a condenser lens 60 for converging the electron beam 2 from the virtual electron source at a predetermined convergence point; a blanking plate 63 which is equipped in the vicinity of the convergence point of the electron beam 2 for turning on/off the electron beam 2 ; a deflector 105 for deflecting the electron beam 2 in the X and Y directions; and an objective lens 4 for converging the electron beam 2 onto an object substrate (wafer 31 ).
[0056] Further, the electron-beam pattern inspection apparatus comprises a specimen chamber 107 in which the object substrate (wafer 31 ) is held in a vacuum; a stage 6 where the wafer 31 is mounted and to which a retarding voltage 108 is applied for enabling detection of an image at an arbitrary position; and a detector 8 for detecting secondary electrons 7 or the like produced from the object substrate to output a detected analog signal. An A/D converter 9 is provided for converting the detected analog signal into a digital image, which is stored in a memory 109 for storing digital image data, and an image processor circuit 10 compares the converted digital image with a reference digital image stored in the memory 109 and identifies a difference found in comparison as a candidate defect 40 . A candidate defect memory part 41 , which stores feature quantity data of each candidate defect 40 , such as coordinate data, projection length data and shape data, is provided in a general control part 110 , in which the overall apparatus control is conducted, with feature quantity data of each pattern defect 11 being received from the candidate defect memory part 41 . A mask region 42 (shown in FIG. 5 ) is set as region data, and a candidate defect located in the mask region 42 is flagged as a masked defect 43 (shown in FIG. 5 ) (control lines from the general control part 110 are not shown in FIG. 8 ). An operation display 45 is provided on which data of pattern defects 11 is displayed, an image of a selected pattern defect 11 is displayed, and the mask region 42 is displayed or edited.
[0057] Still further, the electron-beam pattern inspection apparatus comprises a keyboard, a mouse and a knob (not shown) for operation and control; a Z sensor for measuring the height level of each wafer 31 to maintain a focal point of a detected digital image through control of a current applied to the objective lens by adding an offset 112 ; a loader (not shown) for loading the wafer 31 from its cassette 114 to the specimen chamber 107 and for unloading the wafer 31 from the specimen chamber 107 to the cassette 114 ; an orientation flat detector (not shown) for positioning the wafer 31 according to the circumferential shape of the wafer 31 ; an optical microscope 118 for allowing observation of a pattern on the wafer 31 ; and a standard specimen 119 , which is set on the stage 6 .
[0058] Operations in the first preferred embodiment include a conditioning operation, in which a mask region 42 is set up, and an inspection operation, in which any candidate defect 40 detected in other than the mask region 42 is examined as a pattern defect.
[0059] In the conditioning operation, a user opens a startup screen shown in FIG. 9 on the operation display 45 . On a slot selection part 130 of the startup screen, the user selects a code number of a slot where the wafer 31 to be inspected is contained. Then, on a recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses a recipe creation start button 132 for starting the conditioning operation. The conditioning operation includes contrast setting for the electron optical system, pattern layout setting for the wafer 31 , pattern positioning alignment for the wafer 31 , calibration in which a signal level of the wafer 31 is checked at a position where the signal level is indicated accurately, inspection condition setting, mask region setting, and a setup condition check in trial inspection. The contrast setting, mask region setting, and trial inspection, which form essential parts of the present invention, will be described.
[0060] The general control part 110 provides operational instructions to each part in the following manner.
[0061] First, the general control part 110 issues an operational instruction to the loader (not shown) so that the loader takes the wafer 31 out of the cassette 114 . Then, through the use of the orientation flat detector (not shown), the circumferential shape of the wafer 31 is checked, and the wafer 31 is positioned according to the result of this check. The wafer 31 is then mounted on the stage 6 , and the specimen chamber 107 is evacuated. Simultaneously, the electron optical system and the retarding voltage 108 are conditioned. A voltage is applied to the blanking plate 63 to turn off the electron beam 2 . The stage 6 is moved so that the standard specimen 119 can be imaged, and an output of the Z sensor 113 is made effective. While a focal point of the electron beam 2 from the electron optical system is maintained at a position corresponding to “a value detected by the Z sensor 113 +an offset 112 ”, raster scanning is performed by the deflector 105 . In synchronization with this raster scanning, the voltage applied to the blanking plate 63 is turned off so that the wafer 31 is irradiated with the electron beam 2 as required. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , which then outputs a detected analog signal. Through the A/D converter 9 , the detected analog signal is converted into a digital image. By changing the offset 112 , a plurality of digital images are detected, and in the general control part 110 , an optimum offset for maximizing the sun of image differential values is determined. The optimum offset thus determined is set up as the current offset value.
[0062] After the optimum off set is established, the output of the Z sensor 113 is made ineffective, and a screen transition is made to the contrast adjustment screen shown in FIG. 10 . The contrast adjustment screen comprises: a map display part 55 having a map display area, a button for controlling display of the entire wafer or die map, and a mouse operation command button 140 for controlling position movement or item selection by the use of the mouse (not shown); an image display part 56 , having an image display area and an image changeover button 141 for setting an image magnification, for selecting an optical micrograph image attained through the optical microscope 118 or a SEM image attained through the electron optical system, and for specifying a kind of image; a recipe creation item selection button 142 ; a recipe creation end button 133 ; and a recipe save button 134 . On the contrast adjustment screen, the user sets the mouse operation command button 140 to a movement mode, and performs movement on the map by clicking the mouse to view an image at the current position on the image display part. Then, the user assigns an adjustment item of the electron optical system to the knob, and adjusts each part of the electron optical system to attain proper contrast.
[0063] The recipe creation end button 133 is used for terminating recipe creation; the recipe save button 134 is used for saving recipe condition data; and the recipe creation item selection button 142 is used for setting another condition and issuing an instruction for screen transition. These buttons are available on all of the screens. To open a trial inspection initial screen, as shown in FIG. 11 , the user sets the recipe creation item selection button 142 to a trial inspection item.
[0064] The trial inspection initial screen comprises a map display part 55 , a recipe creation end button 133 , a recipe save button 134 , a recipe creation item selection button 142 , an inspection start button 143 , and an inspection end bit ton 144 . The user sets the mouse operation command button 140 to a selection mode. Then, by clicking a die on the map display part 55 , the user can select/deselect the die for trial inspection. Each die can thus be selected for trial inspection. After selecting any die for trial inspection, the user presses the inspection start button 143 to start trial inspection. When trial inspection is started, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon. A pre-measured offset value inherent in the wafer 31 is added to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning line 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization with this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is turned off to let the electron beam 2 fall on the wafer 31 for scanning the surface thereof. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is attained. The digital image thus attained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases were the entire surface of the wafer 31 is inspected, the scanning sequence shown in FIG. 12 is adopted.
[0065] When the detection position A 35 is selected in the image processor circuit 10 , an image attained at the detection position A 35 is compared with an image attained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in the comparison, the difference is extracted as a candidate defect 40 to prepare a list of pattern defects 11 . The list of pattern defects 11 thus prepared is sent to the general control part 110 . In the general control part 110 , feature quantity data of each pattern defect 11 is taken out of the candidate defect memory part 41 . A pattern defect 11 located in the mask region 42 , which has been registered in a recipe, is flagged as a masked defect 43 (feature quantity data thereof is flagged). After completion of inspection of the entire region of interest, the user opens a trial inspection defect check screen shown in FIG. 13 .
[0066] The trial inspection defect check screen comprises a defect display editing part 150 for displaying feature quantity data of defects and editing classification thereof, a map display part 55 in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 , an image display part 56 in which an image taken at the current position is displayed, a display changeover button 151 for turning on/off masked defects 43 , and other buttons which have already been described. The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the nap display part 55 . Thus, an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 . At this step, if it is desired to treat the pattern defect 11 as a masked defect, a particular class code is assigned thereto. Thus, it can be identified as a masked defect on the map display part 55 . After completion of the defect classification, the user makes a transition to a mask region setting screen, as shown in FIG. 14 , by using the recipe creation item selection button, or the user returns to the trial inspection initial screen by pressing the inspection end button.
[0067] The mask region setting screen comprises a map display part 55 in which a current position indicator 59 indicating the current position, class code symbols of pattern, defects 11 and a mask region 42 are displayed on a layout of the wafer 31 ; an image display part 56 in which an image taken at the current position is displayed; a display changeover button 151 for turning on/off masked defects 43 , a new region button 160 for creating a new mask region; a completion button 161 for indicating the end of creation of a new mask region; and other buttons which have already described. Note that the map display part 55 presents the entire die region. The current position indicator 59 and pattern defects 11 in the entire die region are indicated in representation of on-die coordinates.
[0068] The user sets the mouse operation command button 140 to the movement mode, and then clicks in the vicinity of a class code of any defect to be masked for making movement thereto. Thus, an image of the defect to be masked is presented on the image display part 56 . If the user judges that a mask region should be formed, the user presses the new creation button 160 to select a region creation mode. In this mode, the user defines a mask region by clicking at the upper left corner and the lower right corner thereof on the image display part. The mask region thus defined (mask region 42 ) is indicated on the map display part 55 . After creating the mask region, as mentioned above, the user can turn on/off masked defects 43 by pressing the display changeover button 151 to confirm the location of the defect to be masked. When the mask region 42 is set tp as required, the user presses the recipe save button 134 for saving data of the mask region 42 in a recipe.
[0069] After saving the data of the mask region 42 , the user presses the completion button 161 to return to the trial inspection defect check screen. Further, on the trial inspection defect check screen, the user presses the inspection end button 144 to return to the trial inspection initial screen. Then, it is also possible for the user to select another die for trial inspection. For confirming and terminating the above-mentioned recipe creation session, the user presses the recipe creation end button 133 . Upon completion of the recipe creation, the wafer 31 is unloaded back to the cassette 114 .
[0070] The following description is directed to the inspection operation in which any candidate defect detected in other than the mask region is examined as a pattern defect. In the inspection operation, the user opens the startup screen shown in FIG. 9 on the operation display 45 . On the slot selection part 130 of the start tp screen, the user selects a code number of a slot were the wafer 31 to be inspected is contained. Then, on the recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses the inspection start button 330 for starting the inspection operation. After wafer loading, alignment and calibration are performed, inspection processing is carried out. Then, defect check and defect data output are performed, and wafer unloading is carried out at the end of inspection. The inspection processing and defect check, which form essential parts of the present invention, will now be described.
[0071] When the user presses the inspection start button 330 to indicate the start of inspection, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon. A pre-measured offset value inherent in the wafer 31 is added to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning line 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization with this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is turned off to let the electron beam 2 fall on the wafer 31 for scanning the surface thereof. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is attained. The digital image thus attained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases where the entire surface of the wafer 31 is inspected, the scanning sequence shown in FIG. 12 is adopted.
[0072] When the detection position A 35 is selected in the image processor circuit 10 , an image attained at the detection position A 35 is compared with an image attained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in comparison, the difference is extracted as a candidate defect 40 to prepare a list of pattern defects 11 . The list of pattern defects 11 thus prepared is sent to the general control part 110 . In the general control part 110 , feature quantity data of each pattern defect 11 is taken out of the candidate defect memory part 41 . A pattern defect 11 located in the mask region 42 , which has been registered in a recipe, is flagged as a masked defect 43 (feature quantity data thereof is flagged). After completion of inspection of the entire region of interest, the inspection defect check screen shown in FIG. 15 is opened.
[0073] The inspection defect check screen comprises a defect display editing part 150 for displaying feature quantity data of defects and editing classification thereof, a map display part 55 in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 , an image display part 56 in which an image taken at the current position is displayed, a display changeover button 151 for turning on/off masked defects 43 , and an inspection end button 144 for indicating the end of inspection.
[0074] The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the map display part 55 . Thus, an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 . Using the display changeover button 151 , the user can turn on/off masked defects 43 to check for any pattern defect in the mask region 41 . To terminate the inspection defect check session mentioned above, the user presses the inspection end button 144 . Each classified pattern defect 11 and feature quantity data thereof are stored into memory means (not shown) in the general control part 110 , and also delivered to external memory means (not shown) through a communication line (not shown) or to other inspection/observation means (not shown). Then, control is returned to the initial screen.
[0075] According to one aspect of the first preferred embodiment, the entire surface of each wafer can be inspected using a SEM image thereof without regard to pattern defects in the mask region 42 , i.e., true pattern defects 57 alone can be indicated to the user for easy identification thereof.
[0076] Further, according to another aspect of the first preferred embodiment, it is also possible to display masked defects in the mask region 42 . Therefore, in cases where rough patterning is used to form a redundant power wiring layer, the degree of roughness in patterning can be examined by turning on/off the masked defects.
[0077] Still further, according to another aspect of the first preferred embodiment, the mask region 42 can be set so as to mask false defects which have been identified under actual inspection conditions. It is therefore possible for the user to define proper masking.
[0078] Furthermore, according to another aspect of the first preferred embodiment, a different mask region 42 can be created additionally. Therefore, in cases where masking has been defined using an object containing a small degree of random variation, the user can set up a new mask region additionally for providing proper masking as required.
[0079] In a first modified form of the first preferred embodiment, mask region management may be implemented in a part of image processing function hardware, instead of using the general control part that is a computer system. In this modified arrangement, essentially the same functionality is provided. Since the number of detectable defects is limited in terms of output capacity, this limitation can be removed by using image processing function hardware for mask region management.
[0080] In a second modified form of the first preferred embodiment, plural kinds of mask regions may be set up while only one kind of mask region has been treated in the forgoing description. In this modified arrangement, false defects due to plural kinds of causes can be classified for defect data management. By turning on/off indications of false defects according to each kind of cause, the user can check the conditions thereof. Thus, it is possible for the user to preclude only minimum false defects for carrying out proper inspection.
[0081] In a third modified form of the first preferred embodiment, a mask region on the mask region setting screen may be automatically defined as a rectangular region having a size approximately two tines as large as the projection length of any false defect not to be detected. By merging neighboring mask regions, a mask region is determined using data of pattern defects classified without intervention of the user. In this modified arrangement, a flask region can be generated precisely through automatic operation. For example, masking at hundreds of points can be provided automatically so as to allow for easy identification. As a further modified form of this modification, there may be provided an arrangement in which an automatically determined mask region can be redefined or edited.
[0082] In a fourth modified form of the first preferred embodiment, a mask region may be determined using design data in inspection of rough patterning for power wiring, ion implantation, or the like. In this modified arrangement, the user can set up a mask region for each kind of false defect while saving the time of input.
[0083] In a fifth modified form of the first preferred embodiment, pattern defects are indicated on layout information at a networked CAD display terminal instead of being indicated on layout information stored in the inspection apparatus. In this modified arrangement, possible defects on each layer in rough patterning and fine patterning can be identified with ease.
Embodiment 2
[0084] A second preferred embodiment of the present invention will be described. FIG. 16 shows an example of the configuration of an electron-beam pattern inspection apparatus according to the second preferred embodiment of the present invention. The electron-beam pattern inspection apparatus comprises an electron optical system including: an electron source 1 , for emitting an electron beam 2 from an electron gun in which the electron beam 2 from the electron source 1 is extracted and accelerated by an electrode to produce a virtual electron source at a predetermined point through an electrostatic or magnetic field superimposing lens; a condenser lens 60 for converging the electron beam 2 from the virtual electron source at a predetermined convergence point; a blanking plate 63 which is equipped in the vicinity of the convergence point of the electron beam 2 for turning on/off the electron beam 2 ; a deflector 105 for deflecting the electron beam 2 in the X and Y directions; and an objective lens 4 for converging the electron beam 2 onto an object substrate.
[0085] Further, the electron-beam pattern inspection apparatus comprises a specimen chamber 107 in which the object substrate (wafer 31 ) is held in a vacuum; a stage 6 where the wafer 31 is mounted and to which a retarding voltage 108 is applied for enabling detection of an image at an arbitrary position; and a detector 8 for detecting secondary electrons 7 or the like produced from the object substrate to output a detected analog signal. An A/D converter 9 is provided for converting the detected analog signal into a digital image, which is stored in a memory 109 for storing digital image data, and an image processor circuit 202 compares the converted digital image with a reference digital image stored in the memory 109 and identifies a difference, found in the comparison by changing an image processing condition 201 for each image processing region 200 , as a pattern defect 11 . A general control part 110 is provided, in which feature quantity data of each pattern defect 11 , such as coordinate data, projection length data and shape data, is handled (control lines from the general control part 110 are not shown in FIG. 16 ); and an operation display 45 is provided on which data of pattern defects 11 is displayed, an image of a selected pattern defect 11 is displayed, and each image processing region 200 is displayed or edited.
[0086] Still further, the electron-beam pattern inspection apparatus comprises a keyboard, a mouse and a knob (not shown) for operation and control; a Z sensor 113 for measuring the height level of each wafer 31 to maintain a focal point of a detected digital image through control of a current applied to the objective lens by adding an offset 112 ; a loader (not shown) for loading the wafer 31 from its cassette 114 to the specimen chamber 107 and unloading the wafer 31 from the specimen chamber 107 to the cassette 114 ; an orientation flat detector (not shown) for positioning the wafer 31 according to the circumferential shape of the wafer 31 ; an optical microscope 118 for allowing observation of a pattern on the wafer 31 ; and a standard specimen 119 which is set on the stage 6 .
[0087] Operations in the second preferred embodiment include a conditioning operation, in which an image processing region 200 and an image processing condition 201 thereof are set up, and an inspection operation, in which pattern defects 11 are detected.
[0088] In the conditioning operation, the user opens the startup screen shown in FIG. 9 on the operation display 45 . On a slot selection part 130 of the startup screen, the user selects a code number of a slot where the wafer 31 to be inspected is contained. Then, on a recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses a recipe creation start button 132 for starting the conditioning operation. The conditioning operation includes contrast setting for the electron optical system, pattern layout setting for the wafer 31 , pattern positioning alignment for the wafer 31 , calibration in which a signal level of the wafer 31 is checked at a position were the signal level is indicated accurately, inspection condition setting image processing region setting for specifying an image processing region 200 and an image processing condition 201 thereof, and setup condition check in trial inspection. The contrast setting, image processing region setting, and trial inspection, which form essential parts of the present invention, will now be described.
[0089] The general control part 110 provides operational instructions to each part in the following manner. First, the general control part 110 issues an operational instruction to the loader (not shown) so that the loader takes the wafer 31 out of the cassette 114 . Then, through the use of the orientation flat detector (not shown), the circumferential shape of the wafer 31 is checked, and the wafer 31 is positioned according to the result of this check. The wafer 31 is then mounted on the stage 6 , and the specimen chamber 107 is evacuated. Simultaneously, the electron optical system and the retarding voltage 108 are conditioned. A voltage is applied to the blanking plate 63 to turn off the electron beam 2 . The stage 6 is moved so that the standard specimen 119 can be imaged, and an output of the Z sensor 113 is made effective. While a focal point of the electron beam 2 is maintained at a position corresponding to “a value detected by the Z sensor 113 +an offset 112 ”, raster scanning is performed by the deflector 105 . In synchronization with this raster scanning, the voltage applied to the blanking plate 63 is turned off so that the wafer 31 is irradiated with the electron beam 2 as required. Backscattered, electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , which then outputs a detected analog signal. Through the A/D converter 9 , the detected analog signal is converted into a digital image. By changing the offset 112 , a plurality of digital images are detected, and in the general control part 110 , an optimum offset for maximizing the sum of image differential values is determined. The optimum offset 111 thus determined is set up as the current offset value.
[0090] After the optimum offset is established, the output of the Z sensor 113 is made ineffective and a screen transition is made to a contrast adjustment screen, such as shown in FIG. 10 . The contrast adjustment screen comprises: a map display part 55 having a map display area, a button for controlling display of the entire wafer or die map, and a mouse operation command button 140 for controlling position movement or item selection by the use of the mouse 121 (not shown); an image display part 56 having an image display area and an image changeover button 141 for setting an image magnification, selecting an optical micrograph image attained through the optical microscope 118 or a SEM image attained through the electron optical system, and specifying a kind of image; a recipe creation item selection button 142 ; a recipe creation end button 133 ; and a recipe save button 134 . On the contrast adjustment screen, the user sets the mouse operation command button 140 to a movement mode, and performs movement on the map by clicking the mouse to view an image at the current position on the image display part. Then, the user assigns an adjustment item of the electron optical system to the knob, and adjusts each part of the electron optical system to attain proper contrast.
[0091] The recipe creation end button 133 is used for terminating recipe creation; the recipe save button 134 is used for saving recipe condition data; and the recipe creation item selection button 142 is used for setting another condition and issuing an instruction for screen transition. These buttons are available on all the screens. To open a trial inspection initial screen, such as shown in FIG. 11 , the user sets the recipe creation item selection button 142 to a trial inspection item.
[0092] The trial inspection initial screen comprises a map display part 55 , a recipe creation end button 133 , a recipe save button 134 , a recipe creation item selection button 142 , an inspection start button 143 , and an inspection end button 144 . The user sets the mouse operation command bitten 140 to a selection mode. Then, by clicking a die on the map display part 55 , the user can select/deselect a die for trial inspection. Each die can thus be selected for trial inspection. After selecting any die for trail inspection, the user presses the inspection start button 143 to start trial inspection. When trial inspection is started, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon.
[0093] A pre-measured offset value inherent in the wafer 31 is added to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning line 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization with this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is turned off to let the electron beam 2 fall on the wafer 31 , for scanning the surface thereof. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is attained. The digital image thus attained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases where the entire surface of the wafer 31 is inspected, the scanning sequence shown in FIG. 12 is adopted.
[0094] When the detection position A 35 is selected in the image processor circuit 202 , an image attained at the detection position A 35 is compared with an image attained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in comparison, the difference is extracted as a pattern defect 11 to prepare a list of pattern defects 11 . The list of pattern defects 11 thus prepared is sent to the general control part 110 . After completion of inspection of the entire region of interest, the user opens a trial inspection defect check screen, such as shown in FIG. 13 .
[0095] The trial inspection defect check screen comprises a defect display editing part 150 for displaying feature quantity data of defects and editing classification thereof a map display part 55 in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 , an image display part 56 in which an image taken at the current position is displayed, a display changeover button 151 for turning on/off masked defects 43 , and other buttons which have already been described.
[0096] The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the map display part 55 . Thus, an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 . At this step, if it is desired to treat the pattern defect 11 as a masked defect, a particular class code is assigned thereto. Thus, it can be identified as a masked defect on the map display part 55 . After completion of the defect classification, the user makes a transition to an image processing region setting screen shown in FIG. 17 by using the recipe creation item selection button, or the user returns to the trial inspection initial screen by pressing the inspection end button.
[0097] The image processing region setting screen comprises a map display part 55 in which a current position indicator 59 indicating the current position, class code symbols of pattern defects 11 , and an image processing region 200 are displayed on a layout of the wafer 31 ; an image display part 56 in which an image taken at the current position is displayed; a defect redisplay button 207 for defect indication based on feature quantity image data of each pattern defect 11 ; a new region button 160 for creating a new region; a completion button 161 for indicating the end of creation of a new region, and other buttons which have already described. Note that the map display part 55 presents the entire die region. The current position indicator 59 and pattern defects 11 in the entire die region are indicated in representation of on-die coordinates. The user sets the mouse operation command button 140 to the movement mode, and then clicks in the vicinity of a class code of any defect corresponding to the image processing condition 201 to be changed for making movement thereto. Thus, an image of the defect of interest is presented on the image display part 56 .
[0098] If the user judges that the image processing condition 201 should be changed, the user presses the new creation button 160 to select a region creation mode. In this mode, the user defines a region by clicking at the upper left corner and the lower right corner thereof on the image display part, and the user provides a correspondence between an image processing condition number 206 of the region and a class code. Reference is made to the feature quantity image data 203 of a pattern defect 11 having the class code which corresponds to the image processing condition number, and the image processing condition 201 is set up for the image processing condition number so that all-defects detection will not be made by the image processor circuit or software in the general control part (computer). As required, the user adjusts the image processing condition 201 manually. Using a special condition on/off button 208 , the user specifies whether or not the image processing condition 201 is to be applied at the time of inspection. On the map display part 55 , the defined region is indicated as an image processing region 200 together with the image processing condition number. After creating the image processing region 200 as mentioned above, the user presses the defect redisplay button 207 to confirm that each pattern defect 11 belonging to the image processing region 200 is not indicated. When the image processing region 200 is set up as required, the user presses the recipe save bitten 134 . Thus, data regarding the image processing region 200 , the image processing condition number corresponding thereto, and the image processing condition 201 for each image processing number are saved in a recipe.
[0099] After saving the above data, the user presses the completion button 161 to return to the trial inspection defect check screen. Further, on the trial inspection defect check screen, the user presses the inspection end button 144 to return to the trial inspection initial screen. Then, it is possible for the user to select another die for trial inspection. For confirming and terminating the above-mentioned recipe creation session, the user presses the recipe creation end button 133 . Upon completion of the recipe creation, the wafer 31 is unloaded back to the cassette 114 .
[0100] The following describes the inspection operation. In the inspection operation, the user opens the startup screen shown in FIG. 9 on the operation display 45 . On the slot selection part 130 of the startup screen, the user selects a code number of a slot where the wafer 31 to be inspected is contained. Then, on the recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses an inspection start button 330 for starting the inspection operation. After wafer loading, alignment and calibration are performed, inspection processing is carried out. Then, defect check and defect data output are performed, and wafer unloading is carried out at the end of inspection. The inspection processing and defect check, which form essential parts of the present invention, will now be described.
[0101] When the user presses the inspection start button 330 to indicate the start of inspection, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon. A pre-measured offset value inherent in the wafer 31 is added to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning line 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization of this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is tuned off to let the electron beam 2 fall en the wafer 31 for scanning the surface thereof. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is attained. The digital image thus attained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases where the entire surface of the wafer 31 is to be inspected, the scanning sequence shown in FIG. 12 is adopted.
[0102] When the detection position A 35 is selected in the image processor circuit 202 , an image attained at the detection position A 35 is compared with an image attained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in comparison, the difference is extracted as a pattern defect 11 to prepare a list of pattern defects 11 . The list of pattern defects 11 thus prepared is sent to the general control part 110 . After completion of inspection of the entire region of interest, an inspection defect check screen, such as shown in FIG. 15 , is opened.
[0103] The inspection defect check screen comprises a defect display editing part 150 for displaying feature quantity data of defects and editing classification thereof, a map display part 55 in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 , an image display part 56 in which an image taken at the current position is displayed, a display changeover button 151 for turning on/off masked defects 43 , and an inspection end button 144 for indicating the end of inspection. The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the map display part 55 . Thus, an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 .
[0104] A display changeover button 209 is provided for turning on/off the display for the image processing condition 201 in the image processing region 200 . With this button, the user can perform a display changeover according to whether or not the image processing condition 201 is applied to each pattern defect 11 in the image processing region 200 . If, by using the special condition on/off button 208 , the user has specified that the image processing condition 201 is to be applied at the time of inspection, a display changeover with the image display changeover button 209 is not available since the image processing condition 201 is already applied. To terminate the inspection defect check session mentioned above, the user presses the inspection end button 144 . Each classified pattern defect 11 and feature quantity data thereof are stored into memory means (not shown) in the general control part 110 , and they are also delivered to external memory means (not shown) through a communication line (not shown) or to other inspection/observation means (not shown). Then, control is returned to the initial screen.
[0105] According to one aspect of the second preferred embodiment, the entire surface of each wafer can be inspected using a SEM image thereof without regard to pattern defects in the image processing region 200 , i.e., true pattern defects 57 only can be indicated to the user for easy identification thereof.
[0106] Further, according to another aspect of the second preferred embodiment, it is possible to display defects in the image processing region 200 . Therefore, in cases where rough patterning is used to form a redundant power wiring layer, the degree of roughness in patterning can be examined by means of display changeover.
[0107] Still further, according to another aspect of the second preferred embodiment, an image processing condition can be set so that false defects identified under actual inspection conditions will not be detected. It is therefore possible for the user to specify a threshold properly just as required.
[0108] Furthermore, according to another aspect of the second preferred embodiment, a different image processing region 200 can be created additionally. Therefore, in cases where the image processing condition 201 has been defined using an object containing a small degree of random variation, the user can set up a new image processing region additionally to provide proper conditioning for image processing as required.
[0109] Moreover, according to another aspect of the second preferred embodiment, the image processing condition 201 is adjustable without completely deleting data of pattern defects 11 an the image processing region 200 . Therefore, the user can adjust the image processing condition 201 so that false defect detection will be prevented as required while possible defects remain inspectable.
[0110] Still further, according to another aspect of the second preferred embodiment, in cases where, by using the special condition on/off button 208 , the user has specified that the image processing condition 201 is not to be applied at the time of inspection, it is possible to alter the image processing region 200 and the image processing condition 201 . Therefore, even if it becomes necessary to provide a different image processing condition due to variation in a fabrication process, the user has only to adjust the image processing condition 201 . Thus, inspection can be carried out using feature quantity data acquired already.
Embodiment 3
[0111] A third preferred embodiment of the present invention will now be described.
[0112] FIG. 18 shows an example of the configuration of an electron-beam pattern inspection apparatus according to the third preferred embodiment of the present invention. The electron-beam pattern inspection apparatus comprises an electron optical system including: an electron source 1 for emitting an electron beam 2 in the form of an electron gun in which the electron beam 2 from the electron source 1 is extracted and accelerated by an electrode to produce a virtual electron source at a predetermined point through an electrostatic or magnetic field superimposing lens; a condenser lens 60 for converging the electron beam 2 from the virtual electron source at a predetermined convergence point; a blanking plate 63 which is equipped in the vicinity of the convergence point of the electron beam 2 for turning on/off the electron beam 2 ; a deflector 105 for deflecting the electron beam 2 in the X and Y directions; and an objective lens 4 for converging the electron beam 2 onto an object substrate 5 .
[0113] Further, the electron-beam pattern inspection apparatus comprises: a specimen chamber 107 in which the object substrate (wafer 31 ) is held in a vacuum; a stage 6 where the wafer 31 is mounted and to which a retarding voltage 108 is applied for enabling detection of an image at an arbitrary position; and a detector 8 for detecting secondary electrons 7 or the like produced from the object substrate to output a detected analog signal. An A/D converter 9 is provided for converting the detected analog signal into a digital image, which is stored in a memory 109 for storing digital image data, and an image processor circuit 10 compares the converted digital image with a reference digital image stored in the memory 109 and identifies a difference found in the comparison as a candidate defect 40 . A candidate defect memory part 41 is provided for storing feature quantity data 203 of each candidate defect 40 , such as coordinate data, projection length data and shape data. A feature quantity check part 251 is provided in which feature quantity data 203 of each candidate defect 40 is received from the candidate defect memory part 41 and it is checked to see whether the candidate defect 40 meets prespecified feature quantity data 250 . A detail image processing part 252 is provided in which, under an image processing condition 201 specified for each feature quantity data, a judgment for determining each pattern defect 11 is formed on the candidate defect 40 that has proved to meet the prespecified, feature quantity data 250 as determined by the feature quantity data check part 251 , and a general control part 110 receives data of each pattern defect 11 from the detail image processing part 252 (control lines from the general control part 110 are not shown in FIG. 18 ). An operation display 45 is provided on which data of pattern defects 11 is displayed, an image of a selected pattern defect 11 is displayed, and the image processing region 200 is displayed or edited.
[0114] Still further, the electron-beam pattern inspection apparatus comprises a keyboard, a mouse and a knob (not shown) for operathen and control; a Z sensor 113 for measuring the height level of each wafer 31 to maintain a focal point of a detected digital image through control of a current applied to the objective lens by adding an offset 112 ; a loader (not shown) for loading the wafer 31 from its cassette 114 to the specimen chatter 107 and unloading the wafer 31 from the specimen chamber 107 to the cassette 114 ; an orientation flat detector (not shown) for positioning the wafer 31 according to the circumferential shape of the wafer 31 ; an optical microscope 118 for providing for observation of a pattern on the wafer 31 ; and a standard specimen 119 which is set en the stage 6 .
[0115] Operations in the third preferred embodiment include a conditioning question, in which feature quantity data 250 and an image processing condition 201 thereof are set up, and an inspection operation, in which pattern defects 11 are detected.
[0116] In the conditioning operation, the user opens the startup seen shown in FIG. 9 on the operathen display 45 . On a slot selection part 130 of the startup screen, the user selects a code number of a slot where the wafer 31 to be inspected is contained. Then, on a recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses a recipe creation start button 132 for starting the conditioning operation. Conditioning operation includes contrast setting for the electron optical system, pattern layout setting for the wafer 31 , pattern positioning alignment for the wafer 31 , calibration in which a signal level of the wafer 31 is checked at a position where the signal level is indicated accurately, inspection condition setting, image processing feature quantity data setting for specifying feature quantity data 250 and an image processing condition 201 thereof, and setup condition check in trial inspection. The contrast setting, image processing feature quantity data setting, and trial inspection, which form essential parts of the present invention, will now be described.
[0117] The general control part 110 provides operational instructions to each part in the following manner. First, the general control part 110 issues an operational instruction to the loader (not shown) so that the loader takes the wafer 31 out of the cassette 114 . Then, through the use of the orientation flat detector (not shown), the circumferential shape of the wafer 31 is checked, and the wafer 31 is positioned according to the result of this check. The wafer 31 is then mounted on the stage 6 , and the specimen chamber 107 is evacuated. Simultaneously, the electron optical system 106 and the retarding voltage 108 are conditioned. A voltage is applied to the blanking plate 63 to turn off the electron beam 2 . The stage 6 is moved so that the standard specimen 119 can be imaged, and an output of the Z sensor 113 is made effective. While a focal point of the electron beam 2 is maintained at a position corresponding to “a value detected by the Z sensor 113 +an offset 112 ”, raster scanning is performed by the deflector 105 . In synchronization with this raster scanning, the voltage applied to the blanking plate 63 is turned off so that the wafer 31 is irradiated with the electron beam 2 as required.
[0118] Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , which then outputs a detected analog signal. Through the A/D converter 9 , the detected analog signal is converted into a digital image. By changing the offset 112 , a plurality of digital images are detected, and in the general control part 110 , an optimum offset for maximizing the sun of image differential values is determined. The optimum offset thus determined is set up as the current offset value. After the optimum offset is established, the output of the Z sensor 113 is made ineffective, and a screen transition is made to a contrast adjustment screen, such as shown in FIG. 10 .
[0119] The contrast adjustment screen comprises: a map display part 55 having a map display area, a button for controlling display of the entire wafer or die, map, and a mouse operation command button 140 for controlling position movement or item selection by the use of the mouse (not shown); an image display part 56 having an image display area and an image changeover button 141 for setting an image magnification, selecting an optical micrograph image obtained through the optical microscope 118 or a SEM image obtained through the electron optical system, and specifying a kind of image; a recipe creation item selection button 142 ; a recipe creation end button 133 ; and a recipe save button 134 .
[0120] On the contrast adjustment screen, the user sets the mouse operation command button 140 to a movement mode, and performs movement on the map by clicking the mouse to view an image at the current position on the image display part. Then, the user assigns an adjustment item of the electron optical system, to the knob, and adjusts each part of the electron optical system to attain proper contrast. The recipe creation end button 133 is used for terminating recipe creation, the recipe save button 134 is used for saving recipe condition data; and the recipe creation item selection button 142 is used for setting another condition and issuing an instruction for screen transition. These buttons are available on all the screens. To open a trial inspection initial screen, such as shown in FIG. 11 , the user sets the recipe creation item selection button 142 to a trial inspection item.
[0121] The trial inspection initial screen comprises a map display part 55 , a recipe creation end button 133 , a recipe save button 134 , a recipe creation item selection button 142 , an inspection start button 143 , and an inspection end bit ton 144 . The user sets the mouse operation command button 140 to a selection mode. Then, by clicking a die on the map display part 55 , the user can select/deselect the die for trial inspection. Each die can thus be selected for trial inspection. After selecting any die for trial inspection, the user presses the inspection start button 143 to start trial inspection. When trial inspection is started, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon. A pre-measured offset value inherent in the wafer 31 is abed to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning fine 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization with this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is turned off to let the electron beam 2 fail on the wafer 31 for scanning the surface thereof.
[0122] Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is obtained. The digital image thus obtained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases where the entire surface, of the wafer 31 is inspected, a scanning sequence shown in FIG. 12 is carried out.
[0123] When the detection position A 35 is selected in the image processor circuit 10 , an image obtained at the detection position A 35 is compared with an image obtained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in comparison, the difference is extracted as a candidate defect 40 and feature quantity data of the candidate defect 40 is stored into the candidate defect memory part 41 . Simultaneously at the feature quantity data check part 251 , it is checked to see whether the candidate defect 40 meets prespecified feature quantity data 250 or not. If the candidate defect 40 meets the prespecified feature quantity data 250 , data of the candidate defect 40 is sent to the detail image processing part 252 . Then, in the detail image processing part 252 , image processing is carried out under an image processing condition 201 determined for each prespecified feature quantity data to check whether the candidate defect 40 is a pattern defect 11 or not. If the candidate defect 40 is recognized as a pattern defect 11 , an identification, code thereof stored in the candidate defect memory part 41 is sent to the general control part 110 . After completion of inspection of the entire region of interest, a defect check screen, such as shown in FIG. 19 , is opened.
[0124] The defect check screen comprises a defect display editing part 150 for displaying feature quantity data of defects and editing classification thereof; a map display part 55 , in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 ; an image display part 56 , in which an image taken at the current position is displayed; a real/memory image display changeover button 255 for effecting a changeover between a real, image display and a memory image display, and other buttons which have already been described. The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the map display part 55 . Then, if a real image selection has been made with the real/memory image changeover button 255 , a coordinate location of the pattern defect 11 is taken for image acquisition. If a memory image selection has been made with the real/memory image changeover button 255 , an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 . At this step, if it is desired to treat the pattern defect 11 as a defect not to be detected 58 , a particular class code is assigned thereto. Thus, it can be identified as a defect not to be detected on the map display part 55 . After completion of the defect classification, the user makes a transition to an image processing feature quantity data setting screen, as shown in FIG. 20 , using the recipe creation item selection button, or the user returns to the trial inspection initial screen by pressing the inspection end button.
[0125] The image processing feature quantity data setting screen comprises a class code specifying part 262 for specifying a class code of interest 261 ; a defect selection part 263 for selecting defects having the class code of interest in succession; a feature quantity data specifying part 264 for specifying feature quantity data of each selected defect and feature quantity data 250 used as a selection criterion; a map display part 55 ; an image display part 56 , in which an image of each defect 11 is displayed; an image processing condition setting part 265 for setting up an image processing condition number corresponding to an image processing condition 201 to be applied to an image selected by the feature quantity data specifying part 264 ; a defect redisplay button 207 for indicating on the map display part 55 the result of judgment attained after an evaluation image processing part 252 checks to see whether or not an image in the candidate defect memory part 41 is a pattern defect 11 ; a new feature quantity data creation button 266 for creating a new image processing condition number corresponding to prespecified feature quantity data 250 ; a completion button 161 for indicating the end of creation of new feature quantity data; and other buttons which have already described. The recipe save button 134 is provided for saving data in a recipe.
[0126] After saving the data, the user presses the completion button 161 to return to the trial inspection defect check screen. Further, en the trial inspection defect check screen, the user presses the inspection end button 144 to return to the trial inspection initial screen. Then, it is possible for the user to select another die for trial inspection. For confirming and terminating the above-mentioned session, the user presses the recipe creation end button 133 . Upon completion of the recipe creation, the wafer 31 is unloaded back to the cassette 114 .
[0127] The inspection operation will now be described. In the inspection operation, the user opens the startup screen shown in FIG. 9 on the operation display 45 . On the slot selection part 130 of the startup screen, the user selects a code number of a slot where the wafer 31 to be inspected is contained. Then, on the recipe selection part 131 , the user specifies a product type of the wafer 31 and a process step thereof, and the user presses an inspection start button 330 for starting the inspection operation. After wafer loading, alignment and calibration are performed, inspection processing is carried out. Then, defect check and defect data output are performed, and wafer unloading is carried out at the end of inspection. The inspection processing and defect check, which form essential parts of the present invention, will now be described.
[0128] When the user presses the inspection start button 330 to indicate the start of inspection, the stage 6 is driven for movement to a scanning start position of the region to be inspected on the wafer 31 mounted thereon. A pre-measured offset value inherent in the wafer 31 is added to the offset 112 , and the Z sensor 113 is made effective. Then, along the scanning line 33 shown in FIG. 3 , the stage 6 is scanned in the Y direction. In synchronization of this stage scanning, the deflector 105 is scanned in the X direction. During a period of effective scanning, a voltage to the blanking plate 63 is turned off to let the electron beam 2 fall on the wafer 31 for scanning the surface thereof. Backscattered electrons or secondary electrons produced from the wafer 31 are detected by the detector 8 , and through the A/D converter 9 , a digital image of the stripe region 34 is obtained. The digital image thus attained is stored into the memory 109 . After completion of the scanning operation of the stage 6 , the Z sensor 113 is made ineffective. The entire region of interest can be inspected by repeating stage scanning. In cases where the entire surface of the wafer 31 is inspected, the scanning sequence shown in FIG. 12 is employed.
[0129] When the detection position A 35 is selected in the image processor circuit 202 , an image obtained at the detection position A 35 is compared with an image obtained at the detection position B 36 , which has been stored in the memory 109 . If any difference is found in comparison, the difference is extracted as a candidate defect 40 and stored in the candidate defect memory part 41 . Further, the feature quantity data check part 251 selects a candidate defect meeting the prespecified feature quantity data, and using an image processing condition 201 determined by an image processing condition number corresponding to the prespecified feature quantity data, the detail image processing part 252 formed a judgment on whether or not the candidate defect 40 is a pattern defect 11 so as to prepare a list of pattern defects 11 . The list of pattern defects 11 thus prepared is sent to the general control part 110 . After completion of inspection of the entire region of interest, a defect check screen such as shown in FIG. 15 is opened.
[0130] The defect check screen comprises a defect display editing part 150 for displaying feature quantity, data of defects and editing classification thereof; a map display part 55 , in which a current position indicator 59 indicating the current position and class code symbols of pattern defects 11 are displayed on a layout of the wafer 31 ; an image display part 56 in which an image taken at the current position is displayed; a display changeover button 151 for turning on/off candidate defects 41 with pattern defects 11 indicated; and an inspection end bit ten 144 for indicating the end of inspection.
[0131] The user sets the mouse operation command button 140 to the selection mode, and then clicks any pattern defect 11 indicated on the map display part 55 . Thus, an image of the pattern defect 11 is presented on the image display part 56 , and feature quantity data thereof is presented on the defect display editing part 150 . On the defect display editing part 150 , the pattern defect 11 is subjected to classification according to the image and feature quantity data thereof, i.e., a class code is assigned to the feature quantity data of the pattern defect 11 . A display changeover button 209 is provided for turning on/off the display for the image processing condition 201 in the image processing region 200 . With this button, the user can perform a display changeover according to whether or not the image processing condition 201 is applied to each pattern defect 11 in the image processing region 200 . If, by using the special condition on/off button 208 , the user has specified that the image processing condition 201 is to be applied at the time of inspection, a display changeover with the image display changeover button 209 , is not available, since the image processing condition 201 is already applied. To term mate the inspection defect check session mentioned above, the user presses the inspection end button 144 . Each classified pattern defect 11 and feature quantity data thereof are stored into memory means (not shown) in the general control part 110 , and they are also delivered to external memory means (not shown) through a communication line (not shown) or to other inspection/observation means (not shown). Then, control is returned to the initial screen.
[0132] According to one aspect of the third preferred embodiment, the entire surface of each wafer can be inspected using a SEM image thereof to detect true pattern defects 57 only. Thus, the user can identify the true pattern defects 57 with ease.
[0133] Further, according to another aspect of the third preferred embodiment, in cases where rough patterning is used to form a redundant power wiring layer or a pattern edge, the degree of roughness in patterning can be examined by means of display changeover.
[0134] Still further, according to another aspect of the third preferred embodiment, an image processing condition can be set so that false defects identified under actual inspection conditions will not be detected. It is therefore possible for the user to specify a threshold properly just as required.
[0135] Furthermore, according to another aspect of the third preferred embodiment, the image processing condition 201 is adjustable without completely deleting data of pattern defects 11 in the image processing region 200 . Therefore, the user can adjust the image processing condition 201 so that false defect detection will be prevented as require d while possible defects remain inspectable.
[0136] As set forth hereinabove, and according to the present invention, the user can set up a non-inspection region that is effective for a device having a complex, large pattern area to be inspected, such as a wafer. Further, in cases where a considerable difference is found in comparative inspection of detected images, even if the difference is not actually a defect, the present invention makes it possible to avoid false defect detection while carrying out detection of minuscule defects.
[0137] The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description and all changes which care within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
|
An apparatus for processing a defect candidate image, including: a scanning electron microscope for taking an enlarged image of a specimen by irradiating and scanning a converged electron beam onto the specimen and detecting charged particles emanated from the specimen by the irradiation; an image processor for processing the image taken by the scanning electron microscope to detect defect candidates on the specimen and classify the detected defect candidates into one of plural classes; a memory for storing output from the image processor including images of the detected defect candidates; and a display unit which displays information stored in the memory and an indicator, wherein the display unit displays a distribution of the detected and classified defect candidates in a map format by distinguishing by the classified class, and the display unit also displays an image of a defect candidate stored in the memory together with the map which is indicated on the map by the indicator.
| 6
|
RELATED APPLICATIONS
The present invention claims priority to U.S. provisional applications Ser. Nos. 60/401,464 and 60/401,416, filed Aug. 5, 2002, the disclosures of which are incorporated by reference herein. The present application is also related to U.S. application Ser. No. 10/619,051 filed Jul. 14, 2003.
TECHNICAL FIELD
The present invention relates generally to a control apparatus for controlling a system of an automotive vehicle in response to sensed dynamic behavior, and more specifically, to a method and apparatus for desensitizing the activation criteria based on vehicle operating conditions.
BACKGROUND
Dynamic control systems for automotive vehicles have recently begun to be offered on various products. Dynamic control systems typically control the yaw of the vehicle by controlling the braking effort at the various wheels of the vehicle. Yaw control systems typically compare the desired direction of the vehicle based upon the steering wheel angle and the direction of travel. By regulating the amount of braking at each corner of the vehicle, the desired direction of travel may be maintained. Typically, the dynamic control systems do not address rollover (wheels lifting) of the vehicle. For high profile vehicles in particular, it would be desirable to control the rollover characteristic of the vehicle to maintain the vehicle position with respect to the road. That is, it is desirable to maintain contact of each of the four tires of the vehicle on the road.
In vehicle rollover control, it is desired to alter the vehicle attitude such that its motion along the roll direction is prevented from achieving a predetermined limit (rollover limit) with the aid of the actuation from the available active systems such as controllable brake system, steering system and suspension system. Although the vehicle attitude is well defined, direct measurement is usually impossible.
During a potential vehicular rollover event, wheels on one side of the vehicle start lifting, and the roll center of the vehicle shifts to the contact patch of the remaining tires. This shifted roll center increases the roll moment of inertia of the vehicle, and hence reduces the roll acceleration of the vehicle. However, the roll attitude could still increase rapidly. The corresponding roll motion when the vehicle starts side lifting deviates from the roll motion during normal driving conditions.
When the wheels start to lift from the pavement, it is desirable to confirm this condition. This allows the system to make an accurate determination as to the appropriate correction. If wheels are on the ground, or recontact the ground after a lift condition, this also assists with accurate control.
Some systems use position sensors to measure the relative distance between the vehicle body and the vehicle suspension. One drawback to such systems is that the distance from the body to the road must be inferred. This also increases the number of sensors on the vehicle. Other techniques use sensor signals to indirectly detect wheel lifting qualitatively.
One example of a wheel lifting determination can be found in Ford U.S. Pat. No. 6,356,188 and U.S. patent application number 7,109,856, both of which are incorporated by reference herein. The system applies a change in torque to the wheels to determine wheel lift. The output from such a wheel lifting determination unit can be used qualitatively. This method is an active determination since the basis of the system relies on changing the torque of the wheels by the application of brakes or the like. In some situations it may be desirable to determine wheel lift without changing the torque of a wheel.
Due to the inevitable dead spots due to the vehicle configuration, wheel lift detection methods may not be able to identify all the conditions where four wheels are absolutely grounded in a timely and accurate fashion. For example, if the torques applied to the wheels have errors, if the vehicle reference computation has errors or there is not enough excitation in the torque provided, the wheel lift detection may provide erroneous information or no information about the roll trending of the vehicle. Wheel lift information may also be safe-guarded by information regarding the vehicle roll angle information from the various sensors.
In certain driving conditions where the vehicle is moving with all four wheels contacting ground and the wheel lift detection does not detect the grounding condition, the roll information derived from the various sensors may be the sole information for identify vehicle roll trending. If in such driving cases, the vehicle experiences very large lateral acceleration and large roll rate, the grounded conditions might be replaced by erroneous lifting conditions. That is, those signals may predict that the vehicle is in a divergent roll event but the actual vehicle is not in a rolling event at all. Such cases include when the vehicle is driven on a mountain road, off-road or banked road, tire compression or an impact may cause a large normal load. The increased normal load causes a force component to be added to the lateral acceleration sensor output. Hence, a larger than 1 g lateral acceleration is obtained but the actual lateral acceleration of the vehicle projected along the road surface might be in 0.6 g range. An off-road driving condition may also be an off-camber driving condition. When a low speed vehicle is driven on an off-camber road with some hard tire compression or impact, the control system may be fooled to activate un-necessarily.
In order to reduce false activations, it would therefore be desirable to provide a rollover detection system that sensitizes and desensitizes the roll control determination.
SUMMARY
The present invention sensitizes and desensitizes the roll decision based upon various conditions to make the roll decision more accurate.
In one embodiment, a method of densensitizing includes determining a relative roll angle, determining when the vehicle is in a transitional maneuver, and when the vehicle is in a transitional maneuver, setting a roll signal for control to the relative roll angle, reducing control effort and controlling a safety system correspondingly.
In another embodiment, a method of operating a vehicle comprises determining roll condition, holding a peak brake pressure to counteract rollover, determining a first wheel departure angle, determining a second wheel departure angle after the first wheel departure angle, and when the change of the first wheel departure angle and the second wheel departure angle is less than a threshold, releasing the peak brake pressure.
One advantage of the invention is that some or all of the ways in which to sensitize and desensitize may be used alone or simultaneously to improve a safety system such as a rollover control system.
Other advantages and features of the present invention will become apparent when viewed in light of the detailed description of the preferred embodiment when taken in conjunction with the attached drawings and appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic view of a vehicle with variable vectors and coordinator frames.
FIG. 2 is an end view of an automotive vehicle on a bank with definitions of various angles including global roll angle, relative roll angle, wheel departure angle (WDA), road bank angle and body-to-road angle.
FIG. 3A is an end view of an on-camber divergent vehicle tendency.
FIG. 3B is an end view of an automotive vehicle in an off-camber divergent condition.
FIG. 3C is an end view of a vehicle in an on-camber convergent condition.
FIG. 3D is an end view of a vehicle in an off-camber convergent condition.
FIG. 4A is a block diagram of a stability control system.
FIG. 4B is a block diagram of the controller 26 used in the stability control system depicted in FIG. 4A .
FIG. 5 is a block diagrammatic view of the unit 27 depicted in FIG. 4B , which is used for quantitatively and qualitatively determining rollover trend of a vehicle.
FIG. 6 is more detailed view of the sensitizing and desensitizing block of FIG. 5 .
FIG. 7 is a plot of wheel departure angle versus time for normal conditions and for those of the present embodiment.
FIG. 8 is flow chart of the operation of one embodiment of sensitizing according to one embodiment of the present invention.
FIG. 9 is flow chart of the operation of one embodiment of desensitizing according to one embodiment of the present invention.
FIG. 10 is a flow chart illustrating exiting a proportional peak hold strategy.
FIG. 11 is a flow chart illustrating the timing of active wheel lift detection.
DETAILED DESCRIPTION
In the following figures the same reference numerals will be used to identify the same components. The present teachings may be used in conjunction with a yaw control system or a rollover control system for an automotive vehicle. However, the present teachings may also be used with a deployment device such as airbag or roll bar.
Referring to FIG. 1 , an automotive vehicle 10 on a road surface 11 with a safety system is illustrated with the various forces and moments thereon. Vehicle 10 has front right and front left tires 12 a and 12 b and rear right tires and rear left tires 13 a and 13 b , respectively. The vehicle 10 may also have a number of different types of front steering systems 14 a and rear steering systems 14 b including having each of the front and rear wheels configured with a respective controllable actuator, the front and rear wheels having a conventional type system in which both of the front wheels are controlled together and both of the rear wheels are controlled together, a system having conventional front steering and independently controllable rear steering for each of the wheels, or vice versa. Generally, the vehicle has a weight represented as Mg at the center of gravity of the vehicle, where g=9.8 m/s 2 and M is the total mass of the vehicle.
As mentioned above, the system may also be used with active/semi-active suspension systems, anti-roll bar or other safety devices deployed or activated upon sensing predetermined dynamic conditions of the vehicle.
The sensing system 16 is part of a control system 18 . The sensing system 16 may use a standard yaw stability control sensor set (including lateral acceleration sensor, yaw rate sensor, steering angle sensor and wheel speed sensor) together with a roll rate sensor and a longitudinal acceleration sensor. The various sensors will be further described below. The wheel speed sensors 20 are mounted at each corner of the vehicle, and the rest of the sensors of sensing system 16 may be mounted directly on the center of gravity of the vehicle body, along the directions x,y and z shown in FIG. 1 . As those skilled in the art will recognize, the frame from b 1 , b 2 and b 3 is called a body frame 22 , whose origin is located at the center of gravity of the car body, with the b 1 corresponding to the x axis pointing forward, b 2 corresponding to the y axis pointing off the driving side (to the left), and the b 3 corresponding to the z axis pointing upward. The angular rates of the car body are denoted about their respective axes as ω x for the roll rate, ω y for the pitch rate and ω z for the yaw rate. The calculations set forth herein may take place in an inertial frame 24 that may be derived from the body frame 22 as described below.
The angular rate sensors and the acceleration sensors are mounted on the vehicle car body along the body frame directions b 1 , b 2 and b 3 , which are the x-y-z axes of the vehicle's sprung mass.
The longitudinal acceleration sensor 36 is mounted on the car body located at the center of gravity, with its sensing direction along b 1 -axis, whose output is denoted as a x . The lateral acceleration sensor 32 is mounted on the car body located at the center of gravity, with its sensing direction along b 2 -axis, whose output is denoted as ay.
The other frame used in the following discussion includes the road frame, as depicted in FIG. 1 . The road frame system r 1 r 2 r 3 is fixed on the driven road surface, where the r 3 axis is along the average road normal direction computed from the normal directions of the four-tire/road contact patches.
In the following discussion, the Euler angles of the body frame b 1 b 2 b 3 with respect to the road frame r 1 r 2 r 3 are denoted as θ xr ,θ yr and θ zr , which are also called the relative Euler angles.
Referring now to FIG. 2 , the relationship of the various angles of the vehicle 10 relative to the road surface 11 is illustrated. One angle is a wheel departure angle θ wda , which is the angle from the axle or the wheel axis to the road surface 11 . Also shown is a reference road bank angle θ bank , which is shown relative to the vehicle 10 on a road surface. The vehicle 10 has a vehicle body 10 a and vehicle suspension 10 b . The relative roll angle θ xr is the angle between the wheel axle and the body 10 a . The global roll angle θ x is the angle between the horizontal plane (e.g., at sea level) and the vehicle body 10 a.
Referring now to FIG. 3A , vehicle 10 is illustrated in an on-camber divergent state. The on-camber divergent state refers to the vehicle having a greater than zero wheel departure angle, a greater than zero relative roll angle, and a moment represented by arrow 25 tending to increase the relative roll angle and the wheel departure angle. In this example, the bank angle is less than zero.
In FIG. 3B , when the bank angle is greater than zero, the wheel departure angle is greater than zero, the relative roll angle is greater than zero and the moment is also to the right or increasing the relative roll angle and the wheel departure angle, the vehicle is in an off-camber divergent state.
Referring now to FIG. 3C , a bank angle of less than zero, a wheel departure angle greater than zero, and a relative roll angle greater than zero is shown with a roll moment 25 acting to the left. Thus, the vehicle is in an on-camber convergent state. That is, the convergent state refers to the vehicle tending towards not overturning.
Referring now to FIG. 3D , when the bank angle is greater than 0, the wheel departure angle is greater than zero, and the relative roll angle is greater than zero and the roll moment is tending to the left, the vehicle is in an off-camber convergent state. That is, the vehicle is tending toward not rolling over.
Referring now to FIG. 4A , one embodiment of a roll stability control system 18 is illustrated in further detail having a controller 26 used for receiving information from a number of sensors which may include a yaw rate sensor 28 , a speed sensor 20 , a lateral acceleration sensor 32 , a roll rate sensor 34 , a steering angle sensor (hand wheel position) 35 , a longitudinal acceleration sensor 36 , and steering angle position sensor 37 .
In one embodiment, the sensors are located at the center of gravity of the vehicle. Those skilled in the art will recognize that the sensors may also be located off the center of gravity and translated equivalently thereto.
Lateral acceleration, roll orientation and speed may be obtained using a global positioning system (GPS). Based upon inputs from the sensors, controller 26 may control a safety device 38 . Depending on the desired sensitivity of the system and various other factors, not all the sensors 20 , 28 , 32 , 34 , 35 , 36 , and 37 , or various combinations of the sensors, may be used in a commercial embodiment. Safety device 38 may control an airbag 40 , an active braking system 41 , an active front steering system 42 , an active rear steering system 43 , an active suspension system 44 , and an active anti-roll bar system 45 , or combinations thereof. Each of the systems 40 - 45 may have their own controllers for activating each one. As mentioned above, the safety system 38 may be at least the active braking system 41 .
Roll rate sensor 34 may sense the roll condition of the vehicle based on sensing the height of one or more points on the vehicle relative to the road surface. Sensors that may be used to achieve this include a radar-based proximity sensor, a laser-based proximity sensor and a sonar-based proximity sensor.
Roll rate sensor 34 may also sense the roll condition based on sensing the linear or rotational relative displacement or displacement velocity of one or more of the suspension chassis components which may include a linear height or travel sensor, a rotary height or travel sensor, a wheel speed sensor used to look for a change in velocity, a steering wheel position sensor, a steering wheel velocity sensor and a driver heading command input from an electronic component that may include steer by wire using a hand wheel or joy stick.
The roll condition may also be sensed by sensing the force or torque associated with the loading condition of one or more suspension or chassis components including a pressure transducer in active air suspension, a shock absorber sensor such as a load cell, a strain gauge, the steering system absolute or relative motor load, the steering system pressure of the hydraulic lines, a tire lateral force sensor or sensors, a longitudinal tire force sensor, a vertical tire force sensor or a tire sidewall torsion sensor.
The roll condition of the vehicle may also be established by one or more of the following translational or rotational positions, velocities or accelerations of the vehicle including a roll gyro, the roll rate sensor 34 , the yaw rate sensor 28 , the lateral acceleration sensor 32 , a vertical acceleration sensor, a vehicle longitudinal acceleration sensor, lateral or vertical speed sensor including a wheel-based speed sensor, a radar-based speed sensor, a sonar-based speed sensor, a laser-based speed sensor or an optical-based speed sensor.
Based on the inputs from sensors 20 , 28 , 32 , 34 , 35 , 36 , 37 , controller 26 determines a roll condition and controls any one or more of the safety devices 40 - 45 .
Speed sensor 20 may be one of a variety of speed sensors known to those skilled in the art. For example, a suitable speed sensor 20 may include a sensor at every wheel that is averaged by controller 26 . The controller 26 translates the wheel speeds into the speed of the vehicle. Yaw rate, steering angle, wheel speed and possibly a slip angle estimate at each wheel may be translated back to the speed of the vehicle at the center of gravity. Various other algorithms are known to those skilled in the art. For example, if speed is determined while speeding up or braking around a corner, the lowest or highest wheel speed may not be used because of its error. Also, a transmission sensor may be used to determine vehicle speed.
Referring now to FIGS. 4A and 4B , controller 26 is illustrated in further detail. There are two major functions in controller 26 : the rollover trend determination, which is called a sensor fusion unit 27 A, and the feedback control command unit 27 B. The sensor fusion unit 27 A can be further decomposed as a wheel lift detector 50 , a transition detector 52 and a vehicle roll angle calculator 66 .
Referring now to FIG. 5 , the sensor fusion unit 27 A is illustrated in further detail. The sensor fusion unit 27 A receives the various sensor signals, 20 , 28 , 32 , 34 , 35 , 36 , 37 and integrates all the sensor signals with the calculated signals to generate signals suitable for roll stability control algorithms. From the various sensor signals wheel lift detection may be determined by the wheel lift detector 50 . Wheel lift detector 50 includes both active wheel lift detection and passive wheel lift detection, and wheel grounding condition detection. Wheel lift detector is described in co-pending U.S. provisional application Ser. No. 60/400,375 filed Aug. 1, 2002, and U.S. patent application number 7,109,856, which are incorporated by reference herein. The modules described below may be implemented in hardware or software in a general purpose computer (microprocessor). From the wheel lift detection module 50 , a determination of whether each wheel is absolutely grounded, possibly grounded, possibly lifted, or absolutely lifted may be determined. Transition detection module 52 is used to detect whether the vehicle is experiencing aggressive maneuver due to sudden steering wheel inputs from the driver. The sensors may also be used to determine a relative roll angle in relative roll angle module 54 . Relative roll angle may be determined in many ways. One way is to use the roll acceleration module 58 in conjunction with the lateral acceleration sensor. As described above, the relative roll angle may be determined from the roll conditions described above.
The various sensor signals may also be used to determine a relative pitch angle in relative pitch angle module 56 and a roll acceleration in roll acceleration module 58 . The outputs of the wheel lift detection module 50 , the transition detection module 52 , and the relative roll angle module 54 are used to determine a wheel departure angle in wheel departure angle module 60 . Various sensor signals and the relative pitch angle in relative pitch angle module 56 are used to determine a relative velocity total in module 62 . The road reference bank angle block 64 determines the bank angle. The relative pitch angle, the roll acceleration, and various other sensor signals as described below are used to determine the road reference bank angle. Other inputs may include a roll stability control event (RSC) and/or the presence of a recent yaw stability control event, and the wheel lifting and/or grounding flags.
The global roll angle of the vehicle is determined in global roll angle module 66 . The relative roll angle, the wheel departure angle, and the roll velocity total blocks are all inputs to the global roll angle total module 66 . The global roll angle total block determines the global roll angle θ x . An output module 68 receives the global roll angle total module 66 and the road reference bank angle from the road reference bank angle module 64 . A roll signal for control is developed in roll signal module 70 . The roll signal for control is illustrated as arrow 72 . A sensitizing and desensitizing module 74 may also be included in the output module 68 to adjust the roll signal for control.
In the reference road bank angle module 64 , the reference bank angle estimate is calculated. The objective of the reference bank estimate is to track a robust but rough indication of the road bank angle experienced during driving in both stable and highly dynamic situations, and which is in favor for roll stability control. That is, this reference bank angle is adjusted based on the vehicle driving condition and the vehicle roll condition. Most importantly, when compared to the global roll estimate, it is intended to capture the occurrence and physical magnitude of a divergent roll condition (two wheel lift) should it occur. This signal is intended to be used as a comparator against the global roll estimate for calculating the error signal, which is fed back to roll stability controller 26 .
Referring now to FIG. 6 , the operation of the sensitizing/desensitizing module 74 is described in further detail. In this module, the needed control effort used in the roll stability control RSC system is sensitized by deliberately increasing certain thresholds, boosting certain signals and holding certain variables in order to cope with scenarios where the vehicle is in divergent roll trend; the control effort used in RSC is desensitized by deliberately decreasing certain thresholds, exiting holding mode and inserting hysteresis in certain variables in order to cope with the scenarios where the vehicle is not in divergent roll trend but the vehicle sensors cannot distinguish such no-divergent roll trend with the divergent or unstable dynamics. In summary, the sensitization is used to boost the control effort in the side of the vehicle needed, and desensitization is used to detune the control effort in the un-needed side so as to reduce false activations in non-rollover events.
The module has various external inputs that include a relative roll angle θ xr input 80 ; a roll signal for control θ rsfc input 82 ; a roll rate ω x input 84 ; a wheel departure angle θ wda input 86 , a first transitional flag input 88 for left to right transition denoted as T( 0 ) and a second transitional flag 90 denoted as T( 1 ) for right to left transition. The transitional flags are set as the vehicle change from a right to left turn and a left to right turn. The generation of the transitional flags is described in provisional application No. 60/401,416 which is incorporated by reference herein. Other inputs include a final wheel lift status flags input 92 that is denoted by S wld (i). The final wheel lift status flag is set so:
If the ith wheel is absolutely grounded, then S wld (i)=ABSOLUTELY_GROUNDED
If the ith wheel is in the edge of grounding, S wld (i)=POSSIBLY_GROUNDED If the ith wheel is absolutely lifted, then S wld (i)=ABSOLUTELY_LIFTED If the ith wheel is in the edge of lifting S wld (i)=POSSIBLY_LIFTED If the ith wheel's status cannot be firmly identified, S wld (i)=NO_INDICATION Other inputs include a reference bank angle input 94 denoted as θ refbank and a global roll angle input 96 θ x The outputs of the module 74 include a wheel departure angle output 98 denoted by θ wda , a roll signal for control output 100 denoted by θ rsfc , a proper-peak-hold flag: output 102 denoted by F PPH , a reference bank angle output 104 denoted θ refbank and a pre-lift sensing flag output 106 denoted by F PLS .
Predefined Calibratable Parameter Definitions
The module 74 also includes various parameters and thresholds that are defined as follows:
Θ sensitize : the threshold for the relative roll angle used for sensitizing wheel departure angle during transitional maneuvers. Default value used in the present example=45% of roll gradient. α: percentage of relative roll angle boosted for roll signal for control during double wheel lift events. Θ wheel-normal-condition : the threshold for the relative roll angle for starting the computation of the wheel departure angle during normal driving condition. Default value used in the present example=75% of the roll gradient. Θ non-transition : the threshold for the relative roll angle used in starting to adjust the reference bank during non-transitional maneuvers. Default value used in the present example=80% of roll gradient. ΔΘ: the threshold for wheel departure angle drop during to sequential loops used for exiting proportional peak hold mode in PID controller. Default value used in the present example=4 degree. Ω PPH : threshold for the roll angular rate in order to enter proportional peak hold mode. Default value=used in the present example 16 degree per second. Θ PLS : the threshold for the wheel departure angle in order to start the pre-lift sensing. Default value used in the present example=1 degree. T: the threshold for the drive torque at a wheel to start the pre-lift sensing.
Sensitization
Referring now to FIG. 7 , the starting point of computing the wheel departure angle is assumed to be at the time instant where one of the tires is at the edge of losing its normal load, or at the edge of being lifted. The exact time, however, is not typically detectable. Considering all the uncertainties in a vehicle, the approximated timing may be identified based on the wheel lift detection and the vehicle roll information. As shown in FIG. 7 , the time instant where the tire is about to lift is illustrated as t 0 , then before t 0 at time t 01 , the wheel departure angle must have negative value. The wheel departure angle is reset to zero when the computation start. Thus if the computation is started at a time instant earlier than t 0 , the negative wheel departure angle due to tire compression (usually around 1 degree) will be added to the computed wheel departure angle to effectively boost the wheel departure angle. This sensitizes the wheel departure angle. If the start timing for computing wheel departure angle is later than t 0 at time t 02 , the magnitude of the calculated wheel departure angle will be less than the magnitude of the actual value, hence desensitizes the wheel departure angle.
Referring now to FIG. 8 , if the vehicle is near wheel lifting in step 120 , in step 122 the transitional flags are monitored. The vehicle left to right transitional or right to left transitional flags are set to be active due to a dynamic transitional maneuver of the vehicle. In such a case, the vehicle may have a very large roll rate and hence a high roll trend. In this case any late computation of the wheel departure will desensitize the control effort which will have adverse control effect. Hence in this case the wheel departure angle computation is sensitized such that a needed control effort can be boosted.
if ( (T(0) = 1 & & θ xr ≧ Θ sensitize )
∥ (T(1) == 1 & & θ xr ≦ −Θ sensitize )
{
Compute wheel departure angle;
}
else if the normal conditions are met
{
Exit computing wheel departure angle;
}
The relative roll angle is determined in step 124 . Notice that if the normal condition for computing wheel departure starts at a relative roll magnitude Θ normal , then the threshold Θ sensitize for sensitizing wheel departure angle during transitional maneuver could be as small as 50% of Θ normal . In step 126 the transitional flags are monitored and the relative roll angle θ xr exceeds or is equal to the sensitizing threshold and the left to right transition flag is set or the right to left transition flag is set and the relative roll angle θ xr is less than or equal to a negative Θ sensitize threshold. The boosted wheel departure angle is obtained by starting the calculation earlier than at a nominal time t 0 as described above in step 128 . The boosted wheel departure angle will add certain amount of roll angle to the final roll signal for control θ rsfc , hence help increase certain amount of control effort.
If the wheel lift detection methods identify that two wheels at the inside of a turn are both lifted in step 130 , then the vehicle is in a progressive rollover event. In this case significant control effort is required in order to fully control the vehicle body such that rollover can be prevented. One sensitizing method is to further boost the roll signal for control as in step 132 as set forth in the following:
if((S wld (0) == 1 & &S wld (2) == 1 & &θ xr > 0) ∥(S wld (1) == 1 & &S wld (3) == 1 & &θ xr ≦ 0)) { θ rsfc = θ rsfc + α% * θ xr ; }
where α is the percentage of the desired boost. The default value in this example is 10.
In step 134 whether the vehicle is bouncing is determined. When the vehicle has very large roll angle together with a large magnitude of the roll rate during last second, the vehicle will be in a potential bouncing mode. In this case a proportional peak hold of the brake pressure (roll control effort) is conducted. A proportional control term is calculated in:
if (vehicle is in bouncing mode) { Proportianl_control_term=K p θ rsfc-peak } else { Proportianl_control_term=K p θ rsfc }
where θ rsfc-peak is the peak value of the roll signal for control during a specific period of time in step 136 .
Desensitization
Referring now to FIG. 9 , as mentioned above it may also be desirable to desensitize the system in certain situations. For example, during a transitional maneuver, the roll signal for control θ rsfc will be reduced to relative roll angle θ xr if the wheel lift detection algorithms identify that the two wheel at the inside of a turn are absolutely grounded. In this case, the vehicle is not in any roll divergence and the roll angle between the vehicle body and the road surface is exactly the relative roll angle θ xr . Since usually θ xr alone will not be able to initiate PID control, hence resetting θ rsfc to θ xr will exit RSC control. This is set forth in step 140 by first determining if the vehicle is in a transitional maneuver. If the inside wheels are absolutely grounded in step 142 (and there is some roll angle in the right direction) then the roll signal for control is set to the relative roll angle in step 144 .
if( (T(0) == 1
& &S wld (1) == ABSOLUTELY_GROUNDED
& &S wld (3) == ABSOLUTELY_GROUNDED
& &θ xr ≦ 0)
(T(1) == 1
& &S wld (0) == ABSOLUTELY_GROUNDED
& &S wld (2) == ABSOLUTELY_GROUNDED
& &θ xr > 0) )
{
θ rsfc = θ xr + θ wda = θ xr ;
}
During non-transitional maneuver, the roll signal for control θ rsfc will be reduced to relative roll angle θ xr if the wheel lift detection algorithms identify that one of the two inside wheels at a turn is absolutely grounded. In this case, the vehicle is not in any roll divergence and the roll angle between the vehicle body and the road surface is exactly the relative roll angle θ xr . Since usually θ xr alone will not be able to initiate PID control, hence resetting θ rsfc to θ xr will exit RSC control. This is carried out in step 140 when there is no transitional maneuver. In step 146 whether one of two inside wheels is grounded is determined. If one of the two inside wheels are grounded, step 144 is again executed in which the roll signal for control is set to the relative roll angle. This is set forth in the following code.
if( (T(0) == 0
& &(S wld (1) == ABSOLUTELY_GROUNDED
∥ S wld (3) == ABSOLUTELY_GROUNDED)
& &θ xr ≦ 0)
(T(1) == 0
& &(S wld (0) == ABSOLUTELY_GROUNDED
∥ S wld (2) == ABSOLUTELY_GROUNDED)
& &θ xr > 0) )
{
θ rsfc = θ xr + θ wda = θ xr ;
}
In non-transitional maneuver, the reference bank is updated when the magnitude of the relative roll angle is less than a Θ non-transition threshold, which is larger than the Θ wda-normal-condition threshold in step 148 . Hence there is a gap of the relative roll angle which is used to provide certain hysteresis in reference bank angle computation. If the magnitude of the relative roll angle is under the Θ non-transition threshold but greater than Θ wda-normal-condition , even wheel departure angle is already starting to be computed, the reference bank angle will wait until the relative roll angle exceeds Θ non-transition threshold to be adjusted, and hence the roll signal for control to be adjusted. That is, the reference road bank θ ref is set to the maximum of the global roll angle θ x -θ xss or the previously determined reference bank angle. This is set forth in the following code:
if (( θ xr < −Θ non-transition & & ( S wld (1)!= ABSOLUTELY_GROUNDED ∥ S wld (3) != ABSOLUTELY_GROUNDED ) ) ∥ ( θ xr ≧ Θ non-transition & & ( S wld (0)!= ABSOLUTELY_GROUNDED ∥ S wld (2) != ABSOLUTELY_GROUNDED ) ) { θ ref-bank = max( θ x − θ xss ,θref-bank); }
where θ xss =θ x −θ xr −θ wda .
Referring now to FIG. 10 , in step 162 if the incremental correction for the wheel departure angle for two sequential loops exceeds certain magnitude ΔΘ (default value=4 degree), the RSC will exit proportional peak brake pressure holding by resetting the flag F PPH to zero in step 164 . In step 162 the previous wheel departure angle is subtracted from a current wheel departure angle. In this case, the self adjusting feature of the wheel departure angle computation implies that the vehicle is not in a divergent roll motion, hence holding brake pressure will cause the driver an un-easy feeling. Exiting enforced proportional peak hold pressure will allow the roll information of the vehicle to set the control effort to appropriate level.
if (|θ wda (k)−θ wda (k − 1)| > ΔΘ) { F PPH = 0; }
where θ wda (k) denotes the current value of the wheel departure angle and θ wda (k−1) denotes the past value of the wheel departure angle.
In step 166 , if the vehicle roll rate does not exceed a threshold Ω PPH (16 degree/sec in the present example) within last 1 second, the vehicle is identified as not in the bouncing mode. Hence proportional peak hold will be ended in step 164 . In this case, there is no need to hold brake pressure. Exiting enforced proportional peak hold pressure will allow the roll information of the vehicle to set the control effort to appropriate level.
if (|ω x | < Ω PPH during last 1 second)
{
F PPH = 0;
}
Referring now to FIG. 11 , it may be desirable to start active wheel lift detection early. Although the passive wheel lift detection is performed all the time, the active wheel lift detection is conditionally performed. For example, only if the RSC enters PID control mode the active wheel lift detection is activated. Since the PID control is related to roll trend conditioned by the wheel lifting information and there is a delay between the beginning of the active detection and the time when the detection resets the flag, there may be cases where a long lasting un-necessary activation from the PID controller is performed. The active wheel lift detection may thus be performed before the PID controller is activated. The delay due to the active wheel lift detection consequently may be removed. This implies the need for an earlier active wheel lift detection, which may be called pre-lift sensing. That is before entering the PID control mode and the transitional control mode, the active wheel lift detection will start to proceed under certain conditions. One of the conditions is dependent on the wheel departure angle. If the wheel departure angle is greater than certain threshold and the driving torque at the axle is below certain threshold in step 170 , a prelifting flag is set in step 172 , the active wheel lift detection will request engine torque reduction or provide a pressure command to the wheel in step 174 . In this manner, un-necessary false activations can be avoided or the false activation can be shorted in duration. The logic can be expressed as in the following:
if (|θ wda | > Θ PLS & & τ drive ≦ T) { F PLS = 1; }
where F PLS is the flag for pre-lift sensing, i.e, F PLS =1 will initiate pre-lift sensing, and τ drive is the drive torque at the interested wheel.
As is described above, various ways of sensitizing or desensitizing roll control are described. Depending on the various system requirements one, some or all of the ways may be implemented in a commercial embodiment.
While the invention has been described in connection with one or more embodiments, it should be understood that the invention is not limited to those embodiments. On the contrary, the invention is intended to cover all alternatives, modifications, and equivalents, as may be included within the spirit and scope of the appended claims.
|
A method of densensitizing includes determining a relative roll angle, determining when the vehicle is in a transitional maneuver, and when the vehicle is in a transitional maneuver, setting a roll signal for control to the relative roll angle, reducing control effort and controlling a safety system ( 38 ) correspondingly.
| 1
|
RELATED APPLICATIONS
[0001] This application claims the benefit of Provisional Patent Application 61/773,707, filed Mar. 6, 2013.
FIELD OF THE INVENTION
[0002] This invention relates to dressings and bandages for acute and chronic wounds.
BACKGROUND OF THE INVENTION
[0003] Wound management involves removal of all non-viable tissue at the wound site, preserving the remaining viable tissue, and providing a moist but not wet environment. An example of successful burn wound dressing is Biobrane, granted U.S. Pat. No. 4,725,279. In 1979 Biobrane was initially studied by American Burn Surgeons; it is still popular world-wide.
[0004] In 2007 new art was introduced by this inventor with AWBAT and then with AWBAT Plus, granted U.S. Pat. No. 7,815,931 and covered by several copending patent applications. The key to the success of these products was better porosity in the dressing.
[0005] Recently, this inventor has revisited the art of dressing design. The present invention allows passage of fluid adjacent to the wound through the primary dressing into a secondary absorbent dressing as well as improving the kinetics of uninterrupted wound healing. Technology of this dressing has evolved into a new product which possesses all the characteristics and attributes known to be important for optimal wound healing, as well as containing certain advances that result in minimization of wound desiccation and infection complication.
SUMMARY OF THE INVENTION
[0006] Wound sites have variable amounts of exudate/transudate/plasma present, from dry to weepy. The clinician must cleanly debride the wound, close it and manage wound healing in a moist but not wet environment to achieve optimal results in both acute and chronic wounds.
[0007] The present invention provides a dressing that possesses all the properties and attributes of an ideal skin substitute and, in addition, has ‘variable porosity’ controlled by the clinician from zero porosity to what the wound requires. The present invention enables the clinician to move the fluid exuding from the wound through the primary dressing into an absorbent secondary dressing without disturbing the kinetics of healing or causing pain to the patient.
[0008] The present invention is cost effective at every level. Patients get their wounds managed with minimal pain and optimal healing times. The dressing is cost effective as the hospital needs to inventory only one primary dressing for acute wounds (burns) and one for chronic wounds; each has a two year shelf-life at room temperature.
[0009] The present invention is composed of two biological layers sprayed on in separate operations. The first layer sprayed onto the nylon side of the “variable porosity” silicone membrane will be: (1) a solution of pure Aloe (Aloesin, Immuno10, Qmatrix and Loesyn—each hydrophilic and hygroscopic.); (2) a solution of pure Aloe and hypoallergenic USP Pharmaceutical Grade porcine gelatin; or (3) a fine suspension of pure Aloe, gelatin and ECM (as fine insoluble particles or hollow spheres in water—the latter possesses improved healing properties). In vitro, the Aloe component has been demonstrated to cause a variety of cells to attach and proliferate; as well as increase synthesis of collagen and alpha smooth muscle actin. ECM may be added to the biologicals described above and is a mixture from human fibroblasts that is known to cause rapid cell proliferation and tissue growth. Previous wound dressings and skin substitutes, as taught in U.S. Pat. No. 7,815,931 contain gelatin, a pure Aloe component, chondroitin 4 & 6 sulfate, and vitamin C & E. In contrast the current dressing will have two layers of biologicals applied in separate spraying operations as described above. The first coat will contact the wound after the second coat of hypoallergenic bovine spongiform encephalopathy (BSE)-free United Staes Pharmaceutical (USP)—grade gelatin interacts with fibrin in the wound to achieve early adherence, The second coat of biologicals stimulates the healing process during the interval where the dressing invention is in contact with the wound and is stable requiring 100 degree water for 30 minutes to remove from the “variable porosity” silicone/nylon surface.
BRIEF DESCRIPTION OF THE FIGURES
[0010] FIG. 1 . The embodiments of the invention, showing the slit openings
[0011] FIG. 2 . The wale and course nature of the woven fabric
[0012] FIG. 3 . An example of punctuate scarring
DETAILED DESCRIPTION
[0013] The present invention is similar in composition to earlier skin substitutes in that they each have a thin silicone component and an underlying thin knitted nylon component. The present invention differs from its ancestors in that it has “variable porosity” controlled by the clinician; the pore size in the thin silicone will be essentially zero (with no stretch, in relaxed mode) to a higher porosity (proportional to the stretch applied). See FIG. 1 for the optional stretch modes. In addition, the present invention differs in the composition of biological coatings applied to both components and how these coatings interact with the wound over time.
[0014] The pores of prior art skin substitutes/dressings are of a fixed size (Biobrane 1.2%; AWBAT and AWBAT Plus 5.5% and 7.5%) in the unstretched open position; the silicone is cured while the skin substitute pores are open. Once cured the pores cannot close or be reduced in size; this causes wound desiccation and punctate scarring. As in FIG. 1 , in contrast, the openings are made after the silicone component has been cured, and are in the shape of slits, not holes. The figure shows the skin substitute silicone layer up with the slits exposed.
[0015] The “wale” and “course” orientations of stitching of the knitted nylon component of the invention are shown in FIG. 2 . The two embodiments of the invention are shown in FIGS. 1A and 1B . In one embodiment, Option A—designed for burns, the slits 103 made in the silicone are approximately 125″ long 101 with a space of 0.25″ between slits 102 ; parallel rows of slits are 0.25″ apart. The parallel rows of slits are oriented such that the slits are parallel to the “wale” orientation of the Jersey stitch pattern of the knitted nylon component. The “wale” orientation has measurably less elongation than the “course” orientation.
[0016] Because of the orientation of the slits, stretch along the axis of the slits is minimal and stretch perpendicular to the slit axes is maximized. With no stretch of the silicone/nylon membrane the slits cannot be seen without magnification while observing from above.
[0017] In the second embodiment, Option B—designed for chronic wounds, a less regular pattern with slits both parallel and perpendicular is preferred. The slits made in the silicone are approximately 0.125 ″ long with a space of 0.50″, between the slits; off-set parallel rows of slits are 0.25″ apart. Rows of slits perpendicular to the above are also 0.125″ long with a space of 0.50″, between the next slit; off-set parallel rows of slits are 0.25″ apart. In this configuration the silicone/nylon membrane can be stretched in any direction and the slits will open. Porosity therefore increases proportional to the amount of stretch applied. Obviously, there is a maximum amount of stretching of the Option B invention before the dressing fails.
[0018] For burns, Option A is preferable, particularly on partial thickness burns where punctate scarring has been observed. In the Option A configuration, with no stretch, the wound is protected by an essentially continuous thin silicone membrane which minimizes wound desiccation and punctate scarring. Option A enables the clinician to stretch the dressing parallel to the direction of the slits with minimal opening of the slits. This is parallel to the “wale” direction of the underlying fabric. Fluids from the wound can still escape through the closed slits and be absorbed into a secondary dressing, which can be removed and replaced without interfering with the healing process or causing pain to the patient.
[0019] The combination of a primary dressing that requires minimal changes and a secondary dressing that is easy to change and replace reduces wound maintenance costs which benefits patient, staff and hospital. An example of punctate scarring is illustrated in FIG. 3 ; the figure shows the skin of a patient whose burn was covered with the ancestor AWBAT dressing with a fixed porosity of at least 5.5%.
[0020] Chronic, slow healing wounds require similar treatment as burns in that all necrotic tissue must be removed before closing the wound with a primary dressing. In the chronic wound, exudate and other fluids are often removed with negative pressure wound therapy (NPWT). A negative pressure above the wound or a positive pressure from the wound causes exudate and other wound fluids to pass through the primary dressing into a secondary dressing. The primary dressings currently used during NPWT are: urethane foam, polyvinyl alcohol foam or cotton gauze; all require frequent dressing changes and infection complications have been reported when these dressings are not changed frequently.
[0021] The use of the present invention has a large benefit because it is stable on the wound, compatible with or without NPWT, and possesses biologicals that aid in the healing process. Option B of the invention is preferred for closing the chronic wound because it provides greater porosity as well as an increased rate of porosity, compared to Option A, when the dressing is stretched in any direction the appropriate amount. Since chronic wounds are generally in the lower extremities, punctate scarring is not a clinical concern. An example of chronic wounds that benefit from this novel art are: pressure sores, diabetic ulcers and chronic vascular ulcers.
[0022] The present invention will have two layers of biologicals; first a clotting outer layer containing hypoallergenic BSE free USP Pharmaceutical grade gelatin. This layer contacts the wound first and stimulates initial adherence of the dressing to the cleanly debrided wound.
[0023] The second layer of pure Aloe or Aloesin, pure Aloe and BSE free gelatin, or a mixture of pure Aloe, BSE free gelatin and ECM interact with the wound to stimulate the rate of healing while adherent to the wound. The first layer is deposited directly on the nylon side of the “variable porosity” silicone/nylon surface and is stable, i.e. requires 100 degree water for 30 minutes to remove from the “variable porosity” silicone/nylon surface.
[0024] These are the preferred embodiments of the invention. The technology to create the two forms of the invention is listed as the preferred embodiments of this invention, but other methods are possible and are within the contemplation of this patent.
|
An improved skin substitute is presented comprised of a silicone layer backed up with a woven nylon fabric layer, the silicone layer possessing a regular pattern of slits that permit the porosity of the skin substitute to be adjusted by clinicians by means of applying tension to the skin substitute that differentially opens the slits. A variety of therapeutic substances can be applied to the skin substitute to promote healing, including aloe and other medicinal preparations.
| 3
|
[0001] The present invention relates to an improved ripper boot and, in particular, to a ripper boot for use in a range of applications involving the ripping or cleaving of hard material. The preferred application of the present invention is in opal mining where hard ground is to be penetrated in an attempt to locate opal.
BACKGROUND OF THE INVENTION
[0002] Ripper boots are typically used where extremely hard rock or compacted soil is encountered and is required to be penetrated and ripped in an attempt to locate and extract precious stones such as opal. The ripper boot includes a carrier which is typically secured to a bulldozer tyne and a ripping tooth section secured to the nose of the carrier to rip through rock, typically to a depth of approximately 300 mm at a time. In the case of opal mining, the loosened rock is then pushed away, while spotters check for signs of opal. The ripping tooth can also be replaceable. The present inventor has identified some problems with such conventional ripper boots.
[0003] Firstly, some replaceable ripping tooth sections are secured to the boot in a rotatable manner. The problem with having a rotatable ripping tooth is that during operation, ground up rock is able to enter into the area between the shaft of the ripping tooth and the ripper boot body. This causes considerable wear and tear when the shaft rotates which may eventually lead to metal fatigue and fracture under extreme loads. A further problem is that the ripping tooth tends to move and chatter during operation which is also undesirable. Further still, where clay fines and other similar material build up in the area surrounding the ripping tooth shaft, the tooth becomes almost impossible to remove. Existing ripper boots having rotatable teeth are also expensive to manufacture, and their use is limited to only a small range of applications.
[0004] The present inventor has further discovered that the “angle of attack” is extremely important in ripping operations, that is, the angle at which the ripping boot rips through the ground. In conventional ripping operations, the angle of attack is typically governed by the angle at which the end of the bulldozer tyne extends because it is the tyne that carries the ripper boot. The position of the bulldozer tyne is adjustable, however, its movement is restricted and often a desired angle of attack is not attainable.
[0005] When the tooth is ripping at too steep an angle, that is, when the angle between the longitudinal axis of the ripping tooth and the ground surface is too great, the ripper boot will begin to chatter which may result in increased wear and tear on the ripping tooth, metal fatigue and eventual fracture in the ripping tooth. In such circumstances, the load on the bulldozer is also increased which leads to increased fuel consumption. The nose of the ripping tooth tip may also drag when the angle is too steep, and the ripping tooth is prone to being ripped out. In general, where the angle of attack is not correct, the required cleaving effect of the boot is reduced. In fact, it has been found that very small variations in ripping tooth angle can have major effects on the effectiveness of the ripping operation.
[0006] It is therefore an object of the present invention to overcome at least some of the aforementioned problems or to provide the public with a useful alternative.
SUMMARY OF THE INVENTION
[0007] Therefore in one form of the invention there is proposed a ripper boot of the type adapted to be mounted to a shank of a bulldozer or like equipment, said ripper boot characterised by:
[0000] a carrier means adapted to be connected to said shank;
a tooth housing means including a female socket;
a ripping tooth including a shaft portion and a head portion, said shaft portion being correspondingly shaped with said female socket for removable engagement therewith.
[0008] Preferably the shaft portion of the ripping tooth is tapered to enable engagement with the correspondingly shaped female socket by way of an interference fit.
[0009] In preference the taper on the shaft portion is such that that a free end thereof has a smaller cross-sectional size to that of the opposed end which is integral with the ripping tooth head portion.
[0010] Preferably the shaft portion of the ripping tooth and female socket are of a square cross-section including slightly rounded edges. Alternatively, the cross-section could be circular.
[0011] Preferably the carrier means, tooth housing means, and female socket extend along the same longitudinal axis.
[0012] In preference the shaft portion of the ripping tooth and the carrier means include transverse channels extending therethrough which become co-axially aligned when the shaft portion of the ripping tooth is secured within the female socket, to thereby allow for insertion of a retaining means.
[0013] Preferably the head portion of the ripping tooth includes an outwardly extending shoulder adapted to facilitate removal of the ripping tooth from within the female socket.
[0014] In preference said tooth housing means includes an ejection hole which extends from an exterior of the boot to said female socket so that said tooth may be ejected from said chamber.
[0015] Preferably at least part of the ripping tooth head portion is constructed from high tensile material such as tungsten metal.
[0016] In a further form of the invention there is proposed a ripper boot of the type adapted to be mounted to a shank of a bulldozer or like equipment, said ripper boot including:
[0000] a carrier means adapted to be connected to said shank, said carrier means including a longitudinal axis; and
a ripping tooth removably associated with said carrier means such that said ripping tooth extends at a predetermined angle relative to said longitudinal axis.
[0017] Preferably said ripper boot is configured so that during use, the ripping tooth extends upwardly from said longitudinal axis to thereby become aligned approximately parallel with a ground surface.
[0018] Preferably said predetermined angle is between zero and ninety degrees from the longitudinal axis of the carrier means.
[0019] In preference said predetermined angle is between zero and ten degrees from the longitudinal axis of the carrier means.
[0020] Advantageously said predetermined angle is six degrees from the longitudinal axis of the carrier means.
[0021] Thus, this further form of the invention provides a ripper boot whereby the ripping tooth is angled upwardly with respect to the ripper boot carrier so that the angle of attack of the ripping tooth is raised and becomes almost parallel with the ground. In altering the angle of attack in this way, it has been found that the cleaving effect of the boot is increased, chatter and drag of the boot through the ground is reduced which results in less wear and tear and less likelihood of the tooth being ripped out, as well as decreased load on the bulldozer which also reduces fuel consumption.
[0022] Preferably said ripper boot further includes a tooth mounting portion associated with said carrier means, said tooth mounting portion configured to removably house said ripping tooth so that it extends at said predetermined angle relative to said longitudinal axis.
[0023] In preference said tooth mounting portion is in the form of a solid member which is integrally formed with said carrier means but which extends at said predetermined angle therefrom.
[0024] Preferably said tooth mounting portion includes a longitudinal axis and a female socket aligned therealong, said female socket adapted to receive a shaft portion associated with said ripping tooth.
[0025] Alternatively said tooth mounting portion is in the form of a solid member which is integrally formed with said carrier means and extends along the same longitudinal axis, said solid member including a female socket which extends at said predetermined angle relative to the longitudinal axis for receiving a shaft portion associated with said ripping tooth.
[0026] Preferably said shaft portion is adapted to be fixedly supported within the female socket by way of an interference fit.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate several implementations of the invention and, together with the description, serve to explain the advantages and principles of the invention. In the drawings:
[0028] FIG. 1 illustrates a rear perspective view of an improved ripper boot in accordance with a first aspect of the present invention;
[0029] FIG. 2 illustrates a front perspective view of the improved ripper boot of FIG. 1 ;
[0030] FIG. 3 illustrates a cross-sectional side view of the improved ripper boot of FIG. 1 ;
[0031] FIG. 4 illustrates a cross-sectional top view of the improved ripper boot of FIG. 1 ;
[0032] FIG. 5 illustrates an exploded, partially cross-sectional top view of the improved ripper boot of FIG. 1 ;
[0033] FIG. 6 illustrates a cross-sectional side view of an improved ripper boot including a retaining pin;
[0034] FIG. 7 illustrates a cross-sectional top view of an improved ripper boot including a retaining pin;
[0035] FIG. 8 illustrates a cross-sectional top view of an improved ripper boot in accordance with a second aspect of the present invention;
[0036] FIG. 9 illustrates a cross-sectional side view of the improved ripper boot of FIG. 8 ;
[0037] FIG. 10 illustrates a schematic side view of the improved ripper boot of FIG. 8 when the boot is connected to a bulldozer tyne, and shown in broken lines is a conventional ripper boot arrangement;
[0038] FIG. 11 illustrates a cross-sectional top view of an improved ripper boot in accordance with a third aspect of the present invention;
[0039] FIG. 12 illustrates a cross-sectional side view of the improved ripper boot of FIG. 11 ; and
[0040] FIG. 13 illustrates a bulldozer including an improved ripper boot mounted to the bulldozer tyne in accordance with all aspects of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0041] The following detailed description of the invention refers to the accompanying drawings. Although the description includes exemplary embodiments, other embodiments are possible, and changes may be made to the embodiments described without departing from the spirit and scope of the invention. Wherever possible, the same reference numbers will be used throughout the drawings and the following description to refer to the same and like parts.
[0042] The present invention relates to an improved ripper boot according to three different embodiments 10 a , 10 b and 10 c . The ripper boot 10 a is illustrated in FIGS. 1-7 , ripper boot 10 b in FIGS. 8-10 , and ripper boot 10 c in FIGS. 11-12 . FIG. 13 illustrates a bulldozer 12 to which any one of the ripper boots could be attached. For the purpose of brevity, the first ripper boot 10 a will be described in full detail and any like parts found in the other ripper boots will not be described again and will be referred to using like numbers.
[0043] FIGS. 1-5 illustrate the ripper boot 10 a of the present invention which includes a carrier 14 and a replaceable ripping tooth 16 . In operation, the carrier 14 is placed over and conformed to fit with a ripper boot tyne 18 of a bulldozer 12 or other earth moving machinery, as is shown in FIG. 13 . The various components of the bulldozer 12 are not described herein because bulldozers such as these are well known in the art, and apart from the ripper boot tyne 18 , the remaining components do not perform any function insofar as the present invention is concerned.
[0044] The carrier 14 is held in place by utilisation of a pair of oppositely positioned retaining holes 20 located in the rear hollow portion 22 of the carrier 14 which, in conjunction with a retaining pin 24 , is designed to attach the carrier 14 of the ripper boot 10 a to the available tyne 18 . It is to be understood that the carrier 14 may be conformed to fit any available ripper boot shank, and that any desired attachment means other than the retaining pin 24 and oppositely positioned retaining holes 20 may be used.
[0045] The ripper boot carrier 14 also includes a substantially solid portion 26 at its front. This solid portion 26 provides mass and assists in the ripping mechanism to some degree. Primarily, the solid portion 26 provides a female socket or bore 28 adapted to fixedly house a replaceable ripping tooth 16 . The bore 28 is of a square cross-section and includes longitudinal walls that taper inwardly such that the cross-sectional size of the bore 28 adjacent the hollow portion 22 is less than that adjacent the tooth end. All four edges of the socket 28 are rounded off for additional strength.
[0046] The replaceable ripping tooth 16 is made up of a head portion 30 and a shaft 32 . The shaft 32 of the replaceable ripping tooth 14 is correspondingly shaped with the female socket 28 of the carrier 12 , that is, it too includes tapered walls and is of a square cross-sectional shape having rounded corners. This allows the shaft 32 to be fixedly secured within the female socket 28 by way of an interference fit. As those skilled in the art would realise, an interference fit is extremely strong and will not permit any rotation at all of the replaceable ripping tooth 16 and ensures that no particles enter between the wall of the shaft 32 and the abutting wall of the female socket 28 . In preference, the socket 28 is cast so as to ensure that its dimensions correspond with those of the shaft 32 .
[0047] Once the tooth is fixed within the socket 28 , the head portion 30 extends longitudinally outwards from the solid portion 26 of the boot and therefore tapers at substantially the same angle as the solid portion 26 . The head portion 30 of the tooth is designed not to extend too far outwards from the carrier 14 so as to ensure it is not damaged or broken off during the ripping process. Mounted to the end of the replaceable ripping tooth 16 is a pointed tip 34 which can be made of high tensile strength material, such as tungsten for example. The tip 34 may simply be welded to the replaceable ripping tooth 16 . A high tensile tip 34 ensures that even the hardest rock may be penetrated and that problems associated with existing ripper boot tips which become easily worn are minimised.
[0048] In attaching the replaceable ripping tooth 16 to the carrier 14 as described above, a number of benefits are provided.
[0049] Firstly, chatter is reduced during operation because the tooth 16 is fixed, and wear and tear on the tooth 16 is also reduced in that ground dirt can no longer enter the gap between the tooth shaft 32 and the female socket 28 . This is a major problem with rotatable teeth in that particles abrade against the respective surfaces during operation and lead to metal fatigue and eventual failure in the tooth 16 .
[0050] Secondly, the interference fit allows for easier removal of the ripping tooth 16 in that clay fines are no longer able to build up around the ripping tooth shaft 32 . As mentioned in the preamble of the invention, this often prevents the tooth from being able to be removed. In this case, simply breaking the taper will cause the tooth to fall out, and a means of achieving this will be described shortly.
[0051] Thirdly, the ripper boot of the present invention is not limited in its use and may be used in association with a wide variety of machinery including small to large bulldozer rippers, end cutting bits on dozer blades, dragline buckets, bucket dredges, excavators, and loader bucket teeth. Such boots are also less expensive to manufacture.
[0052] In order to ensure that the replaceable ripping tooth 16 is always fixed within the carrier 14 during use, a secondary locking means may also be used, preferably in the form of a retaining pin 36 . Illustrated in FIGS. 6-7 is a ripper boot 10 including such a retaining pin 36 . The tooth 16 includes a groove 38 extending transversely across a lower side thereof such that when it is fully inserted into socket 28 , the groove 38 becomes co-axially aligned with an aperture 40 which extends transversely through the solid portion 26 of the carrier 12 . Once aligned, the retaining pin 36 may simply be inserted through the aligned holes to lock the tooth in place.
[0053] It is envisaged that an interference fit is adequate in maintaining the tooth fixed within the socket, but a secondary locking means such as this may be used if required. The pin may be of the compressible type whereby prior to insertion, its cross section must be compressed so that following insertion it expands to provide a tighter fit. All other aspects of the ripper boot in FIGS. 6-7 are identical to those in the previous figures.
[0054] Removal of the ripping tooth 16 from the carrier 12 may be accomplished in a number of ways. The tooth 16 includes a protrusion or shoulder 42 extending outwards from the head portion 30 of the tooth 16 which is adapted to facilitate removal of the tooth 16 . The shoulder 42 may be engaged by an appropriate tool and pried off when the tooth has become worn following prolonged use.
[0055] Alternatively, the ripping tooth 16 may be removed by way of insertion of a push rod (not shown) or other similar object through an ejection hole 44 extending from the hollow portion 22 of the carrier 14 to the female socket 28 . As those skilled in the art would appreciate, when the ripping tooth 16 is locked within the female socket 28 , such action will force the ripping tooth 16 from the female socket 28 .
[0056] It is to be understood that the configuration of the ripping tooth 16 may vary. In this case, the pointed tip 34 includes a double inward taper before terminating into a point. This feature, combined with the high tensile properties of the tip 34 , ensures that even the hardest rock may be penetrated with minimal slip and that problems associated with existing ripper boot tips which become easily worn are alleviated. But other types of tips may be used such as single taper tips, or curved tips. Further, the cross-sectional shape of the ripping tooth shaft 32 and carrier bore 28 need not be square but may be any other shape such as triangular or circular, provided an interference fit is still achievable.
[0057] It is to be further understood that the configuration of the female socket 28 in the area adjacent the end of the ripping tooth shaft 32 may also vary. For example, in the drawings there is shown a clearance 46 between the end of the shaft 32 and the end of the bore 28 , as well as the ejection hole 44 . Another variation could be for the tapered walls of the bore 28 to simply extend the entire distance through to the hollow portion 22 as is the case in the second and third embodiments of the invention. A still further variation may be where there is no gap at all between the hollow portion 22 of the boot 12 and the bore 28 .
[0058] In using a replaceable ripping tooth that is adapted to be fixed during operation, such as those disclosed in the present invention, it has been found that previously encountered problems relating to ripper boot chatter, wear and tear on the ripping tooth, ripping tooth fracture, and other associated problems have been significantly reduced. More specifically, such ripper boots have resulted in benefits such as fuel savings of up to 10% due to reduced load on the bulldozer, savings of up to 50% in working time because of the ability to rip rock precisely, and total cost savings including manufacturing cost of up 10-20%.
[0059] The second embodiment of the invention is illustrated in FIGS. 8-9 and relates to a ripper boot 10 b which has the same interference fit tooth 16 as described above, but which includes an alternate angle of attack.
[0060] This angle of attack concept can be clearly appreciated in FIG. 10 which illustrates the ripper boot 10 b of the present invention, as well as a conventional ripper boot 48 in broken lines for the purpose of comparison. Those skilled in the art will appreciate that where the solid portion of the conventional ripper boot 48 extends in the same longitudinal direction as that of the carrier 14 , the solid portion 26 of the ripper boot 10 b is angled upwardly with respect to the carrier 14 when fully assembled. In having an upwardly angled solid portion 26 , those skilled in the art will appreciate that the ripping tooth 16 once inserted will also be angled with respect to the carrier 14 .
[0061] The angle of the solid portion 26 is shown in the drawings to be quite substantial for the purpose of clarity, however, through experimentation it has been found that an angle of approximately 6 degrees from the longitudinal axis of the carrier body is optimal. At this angle, the outer surface of the ripping tooth becomes aligned approximately parallel with the layers of rock being cleaved. These layers are typically, but not always, parallel with the ground surface.
[0062] Existing ripper boots may be modified to include the features of ripper boot 10 b . For example, a saw cut may be made at the junction between the carrier 14 and the solid portion 26 of the ripper boot 10 a of the first embodiment. The cut would be made at a desired angle relative to the longitudinal axis of the carrier. Then, when a solid portion is welded to the angled end of the carrier 14 , those skilled in the art will appreciate that it will extend at an angle corresponding with the angle of the cut.
[0063] It has been found that when the tooth is positioned at this angle, the boot cleaves through the ground more efficiently than hitherto known ripper boot arrangements resulting in similar benefits to those mentioned above including reduced chatter, reduced wear and tear on the tooth, and reduced load on the bulldozer. It is to be understood that the angle at which the solid portion 26 extends with respect to the carrier 14 may be made to vary depending on the required operation.
[0064] FIGS. 11-12 illustrate a ripper boot 10 c according to a third aspect of the present invention. The ripper boot 10 c differs from the ripper boot 10 b slightly in that rather than the solid portion 26 of the boot being angled, it extends longitudinally with respect to the carrier 12 as was the case in the ripper boot 10 a of the first embodiment. In this case though, a raised angle of attack is achieved by having a female socket 28 cast at a predetermined angle through the solid portion 26 of the boot so that the ripping tooth 16 may extend outwards therefrom at that angle. Again, for the purpose of brevity, the same reference numbers have been used.
[0065] The angle is such that in use, the ripping tooth 16 will extend slightly upwardly so as to become more parallel with the ground surface. The benefits of having a raised angle of attack as provided by this third embodiment of the invention have been described above.
[0066] Although not illustrated, it is to be understood that this ripper boot 10 c could also include a retaining pin for additional support as described previously.
[0067] Ripper boot 10 a could also be modified to include an angled ripping tooth according to this third embodiment by making a straight saw cut at the junction between the carrier 12 and the solid portion 26 and simply replacing the solid portion with one that has an angled bore cast there through.
[0068] Further advantages and improvements may very well be made to the present invention without deviating from its scope. Although the invention has been shown and described in what is conceived to be the most practical and preferred embodiment, it is recognized that departures may be made therefrom within the scope and spirit of the invention, which is not to be limited to the details disclosed herein but is to be accorded the full scope of the claims so as to embrace any and all equivalent devices and apparatus.
[0069] In any claims that follow and in the summary of the invention, except where the context requires otherwise due to express language or necessary implication, the word “comprising” is used in the sense of “including”, i.e. the features specified may be associated with further features in various embodiments of the invention.
|
The present invention relates to improvements to ripper boots of the type adapted to be mounted to a bulldozer tyne for use in cleaving through hard ground. The ripper boot embodied in the present invention has particular application in opal mining where sometimes extremely hard ground is to be penetrated and ripped. The ripper boot includes a replaceable ripping tooth which is secured within the boot by way of an interference fit so that during use, it does not rotate. The interference fit prevents particular matter from entering between the walls of the tooth and the associated socket. In further forms of the invention, the replaceable ripping tooth is angled upwardly with respect to the carrier so that the angle of attack of the ripping tooth is raised so that it is almost parallel with the ground. The ripper boot provides a number of benefits including improved cleaving effect, reduced chatter and drag, reduced wear and tear, and reduced load on associated machinery.
| 4
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is the U.S. National Stage Application (filed under 35 U.S.C. 371) of prior International Application No. PCT/US12/66895, filed Nov. 28, 2012, and published on Jun. 6, 2013 as WO 2013/082188, which claims the benefit of/priority to U.S. Provisional Application No. 61/629,762 filed Nov. 28, 2011.
FIELD OF THE INVENTION
[0002] The present invention relates to martensitic steel compositions and methods of production thereof. More specifically, the martensitic steels have tensile strengths ranging from 1700 to 2200 MPa. Most specifically, the invention relates to thin gage (thickness of ≦1 mm) ultra high strength steel with an ultimate tensile strength of 1700-2200 MPa and methods of production thereof.
BACKGROUND OF THE INVENTION
[0003] Low-carbon steels with martensitic microstructure constitute a class of Advanced High Strength Steels (AHSS) with the highest strengths attainable in sheet steels. By varying the carbon content in the steel, ArcelorMittal has been producing martensitic steels with tensile strength ranging from 900 to 1500 MPa for two decades. Martensitic steels are increasingly being used in applications that require high strength for side impact and roll over vehicle protection, and have long been used for applications such as bumpers that can readily be rolled formed.
[0004] Currently, thin gage (thickness of ≦1 mm) ultra high strength steel with ultimate tensile strength of 1700-2200 MPa with good roll formability, weldability, punchability and delayed fracture resistance is in demand for the manufacture of hang on automotive parts such as bumper beams. Light gauge, high strength steels are required to fend off competitive challenges from alternative materials, such as lightweight 7xxx series of aluminum alloys. Carbon content has been the most important factor in determining the ultimate tensile strength of martensitic steels. The steel has to have sufficient hardenability so as to fully transform to martensite when quenched from a supercritical annealing temperature.
SUMMARY OF THE INVENTION
[0005] The present invention comprises a martensitic steel alloy that has an ultimate tensile strength of at least 1700 MPa. Preferably, the alloy may have an ultimate tensile strength of at least 1800 MPa, at least 1900 MPa, at least 2000 MPa or even at least 2100 MPa. The martensitic steel alloy may have an ultimate tensile strength between 1700 and 2200 MPa. The martensitic steel alloy may have a total elongation of at least 3.5% and more preferably at least 5%.
[0006] The martensitic steel alloy may be in the form of a cold rolled sheet, band or coil and may have a thickness of less than or equal to 1 mm. The martensitic steel alloy may have a carbon equivalent of less than 0.44 using the formula Ceq=C+Mn/6+(Cr+Mo+V)/5+(Ni+Cu)/15, where Ceq is the carbon equivalent, and C, Mn, Cr, Mo, V, Ni, and Cu are in wt. % of the elements in the alloy.
[0007] The martensitic steel alloy may contain between 0.22 and 0.36 wt. % carbon. More specifically, the alloy may contain between 0.22 and 0.28 wt. % carbon or in the alternative the alloy may contain between 0.28 and 0.36 wt. % carbon. The martensitic steel alloy may further contain between 0.5 and 2.0 wt. % manganese. The alloy may also contain about 0.2 wt. % silicon. The optionally may contain one or more of Nb, Ti, B, Al, N, S, P.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIGS. 1 a and 1 b are schematic illustrations of annealing procedures useful in producing the alloys of the present invention;
[0009] FIGS. 2 a , 2 b and 2 c are SEM micrographs of experimental steels with 2.0% Mn-0.2% Si and various carbon contents ( 2 a has 0.22% C; 2 b has 0.25% C; and 2 c has 0.28% C) after hot rolling and simulated coiling at 580° C.;
[0010] FIG. 3 is a plot of the tensile properties at room temperature of experimental steel hot bands useful in producing alloys of the present invention;
[0011] FIGS. 4 a - 4 b are SEM micrographs of experimental steels with 0.22% C-0.2% Si-0.02% Nb and two different Mn contents ( 4 a has 1.48% and 4 b has 2.0%) after hot rolling and simulated coiling at 580° C.;
[0012] FIG. 5 is a plot of the tensile properties at room temperature of another experimental steel hot bands useful in producing alloys of the present invention;
[0013] FIGS. 6 a - 6 b are SEM micrographs of experimental steels with 0.22% C-2.0% Mn-0.2% Si and different Nb contents ( 6 a has 0% and 6 b has 0.018%) after hot rolling and simulated coiling at 580° C.;
[0014] FIG. 7 is a plot of the tensile properties at room temperature of yet another experimental steel hot bands useful in producing alloys of the present invention;
[0015] FIGS. 8 a - 8 f illustrate the effects of soaking temperature (830, 850 and 870° C.) and steel composition ( FIGS. 8 a & 8 b show varied C, 8 c & 8 d show varied Mn and 8 e & 8 f show varied Nb) on the tensile properties of steels of the present invention;
[0016] FIGS. 9 a - 9 f show the effects of quenching temperature (780,810 and 840° C.) and steel composition ( FIGS. 9 a & 9 b show varied C, 9 c & 9 d show varied Mn and 9 e & 9 f show varied Nb) on tensile properties of additional steels of the present invention;
[0017] FIGS. 10 a and 10 b are schematic depictions of the additional anneal cycles useful in producing alloys of the present invention;
[0018] FIGS. 11 a and 11 b plot the tensile properties at room temperature of hot bands useful in producing steels of the present invention, after hot rolling and simulated coiling at 580° C.;
[0019] FIGS. 12 a - 12 d are SEM micrographs at 1000× of the microstructure of hot band steels after hot rolling and simulated coiling at 660° C.;
[0020] FIGS. 13 a - 13 b plot the tensile properties of experimental hot band steels at room temperature;
[0021] FIGS. 14 a - 14 d represent the effects of soaking temperature (830° C., 850° C. and 870° C.), coiling temperature (580° C. and 660° C.), and alloy composition (Ti, B and Nb additions to the base steel) on the tensile properties of the steels after anneal simulation;
[0022] FIGS. 15 a - 15 d show the effects of quenching temperature (780° C., 810° C. and 840° C.), coiling temperature (580° C. and 660° C.), and alloy composition (Ti, B and Nb additions to the base steel) on the tensile properties of the steels after anneal simulation;
[0023] FIGS. 16 a - 16 c are even more schematic depictions of anneal cycles useful in producing the alloys of the present invention;
[0024] FIGS. 17 a to 17 e are SEM micrographs at 1,000× of hot rolled steels (0.28 to 0.36% C) after hot rolling and simulated coiling at 580° C.;
[0025] FIGS. 18 a and 18 b plot the corresponding tensile properties of the hot rolled steels of FIGS. 17 a - 17 e , at room temperature (after hot rolling and simulated coiling at 580° C.);
[0026] FIGS. 19 a - 19 e are SEM micrographs at 1,000× of hot rolled steels (0.28 to 0.36% C) after hot rolling and simulated coiling at 660° C.;
[0027] FIGS. 20 a and 20 b plot the corresponding tensile properties of the hot rolled steels of FIGS. 19 a - 19 e , at room temperature (after hot rolling and simulated coiling at 660° C.);
[0028] FIGS. 21 a - 21 d represents the effects of soaking temperature (830° C., 850° C. and 870° C.), coiling temperature (580° C. and 660° C.), and alloy composition (C content and B addition to the base steel) on the tensile properties of the steels after annealing simulation;
[0029] FIGS. 22 a - 22 d show the effects of quenching temperature (780° C., 810° C. and 840° C.), coiling temperature (580° C. and 660° C.), and alloy composition (C content and B addition to the base steel) on the tensile properties of the steels after annealing simulation;
[0030] FIGS. 23 a - 23 d illustrates the effect of composition and annealing cycle on ( 23 a - 23 b ) tensile strength and ( 23 c - 23 d ) ductility;
[0031] FIGS. 24 a - 24 l are micrographs of four alloys which were annealed using various soak/quenching temperature pairs; and
[0032] FIGS. 25 a - 25 d show the tensile properties of the steels with 0.5% to 2.0% Mn after coiling at 580° C., cold rolling (50% cold rolling reduction for the steel with 0.5 and 1.0% Mn and 75% cold rolling reduction for the steel with 2.0% Mn) and various annealing cycles.
DETAILED DESCRIPTION OF THE INVENTION
[0033] The present invention is a family of martensitic steels with tensile strength ranging from 1700 to 2200 MPa. The steel may be thin gauge (thickness of less than or equal to 1 mm) sheet steel. The present invention also includes the process for producing the very high tensile strength martensitic steels. Examples and embodiments of the present invention are presented below.
Example 1
Materials and Experimental Procedures
[0034] Table 1 shows the chemical compositions of some steels within the present invention, which includes a range of carbon content from 0.22 to 0.28 wt % (steels 2, 4 and 5), manganese content from 1.5 to 2.0 wt % (steels 1 and 3) and niobium content from 0 to 0.02 wt % (alloys 2 and 3). The remainder of the steel composition is iron and inevitable impurities.
[0000]
TABLE 1
ID
Steel
C
Mn
Si
Nb
Al
N
S
P
1
0.22C—1.5Mn—0.018Nb
0.22
1.48
0.198
0.019
0.036
0.0043
0.002
0.006
2
0.22C—2.0Mn
0.22
2.00
0.199
—
0.027
0.0049
0.002
0.006
3
0.22C—2.0Mn—0.018Nb
0.22
2.00
0.197
0.018
0.033
0.0045
0.002
0.006
4
0.25C—2.0Mn
0.25
1.99
0.201
—
0.025
0.005
0.003
0.009
5
0.28C—2.0Mn
0.28
2.01
0.202
—
0.032
0.0045
0.003
0.007
[0035] Five 45 Kg slabs were cast in the laboratory. After reheating and austenitization at 1230° C. for 3 hours, the slabs were hot rolled from 63 mm to 20 mm in thickness on a laboratory mill. The finishing temperature was about 900° C. The plates were air cooled after hot rolling.
[0036] After shearing and reheating the pre-rolled 20 mm thick plates to 1230° C. for 2 hours, the plates were hot rolled from a thickness of 20 mm to 3.5 mm. The finish rolling temperature was about 900° C. After controlled cooling at an average cooling rate of about 45° C./s, the hot bands of each composition were held in a furnace at 580° C. for 1 hour, followed by a 24-hour furnace cooling to simulate the industrial coiling process.
[0037] Three JIS-T standard specimens were prepared from each hot band for room temperature tensile test. Microstructure characterization of hot bands was carried out by Scanning Electron Microscopy (SEM) at the quarter thickness location in the longitudinal cross-sections.
[0038] Both surfaces of the hot rolled bands were ground to remove any decarburized layer. They were then subjected to 75% lab cold rolling to obtain full hard steels with final thickness of 0.6 mm for further annealing simulations.
[0039] Annealing simulation was performed using two salt pots and one oil bath. The effects of soaking and quenching temperatures were analyzed for all of the steels. A schematic illustration of the heat treatment is shown in FIGS. 1( a ) and 1 ( b ). FIG. 1( a ) illustrates the annealing processes with different soaking temperatures from 830° C. to 870° C. FIG. 1( b ) illustrates the annealing processes with different quenching temperatures from 780° C. to 840° C.
[0040] To study the effect of soaking temperature, the annealing process included reheating the cold rolled strips (0.6 mm thick) to 870° C., 850° C. and 830° C. respectively followed by isothermal holding for 60 seconds. The samples were immediately transferred to the second salt pot maintained at a temperature of 810° C. and isothermally held for 25 s. This was followed by a water quench. The samples were then reheated to 200° C. for 60 s in an oil bath, followed by air cooling to room temperature to simulate overage treatment. The holding times at soaking, quenching and overaging temperatures were chosen to closely approximate industrial conditions for this gauge.
[0041] To study the effect of quenching temperature, the analysis includes reheating of cold rolled strips to 870° C. for 60 seconds, followed by immediate cooling to 840° C., 810° C. and 780° C. After a 25 second isothermal hold at the quenching temperature, the specimens were quenched in water. The steels were then reheated to 200° C. for 60 seconds followed by air cooling to simulate the overage treatment. Three ASTM-T standard specimens were prepared from each annealed blank for tensile testing at room temperature.
[0042] The samples processed at 870° C. soaking temperature and quenched from 810° C. were selected for bend testing. A 90° free V-bend with the bending axis in the rolling direction was employed for bendability characterization. A dedicated Instron mechanical testing system with 90° die block and punches was utilized for this test. A series of interchangeable punches with different die radius facilitated the determination of minimum die radius at which the samples could be bent without microcracks. The test was run at a constant stroke of 15 mm/sec until the sample was bent by 90°. A 80 KN force and 5 second dwell time was deployed at the maximum bend angle after which the load was released and the specimen was allowed to spring back. In the present test, the range of die radius varied from 1.75 to 2.75 mm with 0.25 mm incremental increase. The sample surface after bend testing was observed under 10× magnification. A crack length on the sample bending surface that is smaller than 0.5 mm is considered to be a “micro crack”, and any that is larger than 0.5 mm is recognized as a crack and the test marked as a failure. Samples with no visible crack are identified as “passed test”.
Microstructure and Tensile Properties of Hot Rolled Bands
Effect of Composition on Microstructure and Tensile Properties of Hot Rolled Steels
[0043] FIGS. 2 a , 2 b and 2 c are SEM micrographs of experimental steels with 2.0% Mn-0.2% Si and various carbon contents ( 2 a has 0.22% C; 2 b has 0.25% C; and 2 c has 0.28% C) after hot rolling and simulated coiling at 580° C.
[0044] The increase in carbon content resulted in an increase in the volume fraction and the colony size of pearlite. The corresponding tensile properties at room temperature of the experimental steels are plotted in FIG. 3 , where strength in MPa (top half of the graph) and ductility in percentage (bottom half of the graph) are plotted against carbon content. In FIG. 3 and herein, UTS means ultimate tensile strength, YS means yield strength, TE means total elongation, UE means uniform elongation. As shown, the increase in carbon content from 0.22 to 0.28% led to a slight increase in ultimate tensile strength from 609 to 632 MPa, a slight decrease in yield strength from 440 to 426 MPa but little change in ductility (average TE and UE are about 16% and 11% respectively).
[0045] FIGS. 4 a - 4 b are SEM micrographs of experimental steels with 0.22% C-0.2% Si-0.02% Nb and two different Mn contents ( 4 a has 1.48% and 4 b has 2.0%) after hot rolling and simulated coiling at 580° C. An increase in the Mn content resulted in an increase in the volume fraction and in size of pearlite colony. The large grain size in the higher Mn steel can be attributed to grain coarsening during finish rolling and subsequent cooling. The hot rolling finish temperature was about 900° C., which is in the austenite region for both of the experimental steels but it is much higher than the Ar a temperature for the higher Mn steel. Thus, during and after finish rolling, the austenite in the higher Mn steel had a greater opportunity to coarsen, resulting in a coarser ferrite-pearlite microstructure after phase transformation.
[0046] The corresponding tensile properties of the experimental steels with 0.22% C-2.0% Mn at room temperature are plotted in FIG. 5 , where strength in MPa (top half of the graph) and ductility in percentage (bottom half of the graph) are plotted against manganese content. As shown, an increase in the Mn content from 1.48 to 2.0% led to a small increase in the ultimate tensile strength from 655 to 680 MPa, a marked decrease in yield strength from 540 to 416 MPa and a slight decrease in ductility from 22 to 18% for TE and from 12 to 11% for UE. The corresponding yield ratio (YR) dropped from 0.8 to 0.6 and yield point elongation (YPE) decreased from 3.1 to 0.3% with the increase in Mn content. The tremendous decrease in YS, YR and YPE in spite of solid solution strengthening by Mn may be attributed to the formation of martensite in the higher Mn steel. A small amount of martensite (even less than 5%) can create free dislocations surrounding ferrite to facilitate initial plastic deformation, as is well known for DP steels. In addition, higher hardenability of the higher Mn steel may also result in coarse austenite grain size.
[0047] FIGS. 6 a - 6 b are SEM micrographs of experimental steels with 0.22% C-2.0% Mn-0.2% Si and different Nb contents ( 6 a has 0% and 6 b has 0.018%) after hot rolling and simulated coiling at 580° C. An increase in the Nb content resulted in an increase in the volume fraction and colony size of pearlite, which can be explained by higher hardenability of the steel with Nb and lower temperature of pearlite formation.
[0048] The corresponding tensile properties of the compared steels with 0.22% C-2.0% Mn are illustrated in FIG. 7 , where strength in MPa (top half of the graph) and ductility in percentage (bottom half of the graph) are plotted against niobium content. As shown, the addition of 0.018% Nb led to an increase in the ultimate tensile strength (UTS) from 609 to 680 MPa, a small decrease in yield strength (YS) from 440 to 416 MPa and a slight increase in average TE from 16.8 to 18.0% with UE decreasing from 11.8 to 10.8%. The corresponding yield ratio (YR) dropped from 0.72 to 0.61 and yield point elongation (YPE) decreased from 2.3 to 0.3% with the increase in Nb content.
[0000] Tensile Properties of the Investigated Steels after Cold Rolling and Annealing Simulation
[0049] FIGS. 8 a - 8 f illustrate the effects of soaking temperature (830, 850 and 870° C.) and steel composition ( FIGS. 8 a & 8 b show varied C, 8 c & 8 d show varied Mn and 8 e & 8 f show varied Nb) on the tensile properties of steels. The decrease in soaking temperature from 870 to 850° C. resulted in an increase of 28-76 MPa in yield strength (YS) and 30-103 MPa in ultimate tensile strength (UTS), which may be attributed to the smaller grain size at lower soaking temperature. A further decrease in soaking temperature from 850 to 830° C. did not lead to a significant change in UTS. There is no effect of soaking temperature on ductility and the uniform/total elongation ranges from 3 to 4.75% in all the experimental steels. It should be stressed that UTS exceeding 2000 MPa and uniform/total elongation of ˜3.5-4.5% were achieved in the steel with 0.28% C-2.0% Mn-0.2% Si (see FIGS. 8 a - 8 b ).
[0050] FIGS. 9 a - 9 f show the effects of quenching temperature (780, 810 and 840° C.) and steel composition ( FIGS. 9 a & 9 b show varied C, 9 c & 9 d show varied Mn and 9 e & 9 f show varied Nb) on tensile properties of the investigated steels. There is no significant effect of quenching temperature on strength and ductility when 100% martensite is obtained. The uniform/total elongation ranges from 2.75 to 5.5% in all the experimental steels. The data suggests that a wide process window is feasible during anneal.
[0051] FIGS. 8 a , 8 b , 9 a , and 9 b show that an increase in the C content resulted in a significant increase in tensile strength but had little effect on ductility. Taking the annealing cycle of 830° C. (soaking temperature)-810° C. (quenching temperature) as an example, the increase in YS and UTS is 163 and 233 MPa, respectively, when C content is increased from 0.22 to 0.28 wt %. The increase in Mn content from 1.5 to 2.0 wt % has barely any effect on strength and ductility (see FIGS. 8 c , 8 d , 9 c and 9 d ). The addition of Nb (about 0.02 wt %) led to an increase in YS up to 94 MPa with almost no effect on UTS but a decrease in total elongation of 2.4% (see FIGS. 8 e , 8 f , 9 e and 9 f ).
Bendability of the Investigated Steels
[0052] Table 2 summarizes the effects of C, Mn and Nb on tensile properties and bendability of the experimental steels after 75% cold rolling and annealing. The annealing cycle included: heating the cold rolled bands (about 0.6 mm thick) to 870° C., isothermal hold for 60 seconds at soaking temperature, immediate cooling to 810° C., 25 seconds isothermal holding at that temperature, followed by rapid water quench. The panels were then reheated to 200° C. in an oil bath and held for 60 seconds, followed by air cooling to simulate overage treatment. The data shows that carbon has the strongest effect on strength and a slight effect on bendability. The addition of Nb increases yield strength and improves bendability. The improvement in bendability is achieved in spite of marginally inferior elongation. An increase in the Mn content from 1.5 to 2.0% in the Nb bearing steel has no significant effect on tensile properties but results in a big improvement in bendability.
[0000]
TABLE 2
T soak
T GJC
T O\
Gauge
YS
TS
Bendability
Bendability micro
Steel
° C.
° C.
° C.
mm
MPa
MPa
YS/TS
UE %
TE %
YPE %
pass
crack < 0.5 mm
0.22C—1.5Mn—0.018Nb
870
810
200
0.69
1518
1737
0.87
3.6
4
0
4.0t
2.9t
0.22C—2.0Mn—0.018Nb
870
810
200
0.69
1518
1766
0.86
3.8
3.7
0
2.9t
2.5t
0.22C—2.0Mn
870
810
200
0.66
1465
1760
0.83
4.1
4.2
0
3.7t
2.2t
0.25C—2.0Mn
870
810
200
0.68
1533
1858
0.83
4
4.8
0
3.7t
2.6t
0.28C—2.0Mn
870
810
200
0.68
1581
1927
0.82
4.3
4.2
0
4.0t
3.2t
Example 2
[0053] In order to reduce carbon equivalent, thus to improve the weldability of the steels of Example 1, steels containing 0.28 wt % carbon and reduced manganese content (about 1.0 wt % vs. 2.0 wt % of Example 1) along with were produced. The alloys were cast into slabs, hot rolled, cold rolled, annealed (simulated) and over age treated. In addition, the
[0000] effect of Mn content (1.0 and 2.0% Mn) on the properties of hot rolled bands and annealed products are described in detail.
Heat Preparation
[0054] Table 3 shows the chemical compositions of investigated steels. The alloy design analyzed the effects of incorporated Ti (steels 1 and 2), B (steels 2 and 3) and Nb (alloys 3 and 4).
[0000]
TABLE 3
ID
Steel
C
Mn
Si
S
P
N
Al
Ti
B
Nb
1
Base
0.28
0.98
0.204
0.003
0.007
0.0049
0.035
2
Base-Ti
0.28
0.98
0.198
0.003
0.005
0.0047
0.04
0.024
3
Base-Ti—B
0.28
0.98
0.204
0.003
0.005
0.0047
0.04
0.024
0.0018
4
Base-Ti—B—Nb
0.28
0.97
0.202
0.003
0.006
0.0048
0.037
0.024
0.0017
0.029
[0055] Four 45 Kg slabs (one of each alloy) were cast in the laboratory. After reheating and austenitization at 1230° C. for 3 hours, the slabs were hot rolled from 63 mm to 20 mm in thickness on a laboratory mill. The finishing temperature was about 900° C. The plates were air cooled after hot rolling.
Hot Rolling and Microstructure/Tensile Property Investigation
[0056] After shearing and reheating the pre-rolled 20 mm thick plates to 1230° C. for 2 hours, the plates were hot rolled from a thickness of 20 mm to 3.5 mm. The finish rolling temperature was about 900° C. After controlled cooling at an average cooling rate of about 45° C./s, the hot bands of each composition were held in a furnace at 580° C. and 660° C. respectively for 1 hour, followed by a 24-hour furnace cooling to simulate the industrial coiling process. The use of two different coiling temperatures was designed to understand the available process window during hot rolling for the manufacture of this product.
[0057] A recheck of hot band compositions was performed by inductively coupled plasma (ICP). In comparison with ingot derived data, a carbon loss is generally observed in the hot bands. Three JIS-T standard specimens were prepared from each hot band for room temperature tensile tests. Microstructure characterization of hot bands was carried out by Scanning Electron Microscopy (SEM) at the quarter thickness location of longitudinal cross-sections.
Cold Rolling
[0058] After grinding both surfaces of the hot rolled bands to remove any decarburized layer, the steels were cold rolled in the laboratory by 50% to obtain full hard steels with final thickness of 1.0 mm for further annealing simulations.
Annealing Simulation
[0059] The effects of soaking and quenching temperatures during annealing on the mechanical properties of the steels were investigated for all of the experimental steels. A schematic of the anneal cycles is shown in FIGS. 10 a and 10 b . FIG. 10 a illustrates the annealing processes with different soaking temperatures from 830° C. to 870° C. FIG. 10 b illustrates the annealing processes with different quenching temperatures from 780° C. to 840° C.
[0060] The annealing process includes reheating the cold band (about 1.0 mm thick) to 870° C., 850° C. and 830° C. for 100 s, respectively, to investigate the effect of soaking temperature on final properties. After immediate cooling to 810° C. and isothermal holding for 40 s, water quench was applied. The steels were then reheated to 200° C. for 100 s, and followed by air cooling to simulate overaging treatment.
[0061] The annealing process includes reheating the cold band to 870° C. for 100 s and immediate cooling to 840° C., 810° C. and 780° C. respectively to investigate the effect of quenching temperature on the mechanical properties of the steels. Water quench was employed after 40 s isothermal hold at the quenching temperature. The steels were then reheated to 200° C. for 100 s, and followed by air cooling to simulate the overaging treatment.
Tensile Property and Bendability of Annealed Steels
[0062] Three ASTM-T standard tensile specimens were prepared from each annealed band for room temperature tensile test. Samples processed by one annealing cycle were selected for bend testing. This annealing cycle involved the reheating of the cold band (about 1.0 mm thick) to 850° C. for 100 s, immediate cooling to 810° C., 40 s isothermal hold at quench temperature, followed by water quench. The steels were then reheated to 200° C. for 100 s, and followed by air cooling to simulate the overaging treatment. A 90° free V-bend testing along the rolling direction was employed for bendability characterization. In the present study, the range of die radius varied from 2.75 to 4.00 mm at 0.25 mm increments. The sample surface after bend testing was observed under 10× magnification. When the crack length on the sample at the outer bend surface is smaller than 0.5 mm the crack is deemed a “micro crack”. A crack larger than 0.5 mm is recognized as a failure. Samples without any visible crack are identified as “passed test”.
Chemical Analysis of the Hot Bands
[0063] Table 4 shows the chemical compositions of the steels with different Ti, B and Nb contents after hot rolling. Compared with the compositions of ingots (Table 3), there was about 0.03% carbon and 0.001% B loss after hot rolling.
[0000]
TABLE 4
ID
Steel
C
Mn
Si
S
P
N
Al
Ti
B
Nb
1
Base (0.25C—1.0Mn—0.2Si)
0.249
0.985
0.204
0.003
0.007
0.0047
0.034
2
Base-0.025Ti
0.247
0.981
0.197
0.003
0.005
0.005
0.038
0.024
3
Base-0.025Ti—0.001B
0.254
0.996
0.201
0.003
0.005
0.0044
0.039
0.024
0.001
4
Base-0.025Ti—0.001B—0.03Nb
0.251
0.988
0.201
0.003
0.005
0.0044
0.038
0.024
0.001
0.028
Microstructure and Tensile Properties of Hot Bands
[0064] FIGS. 11 a and 11 b show the tensile properties (JIS-T standard) of experimental steels (of Table 4) at room temperature, after hot rolling and simulated coiling at 580° C. The base composition consists of 0.28% C-1.0% Mn-0.2% Si. FIG. 11 a graphically depicts the strength of the four alloys, while FIG. 11 b plots their ductility. It can be seen that the addition of Ti, B and Nb led to significant increases in the ultimate tensile strength from 571 to 688 MPa yield strength from 375 to 544 MPa, and a decrease in total and uniform elongations (TE: from 32 to 13%; UE: from 17 to 11%). The addition of Nb to the Ti—B steel resulted in a pronounced drop in total elongation from 28 to 13%.
[0065] As shown in FIGS. 12 a - 12 d , the microstructure of steels after hot rolling and simulated coiling at 660° C. consist of ferrite and pearlite for each laboratory processed experimental steel. FIGS. 12 a - 12 d are SEM micrographs at 1000× of the base alloy, base alloy+Ti, base alloy+Ti & B, and base alloy+Ti, B and Nb, respectively. The addition of B seems to result in slightly larger sized pearlite islands ( FIG. 12 c ). The ferrite-pearlite microstructure is elongated along the rolling direction in the Nb added steel ( FIG. 12 d ), which may be attributed to the Nb addition retarding austenite recrystallization during hot rolling. Thus, the finish rolling occurred in the austenite non-recrystallization region, and the elongated ferrite-pearlite microstructure was transformed directly from the deformed austenite.
[0066] The corresponding tensile properties of the experimental steels at room temperature are shown in FIGS. 13 a - 13 b . FIG. 13 a graphically depicts the strength of the four alloys, while FIG. 13 b plots their ductility. It can be seen that the addition of Nb (0.03%) led to significant increases in ultimate tensile strength from 535 to 588 MPa and yield strength from 383 to 452 MPa, and slight decreases in total elongation from 31.3 to 29.0% and uniform elongation from 17.8 to 16.4%.
Effect of Coiling Temperature on Tensile Properties
[0067] Comparing the tensile properties in FIGS. 11 and 13 , the increase in coiling temperature from 580° C. to 660° C. led to a decrease in strength and an increase in ductility, attributes favorable for increased cold reduction possibility and enhanced gauge-width capability. The additions of Ti, B and Nb to the base steel have less of an effect on the tensile properties of the steels at the higher coiling temperature of 660° C. in comparison to 580° C. The purpose of studying the effect of coiling at 660° C. in the laboratory was to understand the effect of coiling temperature on both, hot band strength and the strength of the cold rolled and annealed martensitic steels.
[0000] Tensile Properties of the Steels after Annealing Simulation
[0068] FIGS. 14 a - 14 d represent the effects of soaking temperature (830° C., 850° C. and 870° C.), coiling temperature (580° C. and 660° C.), and alloy composition (Ti, B and Nb additions to the base steel) on the tensile properties of the steels after anneal simulation. FIGS. 14 a and 14 b plot the strengths of the four alloys at different soaking temperatures and at coiling temperatures of 580° C. and 660° C., respectively. FIGS. 14 c and 14 d plot the ductilities of the four alloys at different soaking temperatures and at coiling temperatures of 580° C. and 660° C., respectively. It can be seen that a decrease in the soaking temperature from 870° C. to 830° C. resulted in increases in yield strength of 41 MPa and ultimate tensile strength of 56 MPa for Ti—B steel after hot rolling and simulated coiling at 580° C. ( FIG. 14 a ). For Ti—B—Nb steel, after simulated coiling at the same temperature ( FIG. 14 a ), the highest strength was represented at the soaking temperature of 850° C. (YS: 1702 MPa and UTS: 1981 MPa). Further increase or decrease of soaking temperature will not improve the strength of Ti—B—Nb steel. The soaking temperature had no obvious effect on the strength for Ti—B of Ti—B—Nb steels after simulated coiling at 660° C. It also had no significant effect on strength for the base and Ti steels at both coiling temperatures, and no effect on ductility for all of the experimental steels.
[0069] FIGS. 15 a - 15 d show the effects of quenching temperature (780° C., 810° C. and 840° C.), coiling temperature (580° C. and 660° C.), and alloy composition (Ti, B and Nb additions to the base steel) on the tensile properties of the steels after anneal simulation. FIGS. 15 a and 15 b plot the strengths of the four alloys at different quenching temperatures and at coiling temperatures of 580° C. and 660° C., respectively. FIGS. 15 c and 15 d plot the ductilities of the four alloys at different quenching temperatures and at coiling temperatures of 580° C. and 660° C., respectively. A decrease in the quenching temperature from 840° C. to 780° C. resulted in increases in both yield and ultimate tensile strengths of about 50-60 MPa in the base and Ti steels after hot rolling and simulated coiling at 580° C. ( FIG. 15 a ). The quenching temperature had no obvious effect on the strength of base and Ti steels after simulated coiling at 660° C. It also had no significant effect on the strength of Ti—B and Ti—B—Nb steels at both coiling temperatures, and on ductility for all of the experimental steels.
Effect of Coiling Temperature (580° C. and 660° c.)
[0070] Comparing FIGS. 14 a and 15 a with FIGS. 14 b and 15 b , the increase in coiling temperature from 580° C. to 660° C. did not lead to a significant change in the tensile strength, but resulted in a slight decrease in the yield strength of about 50 MPa on average for all of the experimental steels at various annealing conditions. Increasing coiling temperature did not have a measurable effect on ductility in the Ti and Ti—B steels, but slightly reduced by about 0.5%, the ductility of the base and Ti—B—Nb steels. These small changes are, however, within the range of test deviation and therefore, not very significant.
Effect of Composition (Ti, B and Nb)
[0071] As shown in FIGS. 14 a - 14 d and 15 a - 15 d , the addition of Ti and B in 0.28% C-1.0% Mn-0.2% Si steel did not have a significant effect on strength at both coiling temperatures of 580° C. and 660° C. The addition of Nb resulted in increases in yield strength of 45-103 MPa and tensile strength of 26-85 MPa at a coiling temperature of 580° C. ( FIG. 14 a ), but not for 660° C. ( FIG. 14 b ). Except for the Ti added steel which displayed a slightly better ductility at 660° C. coiling temperature ( FIGS. 14 d and 15 d ), alloy additions generally led to a slight decrease in ductility (<1%).
[0000] Bendability of the Steels after Anneal Simulation
[0072] Table 5 summarizes the effect of Ti, B and Nb on the tensile properties and bendability of the steels after 50% cold rolling and annealing after simulated coiling at 580° C. The annealing process consisted of reheating the cold band (about 1.0 mm thick) to 850° C. for 100 seconds, immediate cooling to 810° C., 40 seconds isothermal hold at “quench” temperature, followed by water quench. The steels were then reheated to 200° C. for 100 seconds followed by air cooling to simulate overaging treatment (OA). As shown, it was possible to produce steels with ultimate tensile strength between 1850 and 2000 MPa by varying alloy composition. The steel with only C, Mn and Si demonstrated the best bendability. The addition of Nb increased strength with a slight deterioration of bendability. Bendability pass defined as “micro crack length smaller than 0.5 mm at 10× magnification.
[0000]
TABLE 5
T soak
T quench
T OA
Gauge
YS
UTS
Bendability
ID
Steel
° C.
° C.
° C.
mm
YPE %
MPa
MPa
YS/UTS
UE %
TE %
pass
1
Base (0.28C—1.0Mn—0.2Si)
850
810
200
1.03
0
1599
1896
0.84
4.3
5.7
3.5t
2
Base-0.025Ti
850
810
200
0.99
0
1597
1901
0.84
4
4.8
>4.0t
3
Base-0.025Ti—0.001B
850
810
200
1
0
1578
1886
0.84
3.5
4.9
3.75t
4
Base-0.025Ti—0.001B—0.03Nb
850
810
200
0.99
0
1702
1981
0.86
3.4
4.4
>4.0t
Comparison with Example 1
Effect of Manganese
[0073] The steel with 0.28% C-2.0% Mn-0.2% Si was presented in Example 1 above. We can compare its behavior with the steel of Example 2 containing 0.28% C-1.0% Mn-0.2% Si to investigate the effect of Mn (1.0 and 2.0%) on tensile properties. The detailed chemical compositions of both steels are shown in Table 6.
[0000] TABLE 6 Steel C Mn Si S P N Al Example 1 (0.28C—1.0Mn—0.2Si) 0.249 0.985 0.204 0.003 0.007 0.0047 0.034 Example 2 (0.28C—2.0Mn—0.2Si) 0.25 2.01 0.202 0.003 0.007 0.0045 0.032
Tensile Properties of Hot Rolled Bands with 1.0 and 2.0% Mn
[0074] Table 7 displays the tensile properties of the steels with 1.0% and 2.0% Mn respectively after hot rolling and simulated coiling at 580° C. For the tensile properties of hot rolled bands, the steel with the lower Mn content showed a lower strength than the steel with the higher Mn content (51 MPa lower in YS and 61 MPa lower in UTS). This may facilitate a higher extent of cold rolling for the low Mn steel.
[0000]
TABLE 7
Gauge,
YS,
UTS,
Steel
mm
YPE, %
MPa
MPa
YS/UTS
UE, %
TE, %
0.28C—1.0Mn—0.2Si
3.44
1.68
375
571
0.66
17.6
32.2
0.28C—2.0Mn—0.2Si
3.67
1.82
426
632
0.67
11.3
15.8
[0075] Table 8 shows the tensile properties of the steels with 1.0% and 2.0% Mn respectively after cold rolling (50% cold rolling reduction for the steel with 1.0% Mn and 75% cold rolling reduction for the steel with 2.0% Mn) and various annealing cycles. It can be seen that at the same annealing treatment of 870° C. (soaking), 840° C. (quench) and 200° C. (overaging), Mn content had no significant effect on strength. At the same quenching temperature of 810° C., the decrease in soaking temperature from 870 to 830° C. did not affect the strength of the steel with 1.0% Mn, but significantly increased the strength of the steel with 2.0% Mn by about 90 MPa. This indicates that the steel with 1.0% Mn is quite stable in strength regardless soaking temperature (870 to 830° C.), and the steel with 2.0% Mn is more sensitive to the soaking temperature, perhaps due to grain coarsening at higher anneal temperatures. The steel with 1.0% Mn will be relatively easier to process during manufacturing due to the wider process windows.
[0000] TABLE 8 Gauge T Soak ° C. T Quench ° C. T OA ° C. YS TS Steel mm 100 s 60 s 40 s 25 s 100 s 60 s YPE % MPa MPa YS/UTS UE % TE % 0.28 C 1.03 870 840 200 0 1593 1888 0.84 4.2 6 1.0 Mn 1.03 870 810 200 0 1597 1882 0.85 4.1 5.5 0.2 Si 0.95 870 780 200 0 1652 1945 0.85 4 5.5 1.03 850 810 200 0 1599 1896 0.84 4.3 5.7 1.03 830 810 200 0 1606 1896 0.85 4.3 5.5 0.28 C 0.68 870 840 200 0 1589 1891 0.84 3.8 3.8 2.0 Mn 0.68 870 810 200 0 1581 1927 0.82 4.3 4.3 0.2 Si 0.68 870 780 200 0 1558 1907 0.82 4.5 5.4 0.69 850 810 200 0 1657 2023 0.82 3.6 3.6 0.69 830 810 200 0 1656 2019 0.82 3.4 4.4
Bendability of Annealed Steels with 1.0 and 2.0% Mn
[0076] Table 9 lists the tensile properties and bendability of the steels with 1.0% and 2.0% Mn after anneal simulation. The steel with 1.0% Mn demonstrated a better bendability (3.5t compared to 4.0t) at a comparable strength level. Bendability pass is defined as micro crack length smaller than 0.5 mm at 10× magnification.
[0000]
TABLE 9
Gauge
T Soak
T GJC
T OA
YS
TS
Bendability
Steel
mm
° C.
° C.
° C.
YPE %
MPa
MPa
YS/UTS
UE %
TE %
pass
0.28C—1.0Mn—0.2Si
1.03
850
810
200
0
1599
1896
0.84
4.3
5.7
3.5t
0.28C—2.0Mn—0.2Si
0.68
870
810
200
0
1581
1927
0.82
4.3
4.3
4.0t
Example 3
[0077] To ensure good weldability of the steels, the carbon equivalent (C eq ) should be less than 0.44. The carbon equivalent for the present steels is defined as:
[0000] C eq =C+Mn/6+(Cr+Mo+V)/5+(Ni+Cu)/15.
[0000] Thus, at a C content of 0.28 wt % and Mn content of 1 or 2 wt %, the weld integrity is determined to be unacceptable. The present examples are designed to reduce the Ceq and still meet the strength and ductility needs. High carbon content is beneficial for increasing strength but deteriorates weldability. According to the carbon equivalent formula, Mn is another element which deteriorates weldability. Thus, the motivation is to maintain a certain amount of carbon content (at least 0.28%) to achieve sufficient ultra-high strength and to study the effect of Mn content on UTS. The inventors look to reduce Mn content to improve the weldability but at maintain an ultra-high strength level.
Heat Preparation
[0078] Table 10 shows the chemical compositions of investigated steels in Example 3. The alloy design incorporated the understanding of the effect of C content and B addition on tensile properties in the final annealed products.
[0000]
TABLE 10
No.
ID
C
Mn
Si
Ti
B
Al
N
S
P
C eg
1
28C
0.282
0.577
0.199
0.021
0.02
0.004
0.005
0.004
0.38
2
28C—2B
0.281
0.58
0.197
0.022
0.0016
0.022
0.0042
0.004
0.004
0.38
3
32C
0.321
0.578
0.195
0.021
0.021
0.0044
0.004
0.004
0.42
4
32C—2B
0.323
0.578
0.196
0.022
0.0017
0.032
0.0053
0.004
0.005
0.42
5
36C
0.363
0.58
0.196
0.022
0.025
0.0044
0.004
0.004
0.46
[0079] Five 45 Kg slabs (one of each alloy) were cast in the laboratory. After reheating and austenitization at 1230° C. for 3 hours, the slabs were hot rolled from 63 mm to 20 mm in thickness on a laboratory mill. The finishing temperature was about 900° C. The plates were air cooled after hot rolling.
Hot Rolling and Microstructure/Tensile Property Investigation
[0080] After shearing and reheating the pre-rolled 20 mm thick plates to 1230° C. for 2 hours, the plates were hot rolled from a thickness of 20 mm to 3.5 mm. The finish rolling temperature was about 900° C. After controlled cooling at an average cooling rate of about 45° C./s, the hot bands of each composition were held in a furnace at 580° C. and 660° C. respectively for 1 hour, followed by a 24-hour furnace cooling to simulate industrial coiling process. The use of two different coiling temperatures was designed to understand the available process window during hot rolling for the manufacture of this product.
[0081] Three JIS-T standard specimens were prepared from each hot rolled steel (also known as a “hot band”) for room temperature tensile tests. Microstructure characterization of hot bands was carried out by Scanning Electron Microscopy (SEM) at the quarter thickness location of longitudinal cross-sections.
Cold Rolling and Annealing Simulation
[0082] After grinding both surfaces of the hot rolled bands to remove any decarburized layer, the steels were cold rolled in the laboratory by 50% to obtain full hard steels with final thickness of 1.0 mm for further annealing simulations.
[0083] The effects of soaking, quenching temperatures and a comparison of different combination of soaking and quenching temperatures during annealing on the mechanical properties of the steels were investigated for all of the experimental steels. A schematic of the anneal cycles is shown in FIGS. 16 a - 16 c . FIG. 16 a depicts the anneal cycle with varied soaking temperature from 830° C. to 870° C. FIG. 16 b depicts the anneal cycle with varied quenching temperature from 780° C. to 840° C. FIG. 16 c depicts the anneal cycle with varied combinations of soaking and quenching temperatures.
Effect of Soaking Temperature
[0084] The annealing process includes reheating the cold band (about 1.0 mm thick) to 870° C., 850° C. and 830° C. for 100 seconds, respectively, to investigate the effect of soaking temperature on the final properties. After immediate cooling to 810° C. and isothermal holding for 40 seconds, water quench was applied. The steels were then reheated to 200° C. for 100 seconds, followed by air cooling to simulate overaging treatment.
Effect of Quenching Temperature
[0085] The annealing process includes reheating the cold band to 870° C. for 100 seconds and immediate cooling to 840° C., 810° C. and 780° C. respectively to investigate the effect of quenching temperature on the mechanical properties of the steels. Water quench was employed after 40 seconds of isothermal hold at the quenching temperature. The steels were then reheated to 200° C. for 100 seconds, followed by air cooling to simulate overaging treatment.
Effect of the Different Combination of Annealing Cycle
[0086] The annealing cycle includes reheating the cold rolled steels to 790° C., 810° C. and 830° C. for 100 seconds respectively, immediate cooling to various quench temperatures (770° C., 790° C. and 810° C. respectively), isothermal holding for 40 seconds, followed by water quench. The steels were then reheated to 200° C. for 100 seconds, followed by air cooling to simulate overaging treatment.
Tensile Property and Bendability of Annealed Steels
[0087] ASTM-T standard tensile specimens were prepared from each annealed band for room temperature tensile test. The samples processed by one annealing cycle were selected for bend testing. This annealing cycle involved the reheating of the cold band (about 1.0 mm thick) to 850° C. for 100 seconds, immediate cooling to 810° C., 40 seconds isothermal hold at the quench temperature, followed by water quench. The steels were then reheated to 200° C. for 100 seconds, followed by air cooling to simulate overaging treatment. A 90° free V-bend test along the rolling direction was employed for bendability characterization. In the present study, the range of die radius varied from 2.75 to 4.00 mm at 0.25 mm increments. The sample surface after bend testing was observed under 10× magnification. A crack length on the sample at the outer bend surface that is smaller than 0.5 mm is considered to be a “micro crack”, and a crack larger than 0.5 mm is recognized as a failure. A sample without any length of visible crack is identified as “passed the test”.
Microstructure and Tensile Properties of Hot Bands
[0088] FIGS. 17 a to 17 e are SEM micrographs at 1,000× of hot rolled steels (0.28 to 0.36% C) after hot rolling and simulated coiling at 580° C. The increase in carbon content and the addition of boron led to an increase in martensite volume fraction, which can be attributed to the role of C and B in increasing hardenability. FIG. 17 a is an SEM of the steel with 0.28C. FIG. 17 b is an SEM of the steel with 0.28C-0.002B. FIG. 17 c is an SEM of the steel with 0.32C. FIG. 17 d is an SEM of the steel with 0.32C-0.002B. FIG. 17 e is an SEM of the steel with 0.36C.
[0089] The corresponding tensile properties of the experimental steels at room temperature (after hot rolling and simulated coiling at 580° C.) are shown in FIGS. 18 a and 18 b . FIG. 18 a plots the strength of the alloys versus carbon content, with and without boron. FIG. 18 b plots the ductility of the alloys versus carbon content, with and without boron. The increase in carbon content from 0.28% to 0.36% led to an increase in ultimate tensile strength from 529 to 615 MPa and yield strength from 374 to 417 MPa. Total and uniform elongations remained similar at 29% and 15%, respectively. The addition of 0.002% boron in 0.28 and 0.32% C steels resulted in an increase in UTS of about 40 MPa.
[0090] FIGS. 19 a - 19 e are SEM micrographs at 1,000× of hot rolled steels (0.28 to 0.36% C) after hot rolling and simulated coiling at 660° C. FIG. 19 a is an SEM of the steel with 0.28C. FIG. 19 b is an SEM of the steel with 0.28C-0.002B. FIG. 19 c is an SEM of the steel with 0.32C. FIG. 19 d is an SEM of the steel with 0.32C-0.002B. FIG. 19 e is an SEM of the steel with 0.36C. The addition of boron led to a slight grain coarsening, which may be attributed to B retarding phase transformation during cooling. Thus, the finish rolling occurred in the austenite region with relatively coarse austenite grain size for the B added steels, and the coarse austenite transformed directly to a coarse ferrite-pearlite microstructure.
[0091] The corresponding tensile properties at room temperature (after hot rolling and simulated coiling at 660° C.) are represented in FIGS. 20 a and 20 b . FIG. 20 a plots the strength of the alloys versus carbon content, with and without boron. FIG. 20 b plots the ductility of the alloys versus carbon content, with and without boron. The increase in carbon content from 0.28% to 0.36% did not significantly impact tensile properties. The addition of 0.002% boron in 0.28 and 0.32% C steels resulted in a slight decrease in strength which may be due to grain coarsening. Based on the observed strength levels, the steels should be easily cold rolled to light gauges without any difficulty.
Effect of Coiling Temperature on Tensile Properties
[0092] Comparing the tensile properties in FIGS. 18 a - 18 b and FIGS. 20 a - 20 b , the increase in coiling temperature from 580° C. to 660° C. led to a decrease in strength and an increase in ductility, which attributes favorable the possibility of increased cold reduction and enhanced gauge-width capability. The increase in C content from 0.28% to 0.36% and the addition of B to the base steel have less effect on the tensile properties of the steels at the higher coiling temperature of 660° C. in comparison with 580° C. The purpose of studying the effect of coiling at 660° C. in the laboratory was to understand the effect of coiling temperature on both, hot band strength and the strength of the cold rolled and annealed martensitic steels.
[0000] Tensile Properties of the Steels after Annealing Simulation
Effect of Soaking Temperature (830° C., 850° C. and 870° C.)
[0093] FIGS. 21 a - 21 d represents the effects of soaking temperature (830° C., 850° C. and 870° C.), coiling temperature (580° C. and 660° C.), and alloy composition (C content and B addition to the base steel) on the tensile properties of the steels after annealing simulation. FIGS. 21 a and 21 b plot the strengths of the five alloys at different soaking temperatures and at coiling temperatures of 580° C. and 660° C., respectively. FIGS. 21 c and 21 d plot the ductilities of the five alloys at different soaking temperatures and at coiling temperatures of 580° C. and 660° C., respectively. It can be seen that martensitic steels with UTS level of 2000 to greater than 2100 MPa and TE of 3.5-5.0% can be obtained in the laboratory using the 0.32 and 0.36% C steel compositions at soak temperatures of 830 and 850° C. A decrease in the soaking temperature from 870° C. to 850° C. resulted in a slightly increase in strength for most of the steels. The increase in coiling temperature had no significant effect on strength but slightly improved ductility in most of cases. The increase in C content from 0.28 to 0.36% resulted in an increase in UTS of approximately 200 MPa. The addition of 0.002% B to the base steel led to a decrease in strength for the lower coiling temperature of 580° C. but not for the coiling temperature of 660° C. There was no significant effect of B addition on ductility regardless of coiling temperature.
Effect of Quenching Temperature (780° C., 810° C. and 840° C.)
[0094] FIGS. 22 a - 22 d show the effects of quenching temperature (780° C., 810° C. and 840° C.), coiling temperature (580° C. and 660° C.), and alloy composition (C content and B addition to the base steel) on the tensile properties of the steels after annealing simulation. FIGS. 22 a and 22 b plot the strengths of the five alloys at different quenching temperatures and at coiling temperatures of 580° C. and 660° C., respectively. FIGS. 22 c and 22 d plot the ductilities of the five alloys at different quenching temperatures and at coiling temperatures of 580° C. and 660° C., respectively. It can be seen that martensitic steels with a UTS close to or exceeding 2100 MPa and a TE of 3.5-5.0% can be obtained in the laboratory using the steel with 0.36% C at the soaking temperature of 870° C. and various quench temperatures. In comparison with the results in FIGS. 21 a and 21 b , the steels with not only 0.36% C but also 0.32% C could be heat treated to obtain a UTS level of 2000-2100 MPa and a TE of 3.5-5.0% at soaking temperatures of 830 and 850° C. Thus, a soak temperature of about 850° C. can help to achieve optimal mechanical properties. A decrease in the quenching temperature from 840° C. to 780° C. had no major effect on tensile properties for the steels with 0.32 and 0.36% C regardless of the addition of B and coiling temperature. However, a decrease in the quenching temperature from 840° C. to 780° C. for the steels with 0.28% C (coiling temperature of 580° C.) led to an decrease in strength by 100 MPa when there was no B addition, and this effect became less obvious when there was B addition, i.e. only 40 MPa increase. It demonstrates that B addition is beneficial for the stabilization of tensile properties, especially for the steels with a relatively low C content. The increase in C content from 0.28 to 0.36% resulted in an increase in UTS of approximately 200-300 MPa with no obvious change in ductility especially for the higher coiling temperature of 660° C. Overall, compared to the steels after coiling at 580° C., the tensile properties of the steels coiled at 660° C. had less sensitivity to the quench temperatures.
[0095] FIGS. 23 a - 23 d illustrates the effect of composition and annealing cycle on ( 23 a - 23 b ) tensile strength and ( 23 c - 23 d ) ductility. FIGS. 22 a and 22 b plot the strengths of the five alloys at three different soak/quenching temperature pairs (790° C./770° C., 810° C./790° C., and 830° C./810° C.) and at coiling temperatures of 580° C. and 660° C., respectively. FIGS. 22 c and 22 d plot the ductilities of the five alloys at the three different soak/quenching temperature pairs and at coiling temperatures of 580° C. and 660° C., respectively. The steels processed at a soak temperature of 790° C. and a quench temperature of 770° C. demonstrated the lowest strength, which can be attributed to the incomplete austenitization at 790° C. soaking temperature. FIGS. 24 a - 24 d are micrographs of four of the five alloys which were coiled at 660° C., cold rolled and annealed using the soak/quenching temperature pair 790° C./770° C. As can be seen, ferrite formed after the annealing cycle for all four of the steel compositions. Similarly, FIGS. 24 e - 24 h are micrographs of four of the five alloys which were annealed using the soak/quenching temperature pair 810° C./790° C. Ferrite formation can still be observed for the steels with 0.28% C and 0.32% C. The increase in C content resulted in an increase in hardenability so that less ferrite is formed at the same annealing cycle. Finally, FIGS. 24 i - 24 l are micrographs of four of the five alloys which were annealed using the soak/quenching temperature pair 830° C./810° C. Most of the steels show the highest strength after annealing at these temperatures, which may be due to the almost fully martensitic microstructure obtained.
[0000] Bendability of the Steels after Anneal Simulation
[0096] Table 11 summarizes the effects of C and B on the tensile properties and bendability of the steels after 50% cold rolling and annealing after simulated coiling at 580° C. The annealing process consisted of reheating the cold band (about 1.0 mm thick) to 850° C. for 100 seconds, immediate cooling to 810° C., 40 seconds isothermal hold at “quench” temperature, followed by water quench. The steels were then reheated to 200° C. for 100 seconds, followed by air cooling to simulate overaging treatment (OA). As shown in Table 11, it was possible to produce steels with ultimate tensile strength between 1830 and 2080 MPa by varying alloy composition.
[0000] TABLE 11 T Soak T Quench T OA Gauge YS UTS Bendability ID Steel ° C. ° C. ° C. mm YPE % MPa MPa YS/UTS UE % TE % pass 1 28C 850 810 200 0.93 0 1593 1908 0.83 3.5 4 3.5t 2 28C—B 850 810 200 1.06 0 1540 1838 0.84 3.2 3.2 3.75t 3 32C 850 810 200 0.99 0 1644 2005 0.82 4.1 4.5 4.0t 4 32C—2B 850 810 200 0.99 0 1569 1922 0.82 4 4.9 3.5t 5 36C 850 810 200 0.97 0 1688 2080 0.81 3.5 3.5 4.0t
Comparison with Examples 1 and 2—Effect of Manganese for the Steels with 0.28% C
[0097] The steels with 0.28% C and 1.0%/2.0% Mn were presented above in Examples 1 and 2. We now compare those steels with the steel containing 0.28% C and 0.5% Mn to investigate the effect of Mn (0.5% to 2.0%) on tensile properties. The detailed chemical compositions of the steels are shown in Table 12.
[0000]
TABLE 12
No.
ID
C
Mn
Si
Ti
B
Al
N
S
P
Ceq
1
28C—0.5Mn—Ti
0.282
0.577
0.199
0.021
0.02
0.004
0.005
0.004
0.38
2
28C—0.5Mn—Ti—B
0.281
0.58
0.197
0.022
0.0016
0.022
0.0042
0.004
0.004
0.38
3
28C—1.0Mn—Ti
0.28
0.98
0.198
0.024
0.04
0.0047
0.003
0.005
0.44
4
28C—1.0Mn—Ti—B
0.29
0.98
0.204
0.024
0.0018
0.04
0.0047
0.003
0.005
0.45
5
28C—1.0Mn
0.29
0.98
0.204
0.035
0.0049
0.003
0.007
0.45
6
28C—2.0Mn
0.28
2.01
0.201
0.034
0.005
0.003
0.006
0.62
[0098] Table 13 displays the tensile properties of the steels with 0.5% to 2.0% Mn and the additions of Ti and B after hot rolling and simulated coiling at 580° C. For the steels with Ti addition, the increase in Mn content from 0.5% to 1.0% led to an increase in both yield and tensile strengths and yield ratio but no significant effect on ductility. The addition of B in Ti added steels with 0.5% to 1.0% Mn resulted in an increase in strength. Compared to the steel “28C-1.0Mn”, the addition of Ti was beneficial for increasing both strength and yield ratio, which may be attributed to the effect of Ti precipitation hardening. The steels with the lower Mn content showed a lower strength than the steel with the higher Mn content. This may facilitate a higher extent of cold rolling for the low Mn steel.
[0000]
TABLE 13
Gauge,
YS,
UTS,
Steel
mm
YPE, %
MPa
MPa
YS/UTS
UE, %
TE, %
28C—0.5Mn—Ti
3.89
2.15
374
529
0.71
16.4
29.3
28C—0.5Mn—Ti—B
3.77
1.7
390
567
0.69
15.3
32
28C—1.0Mn—Ti
3.49
3.86
448
612
0.73
15.5
29.6
28C—1.0Mn—Ti—B
3.61
3.93
491
655
0.75
13.7
27.5
28C—1.0Mn
3.44
1.68
375
571
0.66
17.6
32.2
28C—2.0Mn
3.64
1.82
426
632
0.67
11.3
15.8
[0099] FIGS. 25 a - 25 d show the tensile properties of the steels with 0.5% to 2.0% Mn after coiling at 580° C., cold rolling (50% cold rolling reduction for the steel with 0.5 and 1.0% Mn and 75% cold rolling reduction for the steel with 2.0% Mn) and various annealing cycles. The X-axis of FIGS. 25 a - 25 d indicates soak and quench temperature, i.e., 870/840 means soaking at 870° C. and quenching at 840° C. It can be seen that at the same annealing treatment of 850° C.-810° C. (soaking-quenching temperature) and 200° C. (overaging), the increase in Mn content from 0.5% to 1.0% had no significant effect on strength for the steel with Ti, but resulted in an increase in strength for the steel with both Ti and B additions and an increase in ductility. The further increase in Mn content to 2.0% led to a pronounced increase in UTS of over 100 MPa, YS of over 50 MPa and a decrease in ductility. This effect was not applicable for high soaking temperature of 870° C., at which the steels with 2.0% Mn did not show an increase in strength. This indicates that the steel with 2.0% Mn is more sensitive to the soaking temperature, which may be due to grain coarsening at higher anneal temperatures. At the soaking temperature of 870° C., the increase in Mn from 0.5% to 1.0% resulted in increases in both strength and ductility for 810° C. and 780° C. quenching temperatures. The steel with 0.5 to 1.0% Mn will be relatively easier to process during manufacturing due to the wider process windows.
[0000] Bendability of Annealed Steels with 0.5 to 2.0% Mn (0.28% C)
[0100] Table 14 lists the tensile properties and bendability of the steels with 0.5% to 2.0% Mn after anneal simulation, which were previously coiled at 580° C. The steel “28C-0.5Mn—Ti” demonstrated a better bendability than the steel “28C-1.0Mn—Ti” (3.5t compared to 4.0t) at a comparable UTS level of 1900 MPa.
[0000]
TABLE 14
T Soak
T Quench
T OA
Gauge
YS
UTS
Bendability
Steel
° C.
° C.
° C.
mm
YPE %
MPa
MPa
YS/UTS
UE %
TE %
pass
28C—0.5Mn—Ti
850
810
200
0.93
0
1593
1908
0.83
3.5
4
3.5t
28C—0.5Mn—Ti—B
850
810
200
1.06
0
1540
1838
0.84
3.2
3.2
3.75t
28C—1.0Mn—Ti
850
810
200
0.99
0
1597
1901
0.84
4
4.8
>4.0t
28C—1.0Mn—Ti—B
850
810
200
1
0
1578
1886
0.84
3.5
4.9
3.75t
28C—1.0Mn
850
810
200
1.03
0
1599
1896
0.84
4.3
5.7
3.5t
28C—2.0Mn
0.68
870
810
200
0
1581
1927
0.82
4.3
4.3
4.0t
[0101] It is to be understood that the disclosure set forth herein is presented in the form of detailed embodiments described for the purpose of making a full and complete disclosure of the present invention, and that such details are not to be interpreted as limiting the true scope of this invention as set forth and defined in the appended claims.
|
Martensitic steel compositions and methods of production thereof. More specifically, the martensitic steels have tensile strengths ranging from 1700 to 2200 MPa. Most specifically, the invention relates to thin gage (thickness of ≦1 mm) ultra high strength steel with an ultimate tensile strength of 1700-2200 MPa and methods of production thereof.
| 2
|
INTRODUCTION AND BACKGROUND
The present invention relates to a system for forming the shed in a seam weaving portion for joining the ends of a fabric and to a method of forming a woven seam using the system.
As known in the art, the ends of a fabric are joined together to form an endless fabric or the peripheral edge of a fabric is joined to that of another fabric to form a larger piece of fabric. In most of the conventional methods, the ends of the fabric or the peripheral edges are overlapped with each other and then sewn together or bonded together.
However, the above-mentioned conventional method of joining together fabric can not be employed for papermaking fabrics, such as a sheet forming fabric. This is because such papermaking fabrics require a uniform structure and a uniform filtration space. Otherwise, the resultant paper product formed on the fabric is nonuniform in thickness and causes undesirable marking to occur.
In addition, fabrics for use in the manufacture of nonwoven fabrics must have a uniform structure in view of touch, laminatability and uniformity.
Further, the above-mentioned conventional method can not be used for fabrics which are for covering the sludge in a pressure dewatering process. This is because leakage of the sludge occurs due to the presence of the nonuniform filtering area in adjoining ends of a fabric which face each other. A method of alleviating this problem includes removing transversal or weft threads in one of the joining ends over a seam width to leave longitudinal or warp threads alone, introducing the warp threads into a fabric structure of the other joining end, and cutting and removing parallel warp threads of the other joining end. However, this method is not practically available unless the fabric is a coarse mesh.
In this connection, it has been considered to join the ends of a fabric by weaving, in adjoining portions, a fabric which is similar in structure to the main body of the fabric.
According to this prior method, threads which serve as warp threads corresponding to weft threads of the main body of the fabric are separated vertically upwardly to form the shed in a seam weaving portion. On the other hand, threads in both ends of the fabric to be joined are introduced into the shed as weft threads. Thus, a woven seam is formed. However, in order to effectively and mechanically perform the shed formation for weaving, there exists no other means superior to the known Jacquard device.
However, the Jacquard device generally requires longitudinal needles, transverse needles, knives, pattern cards, cylinders for receiving the pattern cards and inevitably has a large size. It is therefore inappropriate to use the Jacquard device in forming a woven seam which is narrow.
In sheet forming fabric, a wide variety of fabric structures are used and multi-layer fabrics have recently been put into use. In this connection, the number of heddles inevitably increases. This results in a further increase the size of the shedding system. Thus, such a conventional shedding system is not satisfactory for use in a seam weaving operation.
In addition, the Jacquard device has heddles each of which is supported at both upper and lower ends thereof and moved for the shed formation. With this structure, it is impossible to separately pick up an individual one of the heddles. When a large number of the heddles are arranged in a seam weaving portion which is narrow, it is difficult to thread the heddles surrounded by a mass of heddle supporting members standing together closely. If a thread is snapped during the seam weaving operation, it is extremely difficult to find the particular heddle in question and to thread the particular heddle for recovery.
In particular, the Jacquard device encounters difficulty in treating multi-layer fabrics, such as double-layer fabrics and triple-layer fabrics, which have recently been put into use.
As is known in the art the term "shed" means the path through and perpendicular to the warp in a loom. The shed is formed by raising some warp threads by means of their harness while others are left down. The shuttle press through the shed to insert the filling. The term "shedding" means the operation of forming a shed in the weaving process. Also as is known in the textile art, the heddle is a cord, round steel wire, or thin flat steel strip, or equivalent with a loop or eye near the center through which one or more warp threads pass on the loom so that their movement may be controlled in weaving. The heddles conventionally are held at both ends by the harness frame. They control the weave pattern and shed as the harnesses are raised and lowered during weaving.
As a result of a study to overcome the above-mentioned disadvantages, it was determined that a shedding system must be modified in order to improve the seam weaving speed and to form a woven seam of a wide variety of fabric structures.
SUMMARY OF THE INVENTION
According to this invention, it is an object to provide a shedding system with heddles supported at one end thereof, comprising a plurality of heddles supported at one ends individually coupled to top end and of piston rods of a plurality of pneumatic cylinders. The device of the invention also includes a control unit for producing a signal to operate the electromagnetic valves, the heddles being moved vertically upwardly and downwardly by stroke movement of the pneumatic cylinders to thereby form the shed in an array of threads individually passing through eyes of the heddles.
In a more detailed aspect, the shedding system of the invention also includes a cooling fan for cooling the electromagnetic valves and a control unit having a memory for memorizing a fabric structure.
Each of the heddles used in the present invention is a solid body formed of metal or plastics.
The heddles can be molded into a shape having an arcuate section or an undulating section. Any suitable metal or plastic having the properties necessary to perform this function can be used to make the heddle.
Another object of the invention is to provide a method of joining the ends of a fabric by a woven seam to form an endless fabric. In carrying out this method an interweaving piece is prepared which is made of the same kind of fabric as the fabric to be joined and which has a width corresponding to that of the woven seam and a length longer than the transverse width of the fabric to be joined. The interweaving piece has one longitudinal end area with a fabric structure left therein and a remaining area containing weft threads alone and with the warp threads removed therefrom. The weft threads are removed in both end zones of the fabric over a width substantially equal to that of the woven seam to form interweaving portions comprising warp threads alone. The interweaving portions are then held on a weaving table so that the interweaving portions face each other at a distance equal to the width of the woven seam so as to define a space therebetween. The interweaving piece is placed in the space so that the fabric structure left at the one longitudinal end area is positioned at one transverse ends of the interweaving portions. The weft threads of the interweaving piece are passed through eyes of a plurality of heddles, the heddles being supported at one end individually coupled to top ends of piston rods of a plurality of pneumatic cylinders. Weights are attached to other ends of the weft threads of the interweaving piece to apply tensile force to the weft threads.
Electromagnetic valves connected to the pneumatic cylinders are operated by a signal from a control unit, to move the heddles vertically upwardly and downwardly by stroke movement of the pneumatic cylinders to thereby form the shed in an array of the weft threads passing through the eyes of the heddles. The warp threads of the interweaving portions are introduced into the shed to thereby form the woven seam in accordance with the invention.
In another embodiment of the invention, the method of joining the ends of a fabric by a woven seam to form an endless fabric is the same as described above except that the warp threads, instead of the weft threads, of the interweaving piece are passed through eyes of the plurality of heddles. In all other respects, this second embodiment is the same as the first method described above.
According to a more detailed aspect of the invention, and in both method embodiments described above the threads of the interweaving portions to be introduced into the shed have a crimp similar to that of the original threads which are introduced into the shed when the fabric to be joined is initially woven.
Still further, the woven seam can be made to have a fabric structure similar to that of the other portion of the fabric by the use of a memory which is included in the control unit of the shedding system and which is for memorizing the fabric structure.
In yet another aspect of the invention, weighted strings are connected to the weft threads of the interweaving piece passing through the eyes of the heddles to apply tensile force to the weft threads during the weaving operation of the fabric structure.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be further understood with reference to the drawings, wherein
FIG. 1 is a perspective view of a shedding system of the invention;
FIG. 2 is a schematic view of a pneumatic cylinder connected to the heddle;
FIG. 3 is a schematic plan view of an interweaving piece;
FIG. 4 is a partial perspective view of the weaving apparatus of the invention illustrating the interweaving piece held on a weaving table;
FIG. 5 is a partial perspective view of the weaving apparatus of the invention showing how the seam weaving method is carried out; and
FIG. 6 is a plan view showing the top ends of warp threads interwoven according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
This invention is characterized in that the heddles are supported at one end thereof and are independent from one another. With this structure, it is possible to separately pick up a desired single one of the heddles among a mass of the heddles.
Accordingly, even if a large number of the heddles are arranged in a narrow limited area, the threading operation is not impeded by other heddles at all. In the case when a thread is snapped in operation of the weaving operation, recovery is readily performed because the particular heddle in question can be easily selected from the mass of heddles in the apparatus. Specifically, the heddles are swingable because they are supported at only one end thereof. Therefore, the mass of the heddles can be manually pushed aside to select the particular heddle in question for recovery. Alternatively, the particular heddle in question can be automatically protruded vertically upwardly or downwardly.
FIG. 1 is a perspective view of a shedding system according to this invention. Each heddle 1 has an eye 5 and is connected to a piston rod 8 of each pneumatic cylinder 2, and the heddles 1 are positioned in the vicinity of an end of a case 7. However, the pneumatic cylinders 2 may be positioned at a center of the case. The case 7 may be a box or a frame.
The control unit 16 consists of a computer and a memory. The memory stores the data of fabric pattern or structure of the area to be shedded. The computer reads the prescribed data stored in the memory and produces the signals each of which designates each of magnetic valves 3 being opened or closed. The control unit 16 may be positioned inside or outside the case 7. Such a control unit is well known in the art, and any suitable control unit can be used for the purposes of the present invention.
The electromagnetic valves 3 are individually connected to the pneumatic cylinders and drive the pneumatic cylinders in response to a signal from the conventional control unit 16.
Cooling fans 4 are for removing heat generated by operation of the pneumatic cylinders. The cooling fans may be arranged at a side surface.
A mobile guide 6 is attached to the case. The case is mounted through the guide on a guide rail of a weaving table to be movable along the weaving table.
FIG. 2 shows the pneumatic cylinder connected to the heddle. The heddle is coupled to a piston rod 8 of the pneumatic cylinder.
FIG. 3 shows an interweaving piece 9. The interweaving piece has at one end thereof a fabric structure comprising weft threads 10 and warp threads 11. In a remaining portion of the interweaving piece all warp threads are removed to leave the weft threads 10 with a crimp. The interweaving piece has a width corresponding to that of a woven seam and a length longer than the transverse width of the fabric to be joined.
FIG. 4 shows the interweaving piece held on a weaving table 13. The fabric structure remaining in the interweaving piece is fixed to the weaving table. The weft threads with a crimp are extended through the eyes of the heddles and subjected to tensile force by weights 12 connected to one ends of the weft threads. The case 7 is mounted on the mobile guide rail of the weaving table.
FIG. 5 is a view illustrating the seam weaving method according to this invention. In a seam weaving portion, end portions 14 of the fabric to be joined are arranged to face each other on the weaving table 13. The interweaving piece comprising the weft threads is placed between the end portions. The case 7 is mounted on the guide rail of the weaving table. The weft threads of the interweaving piece are made to pass through the eyes of the heddles.
The weft threads are removed from the end portions of the fabric to be joined over the width equal to that of the woven seam to leave the warp threads with a crimp.
When the heddles are moved by the pneumatic cylinders, the weft threads passing through the heddles are shifted to form the shed, like the warp threads in an ordinary weaving process. Like ordinary weft threads, the warp threads of the end portions of the fabric are successively introduced into the shed to form a fabric structure. At this time, the movement of the heddles is controlled so as to form the fabric structure similar to that of the main body of the fabric.
As is clear from a woven seam illustrated at the leftmost portion in FIG. 5, the weft threads 10 of the interweaving piece serve as the warp threads in the seam weaving operation while the warp threads 15 of the end portions of the fabric serve as the weft threads.
FIG. 6 shows the top ends of the warp threads which are interwoven. The top ends of the warp threads face each other with the weft threads interposed therebetween. The facing positions are dispersed to form no linear alignment. With this structure, any problems of marking are prevented.
Thus, a fabric structure completely similar to that of the main body of the fabric is formed.
In the conventional Jacquard device, the heddles are supported at both upper and lower ends thereof. Accordingly, the heddles can not be manually pushed aside. On the other hand, it is possible to make a particular heddle be upwardly protruded among a mass of the heddles. However, the particular heddle is not swingable because it is supported at both upper and lower ends. Furthermore, the supporting members of the other heddles closely stand and surround the particular heddle. As a result, threading or recovery operation is extremely difficult. Thus, in the Jacquard device, it is impossible to arrange a concentrated mass of the individual heddles in a narrow area.
The following describes the seam weaving method according to this invention.
At both ends of a fabric to be joined the weft threads are removed from end zones over a predetermined width to prepare interweaving portions exclusively comprising warp threads with a crimp. The interweaving portions with the warp threads alone are folded back and placed on a weaving table to face each other with a predetermined distance left therebetween.
An interweaving piece is made of the same kind of fabric as the fabric to be joined and has a width corresponding to that of a woven seam and a length longer than the transverse width of the fabric to be joined. The interweaving piece has a fabric structure at one end thereof with warp threads retained therein while a remaining area of the interweaving piece contains only weft threads with a crimp with warp threads removed therefrom. The interweaving piece is fixedly located in a space defined between the interweaving portions facing each other so that the one end with the fabric structure is positioned at a seam weaving starting side and the weft threads are parallel to the weaving table. The weft threads of the interweaving piece are made to pass through the eyes of the heddles. The weft threads are subjected to tensile force which is produced by weights attached to one end of the weft threads.
The heddles are individually connected to pneumatic cylinders. The heddles are supported at one ends coupled to the top end and of piston rods of the pneumatic cylinders. Electromagnetic valves of the pneumatic cylinders are operated in response to a signal delivered from a control unit to move the heddles vertically upwardly and downwardly. Consequently, the weft threads of the interweaving piece passing through the heddles are shifted vertically upwardly and downwardly to form the shed. The warp threads of both end portions of the fabric to be joined are introduced into the shed. Thus, seam weaving operation is carried out to integrally join the both end portions by forming a fabric. As described, a woven seam has a structure similar to the other portion of the fabric.
In this seam weaving operation, the weft threads of the interweaving piece are shifted by heddles to form the shed while the warp threads of the main body of the fabric are introduced into the shed. In comparison, when the original fabric is woven, the warp threads are shifted by heddles to form the shed while the weft threads are introduced into the shed.
In the foregoing description, the interweaving piece is prepared by removing the warp thread to leave the weft threads alone. Alternatively, seam weaving operation can also be carried out with the interweaving piece prepared by removing the warp threads to leave the weft threads alone. In this case, the warp threads are removed from the both ends of the fabric to be joined over the width corresponding to that of the woven seam to form the interweaving portion comprising the weft threads alone.
Use may also be made of a combination of an interweaving piece prepared by the weft threads alone and interweaving portions formed by the warp threads alone.
Since the fabric is formed by warp threads and weft threads, the seam weaving operation can be carried out whichever thread is introduced into the shed.
The pneumatic cylinders to be used have a diameter between 2.5 mm-5 mm.
The pneumatic cylinders are driven by electromagnetic valves which are operated in response to a signal from a control unit having a memory for memorizing a structure of a woven seam.
Since heat is generated during the operation of the pneumatic cylinder, it is preferable to provide a cooling device such as a fan.
EXAMPLE 1
The system in FIG. 1 according to this invention was used to join the fabric consisting of single warp threads and double weft threads as shown in Table 1. A woven seam was formed at a rate of 150 mm per hour.
As compared with a conventional manual seam weaving in which a woven seam was formed at a rate of 60 mm per hour, the efficiency is almost three time high.
TABLE 1______________________________________Warp Thread Diameter (mm) 0.62 Number (per inch) 45Upper Weft Thread Diameter (mm) 0.58 Number (per inch) 16Lower Weft Thread Diameter (mm) 0.58 Number (per inch) 16______________________________________
In the shedding system according to this invention, the heddles are connected in a one-to-one correspondence to the pneumatic cylinders and are moved thereby. Since the pneumatic cylinders are very small, a large number of the pneumatic cylinders can be arranged in a seam weaving portion which is narrow. The pneumatic cylinders are driven by electromagnetic valves to cause stroke movement. Accordingly, the shedding system is very compact and can be arranged in the upper or the lower portion of the seam weaving portion.
According to this invention, the heddles are supported at one end thereof so that shedding system for seam weaving operation is small-sized and recovery of a thread snapping accident is facilitated. It is possible to readily and accurately form a woven seam having a desired structure.
Further variations and modifications of the invention will be apparent to those skilled in the art from the foregoing and are intended to be encompassed by the claims appended hereto.
|
A shedding device and a method for joining the ends of a fabric into an endless belt of fabric, or, alternatively, joining the ends of separate pieces of fabric into a single piece of fabric. The shedding device employs a plurality of heddles supported at only one end, allowing the heddles to be individually moved or adjusted. The heddles are connected to the top ends of piston rods of a plurality of pneumatic cylinders. The heddles move up and down to shift threads passing through the heddles, so as to form a shed. The shedding method employs an interweaving piece of fabric, with a portion of the interweaving piece having only weft threads. The weft thread of the interweaving piece interwoven with the warp threads of the ends of the fabric to be joined. Alternatively, the weft threads of the interweaving piece can be interwoven with the weft threads of the ends of the fabric to be joined.
| 3
|
RIGHTS TO INVENTIONS UNDER FEDERAL RESEARCH
There was no federally sponsored research and development concerning this invention.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to land vehicles and more particularly to toolboxes combined with and below the running boards thereof. Those having ordinary skill in this art are the owners of land vehicles.
(2) Description of the Related Art
The personal land vehicles may be characterized as automobiles, pickups, and recreational vehicles. Although automobiles at the present time do not have exterior running boards, pickups and recreational vehicles often have exterior running boards.
Also in America pickups and recreational vehicles are an increasing percentage of the personal vehicles used. There is some indication that they are the major portion of the vehicles sold.
Some pickups and recreational vehicles do not have running boards. Usually running boards are desirable because of the height of the floor board above the road way upon which the vehicles runs.
Although not all of the pickups and recreational vehicles are owned by craftsmen or sportspersons a substantial number are. Normally, people who own pickups or recreational vehicles desire to carry either tools of their craft or equipment for recreation with them.
Therefore, there is a need on this type vehicle for toolboxes. It will be understood that recreation equipment could be stored in the toolboxes as well as the tools of a craft for craftsmen.
Toolboxes under the running boards was a popular consideration over 50 years ago in the early days of the automobile development.
Before this application was filed, a search was made in the U.S. Patent and Trademark Office. Of the 14 patents reported by that search it will be noted that all but one were issued before 1934. The one that was not before 1934 was for a recreational vehicle. (It will be noted that all personal motor vehicles not classified as automobiles or pickups are classified here as recreational vehicles.)
The patents found in the search are listed below.
______________________________________HATFIELD 1,196,453VON SCHRENK 1,310,973HOLLIS 1,422,763LOVELAND 1,453,362KERMODE 1,456,780TICHY ET AL 1,488,720KELLY 1,530,834SMITH 1,628,072LIMBOCKER 1,726,398MOORE 1,784,971REINGOLD 1,850,032MILLER 1,864,607STASSINOS 1,934,567GORE 3,764,048______________________________________
These patents are considered pertinent because the applicant believes the Examiner would consider anything revealed by the search to be relevant and pertinent to the examination of this application.
SUMMARY OF THE INVENTION
(1) Progressive Contribution to the Art
I have invented a combination running board and toolbox which is waterproof, dustproof, and sturdy. Also, and more important, it is easily accessible and attractive, correlating with the pleasing contours normally found upon pickups and recreational vehicles. It is particularly designed for ease in manufacturing being primarily composed of broken or bent sheet metal material. It is also designed to be attached primarily to the wheel wells of the vehicle and extend from the front wheel well to the back wheel well beneath the doors of the vehicle.
(2) Objects of this Invention
An object of this invention is to provide a combination running board and toolbox for wheeled vehicles.
Further objects are to achieve the above with a device that is sturdy, compact, durable, lightweight, simple, safe, efficient, versatile, ecologically compatible, energy conserving, and reliable, yet inexpensive and easy to manufacture, install, and maintain.
The specific nature of the invention, as well as other objects, uses, and advantages thereof, will clearly appear from the following description and from the accompanying drawing, the different views of which are not scale drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side perspective view of the vehicle with the toolbox according to this invention attached thereto.
FIG. 2 is a perspective view from the front and side showing the toolbox and the attachment to the wheel well.
FIG. 3 is a cross sectional view of the box taken substantially along line 3--3 of FIG. 1.
FIG. 4 is a detail view of the lock, bolt, and holder.
FIG. 5 is a sectional view through one end showing the end and the attachment means, taken on line 5--5 of FIG. 3.
FIG. 6 is a detail view of the back catch, shield, and chain flange.
As an aid to correlating the terms describing this invention to the exemplary drawing, the following catalog of elements is provided:
10 vehicle
12 wheels
14 cab
16 bed
18 cab well
20 bed well
22 door
24 front sheet
26 rear sheet
28 top
30 box
32 back
34 bottom
36 side
38 front end
40 rear end
42 end spacers
44 end lips
46 side lip
48 back lip
50 back hip
52 chain flange
54 back shield
56 bolts
58 shield spacers
60 shield flange
62 back catch
64 side face
66 top lip
68 weather stripping
70 holder
72 lock
74 front face
76 rear face
78 lock bolt
80 chains
82 holder slope
84 tread
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings and more particular to FIG. 1 there may be seen a vehicle 10 in the form of a pickup.
The vehicle will have ground engaging wheels 12. The vehicle will have a body which includes two separate parts. First the cab 14 is mounted to the frame (not shown) in the front and the bed 16 is mounted to the frame to the rear. Inasmuch as the frames of the vehicles are not rigid but have a certain amount of flexibility there is a gap between the cab and the bed to permit a certain amount of flexing. Cab wheel well 18 is mounted on the cab and extends over the front wheel 12. Bed wheel well 20 is part of the body at the bed which extends over the rear wheel 12. As customary the vehicle will have door 22 between the wheel wells.
A toolbox attachment means includes a front splash guard or attachment sheet 24. The attachment sheet is flexible or pliable so that it when applied will conform to the contour of the rear of the cab well 18 as shown. Likewise, the rear of the toolbox is attached by a rear splash guard or attachment sheet 26 which is also flexible to conform to the front of the bed wheel well 20.
In some instances the rear splash guard or attachment sheet 26 will be connected to the cab 14 instead of the bed wheel well. In such cases the box 30 will be short and extend only from the cab well 18 to the rear of the cab.
It will be understood that on different vehicles and makes and brands of vehicle that the contour of the wheel wells will be different. However, I have found that if toolbox 30 is assembled with the sheets 24 and 26 thereon that there is no difficulty in the flexible or pliable sheets 24 and 26 conforming to the contour of the wells wherein they are attached.
Top plate or top 28 of the box 30 is immediately below where the bottom of the wheel well joins the body of the vehicle 10. The top 28 is level from front to back. I prefer to mount the top 28 slightly higher than running boards are normally mounted so that if the box is about 41/2 inches deep that it does not project extremely close to the ground. A box which projects about 41/2 inches beneath the top 28 will be only about a 1/2 inch lower than the muffler and exhaust pipes of the vehicle.
The box 30 includes, in addition to the top 28, back panel or back 32 bottom panel or bottom 34, and side panel or side 36. The back 32 and side 36 are normal or 90° to the bottom 34. The back, bottom, and side are formed from a single sheet of metal by braking or bending. The top 28 is a separate piece of metal as are the front end panel or end 38 and rear panel or end 40. The front end and back end are attached to the ends of the back, bottom, and side as by welding.
The attachment sheets 24 and 26 form a means for attaching the box to the wheel wells of the vehicle. The attachment sheets 24 and 26 are conveniently attached to the ends 38 and 40 by bolts and are spaced there from them by one or more end spacers 42.
The top edge of the ends 38 and 40 are bent inward to form end lips 44. The end lips are parallel to the bottom 34. The end lips will be next to the top 28. Side lip 46 is formed by bending the top edge of the side 36 outward. It also will be parallel to the bottom 34 and next to the top 28. Back lip 48 will be made by a brake from a top part of back hip 50 which is made by a brake at the upper edge of the back 32. The back hip 50 will be at a 45° angle to the back 32 and to the back lip 48. The back lip 48 will be next to the top 28 and parallel to the bottom 34.
Chain flange or guide 52 will be formed by a bend at the back lip 48 and will bend downward or into the box 30 by a 45° angle. Back shield 54 is attached to the hip 50 and is parallel thereto. The back shield 54 is conveniently attached by a plurality of bolts 56 and spaced from the hip 50 by washers or shield spacers 58. Shield flange 60 is bent upward from the back shield 54 and is at right angles or normal to the bottom 34.
Back catch 62 on the top 28 is between the shield 54 and the hip 50 and is parallel to each of them. Since it is parallel to the hip, it would be at a 45° angle to the top 28 which is parallel to the bottom 34. Side face 64 on the top 28 extends downward parallel to the side 36. Top lip 66 is bent on the face 64 and extends inward parallel to the bottom 34.
Compressible material in the form of weather stripping 68 is adhered to the underside of the top 28 along the end lips 44, the back lip 48, and the side lip 46. Holder 70 is attached as by welding to the underside of the top 28. It is spaced from the side face 64 distance slightly more than the width of the side lip 46. Therefore with the top 28 in place vertical face of holder 70 (the face parallel to the side 36), will fit against the side 36 and prohibit the top 28 from moving outward or away from the back 32. Gravity as well as lock 72 (to be explained later) prevent the side edge of the top 28 from moving upward. The back catch 62 prevents the back of the top 28 from moving upward.
Front face 74 on the top 28 extends between the front sheet 24 and the front end 38. Rear face 76 upon the top, extends between the rear sheet 26 and the rear end 40. With the top down the top is securely in place. The lock 72 has lock bolt 78 which may bear against the underside of the side lip 46. With the lock bolt 72 bearing against the underside of lip 46, the top 28 cannot be moved upward because of the lock bolt. It cannot be moved outward because of the holder 70. It cannot be moved forward or backward because of faces 74 and 76. Therefore, until the lock 72 is opened by a key (or combination) the contents of the box are secure from theft.
To open the box 30 the bolt 78 is lowered by the key in the lock 72 and the outside edge of the top 28 is moved upward until the lock body 72 contacts the underside of the side lip 46. At this point the holder 70 will be above or clear of the side lip 46. In this position the top 28 can be slid away from the back until the back catch 62 is clear of the back shield 54. At this time, the top is free of the box except for cables or chains 80 which extend from the underside of the top to the chain flange 52. I prefer that the chains be of such a length that they extend from their attachment on the chain flange 52 to the outside edge of the side lip 46. Therefore, they are so arranged so that they will hold the top is a position that gives full access to the box 30 but the top 28 is still in a convenient position. The cables or chains 80 form flexible retainers.
To replace and reconnect the top 28 it is moved into place loosely on the top of the box 30. Then it is slid backward and the back catch 62 will slide under the back shield 54. The top will be guided by chain flange or guide 52. The front side of holder 70 has holder slope 82 which will cause the holder 70 to ride over the side lip 46 so that the top closes naturally and normally.
Suitable tread 84 of antiskid material is applied to the upperside of the top 28 so that when the top of the box 30 is used as a running board it is not slippery. In this regard the top serves two functions. One, is a closure to the toolbox 30 and also as the running board or step to step into the cab of the truck or recreational vehicle.
It will be noted that normally the box 30 is attached to the body of a vehicle by the attachment sheets 24 and 26. In addition to this the shield flange 60 may be bolted to the body of the vehicle below the door 22 of the vehicle.
As mentioned above, there will normally be a certain amount of flexing between the cab 14 and the bed 16. Therefore, it is preferred that the shield flange 60 be bolted to the cab only and not the cab and the bed. However, in certain instances, I have successfully bolted the shield flange 60 to both the cab and the bed.
The shield 54 performs three functions. One it is the holder of the back catch 62 of the top 28. Also it, together with the flange 60, forms the structural member to attach the box to the cab 14 of the vehicle. Also the space between the shield and the hip provides a drainage channel for water to drain from the top.
The top lip 66 functions as a guard for the lock 72 to prevent tampering with the lock.
In this regard the back catch 62 of the top 28 forms at least two functions, that being that it holds the lid down as discussed above and also that it covers the opening in the box to make it waterproof. The space between the ends 38 and 40 and the attachment sheets 24 and 26 forms two functions. One, there is a clearance for the front face 74 and rear face 76 of the top 28 also acts as a water drain between the box and the sheet.
It is well known in the metal working arts particularly with sheet metal that all of the bends, breaks, and turns of the metal give the finished product more rigidity. This is particularly true of the chain flange 52 and the top lip 66 for example. However, the side lip 46 as well as the front end rear faces 74 and 76 also add rigidity to the parts.
The embodiment shown and described above is only exemplary. I do not claim to have invented all the parts, elements, or steps described. Various modifications can be made in the construction, material, arrangement, and operation, and still be within the scope of my invention.
The restrictive description and drawing of the specific examples above do not point out what an infringement of this patent would be, but are to enable one skilled in the art to make and use the invention. The limits of the invention and the bounds of the patent protection are measured by and defined in the following claims.
|
A running board toolbox combination is made for pickups and recreational vehicles. The top plate of the toolbox functions as a running board when closed. The toolbox is attached to the vehicle by a flexible sheet upon each end. Each sheet fits the contours of the wheel well to which it is attached. The top plate opens by sliding into a slot at the back of the box. When closed, the top plate is held in place by a lock bolt against the lip at front. Weather stripping between the top plate and the main body of the box keep the box weatherproof. Furthermore, faces depending from the top plate overlap all edges of the box to prevent water from running into the box. Drainage is provided for the water.
| 1
|
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is entitled to the benefit of and incorporates by reference essential subject matter disclosed in International Patent Application No. PCT/EP2005/011599 filed on Oct. 29, 2005.
FIELD OF THE INVENTION
[0002] The invention concerns a method for manufacturing a fluid line, in which several tubes are wound in parallel along a helical line, provided at least at one end with a connecting element and embedded in a plastic material. Further, the invention concerns a fluid line with several tubes wound in parallel along a helical line and having, at least at one end, a common connecting element, the tubes being embedded in a plastic material.
BACKGROUND OF THE INVENTION
[0003] Such a fluid line is known from WO 2004/046601 A1. For the flow of the fluid the sum of the cross-sections of all tubes is available. The helical line shape of the tubes provides the fluid line with a certain flexibility.
[0004] Such fluid lines are well suited for transporting fluids in technical applications under a high pressure and, if required, also under high temperatures, if such applications are exposed to heavy vibrations and aggressive environmental conditions. Application examples are mobile refrigeration systems, particularly air-conditioning systems in vehicles working with CO 2 . For mounting reasons, such applications require a certain flexibility of the line without weakening the line.
[0005] The manufacturing of such a fluid line, however, requires a certain effort. This is particularly the case for the step of embedding in the plastic material. Usually, for this purpose, the tubes must be stabilised from the inside to prevent them from getting damaged during embedding.
SUMMARY OF THE INVENTION
[0006] The invention is based on the task of simplifying the manufacturing.
[0007] With a method as mentioned in the introduction, this task is solved in that a liquid silicone rubber is used as plastic material.
[0008] Liquid silicone rubbers are plastic materials offering substantial advantages for this application in comparison with previously used silicone rubber or other polymer plastic materials, for example thermo-plastic materials, elastomers or thermo-plastic elastomers. Liquid silicone rubbers are highly elastic, highly temperature resistant two-component plastic materials, which do not cure until the two low-viscous components are brought together under heat absorption. No particular pre-treatment of the tube surfaces is required to ensure a sufficient adhesion of the cured liquid silicone rubber to the surfaces of the tubes. Also in connection with elongations of more than 100%, this adhesion is maintained. Liquid silicone rubbers are, for example, available under the names Dow Corning SILASTIC LSR, Wacker ELASTOSIL LR and GE-Bayer Silopren LSR.
[0009] Preferably, the liquid silicone rubber is applied to the tubes by means of an injection moulding process. With this method, the advantages of liquid silicone rubber are particularly obvious. The liquid silicone rubber, or rather the pre-mixed components of the liquid silicone rubber, can namely be inserted into an injection mould under a relatively low pressure. Usually, relatively low injection pressures of maximum 50 bar will be sufficient. For traditional plastic materials, pressures of several 100 bar were often required, so that the tubes had to be stabilised from the inside.
[0010] Preferably, the tubes are inserted in an injection mould, and subsequently a component mix of the liquid silicone rubber is inserted into the injection mould through a cooled inlet passage. With this method, it is prevented that the viscosity of the mixed components increases in the inlet passage, thus causing clogging. Further, the finished tube can usually be removed from the injection mould without bosses.
[0011] Preferably, the tubes are heated before insertion into the injection mould. Liquid silicone rubber cures under heat absorption. When sufficient heat is supplied, the curing can be accelerated. With a sufficient heat supply, the curing takes place so fast that short fixed cycles in the manufacturing process in the range of a few seconds can be achieved. Heating of the tubes to a temperature in the range from 150 to 200° C. also causes that the adhesion of the liquid silicone rubber to the tubes is improved.
[0012] Alternatively or additionally, the injection mould can be heated. Also this causes an acceleration of the curing process.
[0013] With a fluid line as mentioned in the introduction, the task is solved in that the plastic material is a cured liquid silicone rubber.
[0014] As mentioned above, liquid silicone rubber is a highly elastic plastic material, which is also high-temperature resistant. It is a two-component plastic material, both components having in the separated state, and also for a certain period in the mixed state, a low viscosity, that is, they are highly flowable. Not until being brought together they cure under heat absorption and thus adhere to the tubes in an excellent manner.
[0015] Preferably, the cured liquid silicone rubber covers a connection arrangement between the tubes and the connecting element. Thus, also the joining spots at the connection between tubes and connecting element will be reliably protected against corrosion attacks.
[0016] Preferably, the tubes have a mutual distance, in which the cured liquid silicone rubber is located. In this way, the tubes are prevented from rubbing on each other during operation. This rubbing could cause damage to the tubes.
[0017] Preferably, the cured liquid silicone rubber surrounds a hollow inside an inner chamber surrounded by the tubes. This means that the tubes are covered on the radial inside and the radial outside by the liquid silicone rubber. At the same time, a hollow is located inside the line, in which no cured liquid silicone rubber is available. Apart from the advantage of saved weight, this embodiment has the advantage that other lines, for example electrical wires, can be guided through the hollow.
[0018] Preferably, the connecting element is located outside the longitudinal axis of the helical line. During manufacturing of the line, this permits the insertion of a core to create the hollow. In this case, the connecting element will not prevent the movement of the core during insertion and removal.
[0019] Preferably, the ends of the tubes extend tangentially from the helical line. In this case, they do not have to be bent at the end of the helical line, but are, in a manner of speaking, continuing straight forward.
[0020] In an alternative embodiment it may be provided that the ends of the tubes are bent in parallel to the longitudinal axis of the helical line. In this case, a connecting element can be used that does, in a manner of speaking, continue in a straight line from the fluid line.
[0021] Preferably, the connecting element has a basis plate with through openings, into which the ends of the tubes are inserted. This is a relatively simple way of connecting the tubes to the connecting element and at the same time ensuring that this connection is tight.
[0022] Preferably, the basis plate, together with a housing element, encloses a connection chamber, the housing element having an opening. Eventually, another line or a tube end can be connected to this opening, through which the fluid will be supplied or discharged. The basis plate and the housing element can be manufactured separately and then assembled. The basis plate and the housing element can also be manufactured in one piece.
[0023] Preferably, the ends of the tubes are connected to the basis plate via a soldered or welded connection. On the one side, a soldered or welded connection provides a sufficient mechanical stability. On the other side, this connection also provides a sufficient tightness.
[0024] Preferably, the end of the connecting element facing the tubes comprises a circumferential recess, into which the cured liquid silicone rubber extends. In a manner of speaking, this provides a form-fit connection between the liquid silicone rubber and the connecting element. The connections between the tubes and the connecting element are even better protected against corrosion.
[0025] Preferably, the connecting element has a projection that extends into a chamber circumscribed by the helical line. The projection can be made as an integrated part of the connecting element or as a separate component, which is, for example, fixed on the basis plate. With this embodiment, the end area of the tubes is relieved. After winding and connection to the connecting element, the largest stresses in the individual tubes appear on the one side at the transition from the winding structure into the axial tube ends due to the mechanical deformation, and on the other side at the soldering and welding spots in the basis plate due to thermal load. By means of the projection, these static “prestressed” areas of the tubes can be separated from the spots, which can be stressed during mounting or operation, for example in the form of dynamic load caused by vibrations. Thus, the projection reduces the risk of a line rupture.
[0026] It is preferred that the projection has a length, which at least corresponds to the diameter of the helical line. Or rather, the length corresponds at least to the inner diameter, which is left free by the helically guided tubes. With this length, the projection can provide a sufficient supporting function.
[0027] Preferably, the end of the projection is made to be conical. Thus, it tapers in the direction of its free end. This increases the radial distance between the projection and the tubes in the direction of the free end of the projection, so that a certain flexibility of the line also exists in the area of the projection without causing too large stress loads.
[0028] Preferably, a radial distance is provided between the projection and the tubes, the radial distance being filled with cured liquid silicone rubber. Also this improves the supporting function of the projection, though maintaining the flexibility of the line.
[0029] Alternatively or additionally, it may be provided that the connecting element has a circumferential flange extending in the direction of the tubes, the flange surrounding the helical line in an end area. Thus, the flange forms some sort of “cover” surrounding the end area of the fluid line. Also between this cover and the outsides of the tubes a radial distance can be provided, which is filled with liquid silicone rubber. Additionally, also an improved protection of the connection spots between the tubes and the connecting element against external influences occurs.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] In the following, the invention is described on the basis of preferred embodiments in connection with the drawings, showing:
[0031] FIG. 1 is a schematic view of a fluid line with radially aligned tubes,
[0032] FIG. 2 shows the fluid line according to FIG. 1 with a connecting element at each end,
[0033] FIG. 3 shows the fluid line according to FIG. 2 after embedding in liquid silicone rubber,
[0034] FIG. 4 shows a modified embodiment of a tube bundle with axially aligned tube ends,
[0035] FIG. 5 shows an axial section through the line according to FIG. 4 with connecting element and massive plastic material embedding,
[0036] FIG. 6 shows an embodiment modified in comparison to FIG. 5 , with a hollow inside the liquid silicone rubber,
[0037] FIG. 7 shows a modified embodiment of the line according to FIG. 5 ,
[0038] FIG. 8 shows a second modified embodiment of the line according to FIG. 5 ,
[0039] FIG. 9 shows a third modified embodiment of the line according to FIG. 5 ,
[0040] FIG. 10 shows a schematic view explaining the injection moulding plant, and
[0041] FIG. 11 shows different process steps of the fluid line manufacturing.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0042] FIG. 1 shows a tube spiral 1 of a fluid line 2 . The tube spiral 1 has several, in the present embodiment six, tubes 3 , each tube 3 being wound along a helical line. All tubes 3 extend in parallel, so that the lift height of the helical line corresponds to the sum of the diameters of the six tubes 3 .
[0043] The tubes 3 have ends 4 , 5 , which extend tangentially from the tube spiral 1 . In other words, the ends 4 , 5 of the tubes 3 are parallel to a first plane and vertical to a second plane, which extend through the axis of the tube spiral 1 . This results in a short component length of the tube spiral with ends 4 , 5 . Instead of an alignment of the tube ends 3 in the purely tangential direction, it is also possible to bend the tube ends 3 in another angle, for example parallel to the axis of the tube spiral, if this is advantageous for certain mounting conditions.
[0044] FIG. 2 shows the tube spiral 1 before insertion into an injection moulding tool. Connecting elements 6 , 7 are located at both tube ends 4 , 5 . These connecting elements 6 , 7 can be connected to the ends 4 , 5 of the tubes 3 in a suitable manner, for example by soldering, welding, gluing or another process.
[0045] The connecting elements 6 , 7 serve the purpose of connecting openings 8 of the tube ends 4 , 5 to a common fluid connection. For this purpose, the connecting element 6 has an opening 9 and the connecting element 7 has an opening 10 , which can subsequently be used to connect the fluid line 2 to other components.
[0046] Before insertion into the injection moulding tool, a core 11 is inserted into the tube spiral 1 , the core 11 being meant to keep a hollow inside the tube spiral 1 free during the injection moulding. In this connection, the all sides of the core 11 should have a uniform distance to the tube spiral 1 , so that all the tubes 3 of the tube spiral 1 can be completely covered with the plastic material.
[0047] FIG. 3 shows the fluid line 2 after the injection moulding process. The complete tube spiral 1 and also the tube ends 3 , 4 are surrounded by a coat 12 of cured liquid silicone rubber. The coat 12 has projections 13 , 14 , formed by moulding, which extend up to the connecting elements 6 , 7 .
[0048] Now, the core 11 is removed from the fluid line 2 , so that the fluid line 2 has a cylindrical hollow 15 .
[0049] Liquid silicone rubbers, which are suited for the coat 12 , could be Dow Corning SILASTIC LSR, Wacker ELASTOSIL LR and GE-Bayer Silopren LSR.
[0050] The use of liquid silicone rubber involves the advantage that the coat 12 is highly flexible and also high-temperature resistant. Liquid silicone rubber is a two-component plastic material. In this plastic material, the two low-viscous components do not cure until they are brought together under heat absorption. If, before inserting the tube spiral 1 in an injection mould, the tube spiral 1 and/or the injection mould is heated, the curing process in the injection mould will be so fast that short fixed cycles can be realised. The curing can be achieved within a few seconds.
[0051] The low-viscous components of liquid silicone rubber permit the supply to the injection mould of the mixture of the two components at a relatively low pressure of a few bar. Accordingly, the tubes 3 , which are preferably made of a metal, do not have to be supported from the inside. They can have relatively thin walls without risking to be deformed during the injection moulding.
[0052] As can be seen from FIG. 3 , not only the tubes 3 , but also the connecting elements 6 , 7 , which are fixed on the tubes 3 , are embedded in the plastic material. Thus, also the joining spots at the connection between the tubes 3 and the connecting elements 6 , 7 are reliably protected against corrosion attacks.
[0053] FIG. 4 shows a modified embodiment of a tube spiral 1 , in which the ends 3 have been bent in parallel with the axis of the tube spiral 1 . Also here, six tubes 3 are concerned. In the central area of the view according to FIG. 4 , the tubes are located above each other two by two, so that only four ends 4 of the tubes 3 can be seen.
[0054] The other end of the tube spiral 1 can be made in the same way as the end shown. However, it is also possible to make the other end of the tube spiral 1 as described in connection with, for example, FIG. 1 .
[0055] FIG. 5 shows a fluid line 2 with the tube spiral 1 of FIG. 4 in a section. The plastic material of the coat 12 is, in a manner of speaking, drawn to be transparent, so that the tubes 3 can be seen.
[0056] Between the tubes 3 distances 16 are made, which are also filled with the liquid silicone rubber of the coat 12 . Generally, in connection with shown finished lines, the liquid silicone rubber is always cured. The liquid silicone rubber prevents a rubbing of the tubes 3 on each other, when the fluid line 2 is exposed to vibrations. In the embodiment according to FIG. 5 a hollow 15 is not provided. On the contrary, the liquid silicone rubber does not only surround the tubes 3 in the form of a coat, it also fills the whole inside.
[0057] Compared to the FIGS. 2 and 3 , the fluid line 2 has a modified embodiment of a connecting element 17 . The connecting element 17 has a basis plate 18 , which surrounds a connecting chamber 20 together with a housing element 19 . The housing element 19 has an opening 21 in the direction of the connecting chamber 20 .
[0058] For each end 4 of the tubes 3 , the basis plate 18 has a through bore 22 . The end 4 is guided through the through bore 22 and connected to the basis plate 18 by means of a solder or weld seam 23 . The solder or weld seam 23 has two tasks. Firstly, it mechanically fixes the ends 4 of the tubes 3 to the basis plate 18 . Secondly, it seals the connecting chamber 20 in the direction of the tube spiral 1 .
[0059] As the connection between the ends 4 and the basis plate 18 is made before making the coat 12 of liquid silicone rubber, also the solder or weld seams 23 are covered by the coat 12 of liquid silicone rubber. Thus, external influences are prevented from corroding this solder or weld seam 23 .
[0060] FIG. 6 shows a modified embodiment of the fluid line 2 . Here, the same elements are provided with the same reference numbers. Also here, the liquid silicone rubber of the coat 12 is made to be “transparent”, so that the tubes 3 can be seen.
[0061] Contrary to embodiment of FIG. 5 , the hollow 15 is provided again, which was filled by the core 11 during the injection moulding process. However, it can be seen that both the radial inside and the radial outside of the tubes 3 are covered by the coat 12 of cured liquid silicone rubber. Also here, distances are provided between the tubes 3 , said distances being filled by the cured liquid silicone rubber.
[0062] The side of the housing element 19 facing the tubes 3 is provided with a circumferential recess 24 . This recess 24 is located in the area of the basis plate 18 . If, however, the housing element 19 extends over the basis plate 18 in the direction of the tubes 3 , the recess 24 can also be placed elsewhere. The coat 12 extends into the recess 24 . Thus, an even better sealing in the direction of the weld or solder seams 23 is achieved.
[0063] FIG. 7 shows an embodiment that is much like the embodiment according to FIG. 5 . The same elements are provided with the same reference numbers. Also here, the coat 12 of cured liquid silicone rubber is made to be transparent. It completely fills the tube spiral 1 .
[0064] The connecting element 17 has a projection 25 , which does, over a length corresponding at least to the inner diameter of the tube spiral 1 , extend into the spiral 1 of the tubes 3 . As shown, the projection 25 can be made in one piece with the basis plate 18 . However, it can also be made as a separate component, which is fixed on the basis plate 18 .
[0065] On its complete circumference, the projection 25 has a radial distance 29 to the tubes 3 , which again is filled with the cured liquid silicone rubber.
[0066] At its end, the projection 25 has a conical tapering 26 , in which the distance to the tubes 3 increases.
[0067] With this embodiment, the end area of the tube spiral is relieved. The largest stresses in the individual tubes 3 of metal occur after the winding and the placing of the ends 4 at the connecting element 17 . On the one side they occur at the transition from the spiral structure to the axial ends 4 , mainly caused by the mechanical deformation. On the other side they occur at the fixing spots of the tube ends 4 on the basis plate 18 , mainly caused by thermal load.
[0068] By means of the projection 25 , these statically “prestressed” areas of the line 2 can be separated from the spots, which are dynamically loaded during operation, particularly by vibrations. This reduces the risk of a rupture of the line.
[0069] The radial distance 29 between the tubes 3 and the projection 25 as well as the conical end 26 permit a certain flexibility of the line 2 , also in the area of the projection 25 , without giving rise to excessive stress loads.
[0070] FIG. 8 shows an embodiment of the connecting element 17 modified in comparison with FIG. 7 . Same parts and parts with the same function are provided with the same reference numbers as in FIG. 7 . Also here the coat 12 of cured liquid silicone rubber is shown to be transparent.
[0071] The connecting element 17 has a circumferential flange 27 , which surrounds the tubes 3 in their end area in the manner of a cover. At its open end, the flange 27 has a diameter extension 28 . The flange 27 has a radial distance 29 to the tubes 3 , or their ends 4 , respectively. The coat 12 extends into this distance 29 .
[0072] Also the flange 27 extends in the axial direction of the fluid line 2 over a length, which corresponds to at least the outer diameter of the tube spiral 1 . The mode of functioning is substantially the same as for the projection 25 . Additionally, an even better protection of the solder or weld seam 23 against external influences is achieved.
[0073] FIG. 9 shows an embodiment combining the features of the connecting elements of FIGS. 7 and 8 . The connecting element 17 has both a projection 25 and a circumferential flange 27 . This ensures an even better support of the ends 4 of the tubes 3 .
[0074] FIG. 10 is a schematic view of an injection moulding plant 30 for embedding the tube spiral 1 in the coat 12 . Two components A, B are supplied to a mixer 33 from two containers 31 , 32 . When needed, also a colour 34 can be supplied to the mixer 33 . Via a tube the mixed components A, B are supplied to an injection mould 36 . The injection mould is also called “injection tool”. The injection mould 36 has a connection 37 , in which the tube 35 ends. The connection 37 is cooled. This prevents the mix of the two components A, B from increasing their viscosity and curing already in the connection 37 . Besides, the injection mould 36 is preheated. Before insertion, the tube spiral 1 can be heated, for example to a temperature in the range from 150 to 200° C. The heat supply to the mixed components of the liquid silicone rubber ensures a very fast curing in the hollow 38 of the injection mould 36 . The cooling of the connection 37 permits the manufacturing of a practically boss-free injection moulded part in the form of a fluid line 2 .
[0075] FIG. 11 is a schematic view of some process steps of the manufacturing of the fluid line. Same elements as in the FIGS. 1 to 10 are provided with the same reference numbers.
[0076] The injection mould 36 is opened ( FIG. 11 a ). The tube spiral 1 with the connecting elements 4 , 5 and, if required, the core 11 is inserted in the injection mould 36 , and the injection mould 36 is closed ( FIG. 11 b ). Then, liquid silicone rubber 39 is supplied via the tube 35 and the cooled connection 37 ( FIG. 11 c ). As soon as the hollow 38 is filled ( FIG. 11 d ), a heat supply and/or an amount of time ensures curing of the liquid silicone rubber 39 . As soon as the liquid silicone rubber 39 has cured, the injection mould 36 is opened, and the finished fluid line 2 can be removed ( FIG. 11 e ). A possible core 11 must then be removed. The fluid line 2 with practically no bosses is the result.
[0077] While the present invention has been illustrated and described with respect to a particular embodiment thereof, it should be appreciated by those of ordinary skill in the art that various modifications to this invention may be made without departing from the spirit and scope of the present invention.
|
A method for producing a fluid line ( 2 ) and a corresponding fluid line ( 2 ) are specified, wherein a number of tubes are wound in parallel along a helical line in each case, a connecting element ( 6, 7 ) is fastened to at least one end and the tubes are embedded in a plastic material. It is wished to make production simple. For this purpose, it is envisaged to use a liquid silicone rubber ( 12 ) as the plastic material.
| 1
|
FIELD OF THE INVENTION
This invention relates to the delivery of gases or liquids from storage containers such as pressurized tanks or cylinders. More specifically this invention relates to preventing uncontrolled discharge of gases from such containers.
BACKGROUND OF THE INVENTION
Many industrial processing and manufacturing applications require the use of highly toxic fluids. The manufacture of semiconductor materials represents one such application wherein the safe storage and handling of highly toxic hydridic or halidic gases becomes necessary. Examples of such gases include silane, germane, ammonia, phosphine, arsine, stibine, hydrogen sulfide, hydrogen selenide, hydrogen telluride, and other halide compounds. As a result of toxicity and safety considerations, these gases must be carefully stored and handled in the industrial process facility. The semiconductor industry in particular relies on the gaseous hydrides of arsine (AsH 3 ) and phosphine (PH3) as sources of arsenic (As) and phosphorus (P) in ion implantation. Ion implantation systems typically use dilute mixtures of AsH 3 and PH 3 at pressures as high as 1500 psig. Due to their extreme toxicity and high vapor pressure, their use, transportation and storage raise significant safety concerns for the semiconductor industry.
Looking at arsine handling as a more specific example of how an extremely toxic gas is used by the semiconductor industry, arsine is typically stored in pressurized containers at about 250 psi. The handling of arsine cylinders in production environments presents a wide variety of hazardous situations. A leak in one 140 gram cylinder of arsine could contaminate the entire volume of a 30,000 square foot building with 10 foot high ceilings to the Immediate Danger to Life and Health (IDLH) level. If the leak were large, this could happen in just a minute or two, which would mean that for many hours there would be extremely deadly concentrations in the area near the source of the spill.
An arsine container typically uses a 500 cc gas cylinder with a valve at one end. Liquid arsine pumped at about 250 psi fills the cylinder to about 20% of its capacity (about 140 grams of arsine). Once filled, the valve is closed and a safety cap is installed on the valve outlet port. The cylinder is light (about 5 pounds) and the valve is strong compared to the weight of the cylinder so that dropping the cylinder onto the valve end from 10 or 20 feet above a concrete floor will not breach the integrity of the valve or cylinder. This strength of these small cylinders eliminates the need for the valve protection that usually appears on larger gas cylinders.
An end-user that receives the container will, in a well ventilated area, remove the safety cap, install the container, usually vertically, on the end-use apparatus, and open the valve. The container then dispenses liquid or gas arsine depending on the position of the valve end. If the valve end is down, arsine liquid will be dispensed. If the valve end is up, arsine gas will be dispensed. Regardless of valve position, end-user apparatus always uses arsine in gas phase whether discharged from the cylinder as a gas or converted from liquid to gas within the end-user apparatus.
The saturation pressure of liquid arsine at room temperature (22° C.) is about 250 psi. This means that any leak in the container to apparatus connections or in the end user apparatus itself will have arsine exiting to atmosphere at 250 psi. Thus, connections that remain absolutely leak tight to 250 psi or better must join all parts of the apparatus and supply container. If the end user were to first open the valve and then remove the safety plug, the entire 140 grams of arsine could spill out in as little as one or two seconds, especially if the valve end were down. Such an event could happen if someone turns the valve handle full open hard with enough torque such that the handle sticks sufficiently to mislead someone else into thinking that the valve was closed. Removal of the safety cap or disconnection of the cylinder under the mistaken belief that the valve was closed could then result in a rapid release of arsine.
In view of the serious potential for injury or death that could result from an unintended release of these fluids, the prior art discloses systems for preventing such catastrophic release of toxic fluids. U.S. Pat. No. 4,744,221 teaches the storing and the subsequent delivery of arsine by contacting arsine at a temperature of from about -30° C. to about +30° C. with a zeolite to adsorb arsine on the zeolite for storage. Heating then dispenses the arsine from the zeolite at an elevated temperature of up to about 175° C. The method of the '221 patent imposes a disadvantageous heating requirement on the arsine delivery. One problem with heating is that the storage vessel typically has a significant heat capacity. The heat capacity of the storage vessel introduces a significant lag time in the dispensing operation. Further, heating can decompose the arsine resulting in the formation of hydrogen gas with its potential explosion hazards. Thermal decomposition of arsine also causes an undesired increase in gas pressure for the process system.
U.S. Pat. No. 5,518,528 provides a system for storage and dispensing of hydridic and halidic gases which operates at ambient temperature by using a pressure reduction to desorb toxic fluids from zeolite materials having high storage (sorptive) capacity for these gases. The '528 patent uses a dispensing assembly to provide a pressure below the interior pressure of the storage vessel. The reduced pressure desorbs the sorbate gas from the solid-phase physical sorbent medium. In order to retrieve a significant portion of the arsine off of the adsorbent, very low pressures must be used. When full, the dispensing pressure might be 600 torr. When half full it will be down to about 70 torr. Most mass flow controllers are only rated down to 150 torr operating pressure. At 150 torr 60% of the arsine on the adsorbent remains on the adsorbent. Some modifications to the customer's equipment may be necessary to install the very low pressure mass flow controllers required for utilizing more than 40% of the arsine in an adsorbent type cylinder.
Valve lock arrangements provide more direct means of limiting the flow of liquid from carrier gas storage devices. U.S. Pat. No. 4,738,693 specifically discloses the use of membrane and diaphragm elements to prevent liquid discharge in the delivery of dopines for the semi-conductor industry.
The use of tubes with multiple capillary passages presents problems of forming the capillary structure into an arrangement that is suitably connected to the container that requires the flow restriction. It is known in the art to make a multi-passage capillary assembly using hollow tubes with outer hexagonal profiles. The circular holes in such a bundle are ordered with no void space in the walls. One problem with bundling of hexagonal capillaries is that the glass is typically a low melting point lead glass. Lead glass can be easily cast or shaped through a die to form the required external hex pattern. However, the low melting point of the lead glass results in a structure that is stiff and easy to shatter. Generally, the lower the melting temperature of a glass the greater the modulus of elasticity (stiffness) of that glass. Lead glass with its low melting temperature has a somewhat higher modulus of elasticity than higher melting point glasses. Therefore, for a given strain (deformation), it has higher internal stresses and is accordingly more likely to fracture. Lead glass has a further problem of chemical erosion. But the biggest disadvantage to this approach is the resultant final shape of the assembly which is a hex. Since the ends of the multi-capillary need to be attached to other parts in a gas chromatograph, the hex shape causes difficulties in getting compression type fittings to interface.
The problem of making connections to capillary structures is not a trivial one. The fine diameters of tubing and the low tensile strength of capillary column materials, such as fused silica, makes the arrangement of capillary columns and of capillary connectors for the capillary tubes especially difficult. Although many methods and procedures for making such connections are possible the connections generally require bonding to a conduit that has a circular cross-section. A suitable connection arrangement is described in U.S. Pat. No. 5,692,078.
The obvious solution is to make the outer cross section of the multi-capillary a circle for a more compatible fit to conventional compression fittings. This approach though confronts a mathematical problem that nobody has solved and that is: small circles in a larger circle do not pack in a uniform manner. This problem has presented itself in many different forms over the last several hundred years in stranded steel cables, in electrical conduits, etc. Simply put, circles packed together do not want to form an outer shape of a circle--circles packed together with the proper number of elements form hex shaped outlines.
It is a broad object of this invention to limit the release of toxic gases in the event of a valve or conduit failure.
It is an object of this invention to provide a multi-passage capillary assembly that has high ductility and a cross section compatible with the necessary fittings for sealing fluid flow through the capillary.
It is a further object of this invention to provide a multi-passage capillary assembly that provides a high degree of uniformity in the individual cross sections of the multiple capillaries and has an outer cross section of the assembly that is compatible with the necessary fittings for sealing fluid flow through the capillary passages.
A yet further object of this invention is to provide a discharge system that constrains the flow of gas during normal operation as well as during any kind of valve mishandling or valve failure.
A specific object of this invention is to provide safeguards for the delivery of arsine.
SUMMARY OF THE INVENTION
The apparatus of this invention provides a flow restriction in the storage container in the form of a tube having multiple uniformly shaped capillaries that will positively limit the discharge of gas phase fluid from the container to a low mass flow rate. The mass flow rate is typically at or above the maximum desired flow rate at which the container must supply gas to the end use device, but yet restrictive enough to severely limit any accidental discharge rate. This invention can beneficially supply fluid in any application that consumes the fluid at a relatively low rate in relation to the unrestricted discharge rate from the cylinder. The multiple fine capillary passages provide a highly useful flow restriction where variations in both the length and diameter will allow adjustment of the maximum fluid discharge rate and the multiple flow capillary passages permit continued delivery if minor amounts of impurities plug one or more of the passages. The multiple capillary flow restriction may have a location anywhere upstream of the container outlet or container valve outlet. Preferably the flow restriction has a location inside the cylinder or tank that supplies gas.
The discharge of liquids from the container poses a special hazard since the mass rate discharge of liquid will greatly exceed the mass rate discharge of the corresponding gas through the same restricted opening. Accordingly, the location of the inlet to the flow restrictor can aid in controlling fluid discharge. A particularly beneficial arrangement will locate the inlet to the flow restrictor in a manner that prevents liquid discharge from the container. In the case of arsine, the container is only filled to about 20% liquid by volume. Therefore, locating the inlet to the flow restrictor at the midpoint of the arsine cylinder prevents the discharge of liquid arsine whether the cylinder is located upside down or right side up. Further, locating the inlet at the radial center of the cylinder will prevent liquid discharge for any vertical or horizontal position of the partially filled cylinder.
Accordingly in a broad embodiment this invention is an apparatus for controlling the discharge of pressurized fluids from the outlet of a pressurized tank. The apparatus includes a container for holding a pressurized fluid in an at least partial gas phase, an outlet port for releasing pressurized gas from the container, and a gas flow path defined at least in part by the outlet port for delivering pressurized gas from the container. A restrictor in the form of a tube having multiple capillary sized passages of relatively uniform diameter is located along at least a portion of the gas flow path and restricts the outflow of gas to a minimal rate that is typically less than 100% more than the maximum gas delivery rate required from the container.
The most beneficial use of this invention incorporates the additional safeguard of a regulator that automatically limits the release of any toxic fluid delivered through the outlet of a storage container as claimed in copending application U.S. Ser. No. 062,599 filed Apr. 17, 1998. The regulator uses a condition responsive valve element at or downstream of the storage container outlet to prevent discharge of fluid unless a suitable discharge condition exists outside of the container or is imposed on the pressure regulator. The discharge condition represents a predetermined condition that is highly unlikely to occur during storage or handling of the valve under normal handling and storage procedures and at normal atmospheric conditions. Such conditions may include heating of the regulator, or imposition of an electrical current, voltage potential, magnetic field or extraordinary mechanical forces on or about the regulator. Preferably the regulator will comprise a pressure sensitive element that will prevent discharge of fluid until a preselected pressure condition, or more preferably a vacuum condition, exists downstream of the regulator. As a further safeguard the discharge condition can be specially tailored to be supplied by the end use device such that the discharge condition cannot be imposed until the container is properly positioned within or about, and safely connected to, the end use device. In this manner the invention can provide a fail safe system for delivery of toxic fluids from storage containers. The regulator may have a location upstream or downstream of the container valve. For effectiveness the container valve or the container itself will house the regulator. A location upstream of the container valve offers the most protection to the regulator and its fail safe operation.
Accordingly, in a limited apparatus embodiment this invention is an apparatus for controlling the discharge of pressurized fluids from the outlet of a pressurized container. The apparatus comprises a port body for communication with the outlet of a pressurized container to define a fluid discharge path from the container. A pressure regulator fixed in or ahead of the port body contains a valve element adapted for movement between a sealing position that blocks fluid flow through the fluid discharge path and an open position that permits fluid flow along the fluid discharge path. A diaphragm defines an interior volume isolated from the pressure condition upstream of the port body and engaged with the valve element for controlling the movement of the valve element in a manner that retains the valve element in the sealing position until a pressure differential between the inside of the diaphragm relative to the pressure outside the diaphragm moves the valve element to the open position. A tube defining multiple and uniformly sized capillary passages located along the fluid discharge path restricts the discharge of gas from the fluid outlet port to a mass flow rate of less than 5 cc per minute at standard temperature and pressure (sccm).
Additional objects, embodiments, advantages, and details of the invention are described in the following detailed description of the preferred embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view of a cylinder and head valve assembly incorporating the apparatus of this invention.
FIG. 2 is an enlarged view of the cylinder head assembly.
FIG. 3 is an alternate arrangement for the interior of the cylinder.
FIG. 4 is a section of FIG. 3 taken at lines 4--4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
For purposes of explanation and not limitation this invention is further described in the context of the delivery of arsine gas. Looking then at FIG. 1, the invention in one form looks from the outside like a typical dispensing unit comprising a 500 cc cylinder 10 with cylinder head valve 12 at the top end and having a valve outlet 16. The interior of the cylinder contains a capillary tube 13 having an inlet 14 that supplies arsine gas to a valve inlet 11. Until exhausted, a liquid arsine reservoir 15 at the bottom of cylinder 10 replenishes the arsine gas as it leaves the cylinder and maintains the vapor pressure of the cylinder. A regulator 17, located in valve 12, contains a bellows assembly 28 that automatically controls the discharge of arsine gas from the cylinder. A handle 18 allows manual control of a main valve element 19.
FIG. 2 shows regulator 17 and the internals of head valve 12 in more detail. Following then the path of the arsine gas out of head valve 12, the gas first enters through a tube 13 into valve inlet 11. Tube 13 contains multiple capillary passages of uniform size, similar to those depicted in FIG. 4. The body of head valve 12 contains the regulator 17. Entering gas first contacts a valve element in the form of poppet valve 20. A spring 21 biases poppet valve 20 against a valve seat 22 to create a closed condition along the gas flow path. Spring 21 normally presses poppet valve 20 against valve seat 22 until the diaphragm element of the regulator, in the form of a bellows 23, expands to displace a contact plate 24. Contact plate 24 acts on a control pin 25 that pushes poppet valve 20 away from valve seat 22. Arsine gas may then flow through pin passage 26 around pin 25 and into a bellows chamber 27 that houses the bellows assembly 28.
Bellows assembly 28 consists of a bellows guide 29 that defines an internal pressure chamber 30 having walls 31 that support the inside of bellows 23; an outer sleeve 32 that surrounds the exterior of bellows 23; and a bottom guide plate 33. Sealing contact at the upper end of the bellows 23 with bellows guide 29, and at the lower end of the bellows with contact plate 24, isolate the bellows from pressure within chamber 27 and the gas flow path in general. Internal chamber 30 is typically sealed at atmospheric pressure such that a reduction in pressure within bellows chamber 27 causes the gases in bellows chamber 30 to expand bellows 23 and urge contact plate 24 downward against pin 25. Bellows guide 29 retains sleeve 32 about its outer edge. Sleeve 32 positions with guide plate 33. Together, bellows guide 29, sleeve 32 and guide plate 33 protectively enclose bellows 23. Pin 25 passes through a central hole in the guide plate 33 to maintain its alignment with contact plate 24.
Arsine gas that passes out of bellows chamber 27 flows through a valve inlet port 34 and across sealing surfaces 35. Threaded bushing 36 clamps a multi-layer metallic diaphragm 48 to valve body 50 thereby forming a positive seal against fluid leaking past the valve stem 38. Handle 18 operating in conjunction with threaded valve stem 38, forces piston 51 via friction pad 52 onto diaphragm 48 to move the main valve plunger 37 down against the resisting force of spring 53. Downward movement of plunger 37 forces a Teflon sealing element 54, retained by nut 55, onto valve body 50 to create a seal at surfaces 35. Backing valve stem 38 away from diaphragm 48 allows spring 53 to force valve plunger 37 up, thereby separating the sealing surfaces 35 and permitting gas to flow through port 34. Once past sealing surfaces 35 arsine gas flows from a chamber 40 to an outlet port 41 and to the valve outlet 16.
This regulator arrangement 17 can be set to reliably prevent opening of the poppet valve 20 until pressure within the valve body drops to a vacuum condition. This condition is usually equal to 500 torr or less. With this setting of the regulator, opening of the main valve, with or without the protective cap in place, would not dispense arsine from the cylinder. Since the typical end-user's apparatus operates at pressure less than 100 torr, dispensing arsine at a vacuum, and particularly at pressures of 500 torr or less, has several distinct advantages. For instance there is a negative pressure at all of the arsine gas connections, so leaks can only leak into the end-user apparatus where they are quickly detected by the apparatus itself. Thus, one does not have to check joint by joint to verify that there are no leaks. In addition no external pressure regulators are required for reducing the tank pressure to pressures acceptable to the mass flow controllers. More importantly, an accidental opening or failure of a pipe connection in the arsine system is orders of magnitude less hazardous in a vacuum operated system than in a pressure operated system.
The use of the restricted flow passage further increases safety in the unlikely event that regulator 17 fails to check gas flow when desired. The uniformly sized capillary passages offer the most flexibility and reliability as the flow restrictor. The multiple small diameter bores will desirably limit the transport of gas phase fluids to very low rates while permitting the higher flow of liquids at higher flow mass rates due to their higher density. The capillaries of the restrictor will typically limit the discharge of fluid to not more than 10 sccm and more preferably to less than 5 sccm.
Looking again at FIG. 1 to more fully explain this form of the flow restrictor, capillary tube 13 provides the only exit from cylinder 10. The winding formation of capillary tube 13 maintains inlet 14near the axial and radial center of cylinder 10. The internal diameter of the capillaries will ordinarily not exceed 20 micrometers. For a single capillary, this diameter limits the rate that the 250 psi saturation pressure of arsine can force arsine through the tube to only 60 milligrams per minute. Typical end-users require only 3 to 10 milligrams per minute (1 to 3 sccm). At the 60 milligram rate it would take 40 hours for the container to empty. It would take one hour for a 30 by 30 room with 10 foot ceilings to reach the arsine Immediate Danger To Life and Health (IDLH) level. One hour should provide ample time for alarms to warn personnel to exit and response teams take necessary action. Therefore, the diameter of the multiple capillaries will ordinarily be less than 20 micrometers.
As mentioned, the length as well as the diameter of the capillary may be adjusted to provide a maximum desired flow rate through the restriction. In the case of arsine delivery at the previously mentioned rates, the capillary is typically 15 cm long. For that length, it would require four capillaries in parallel with a diameter of about 9 micrometers to provide about the same flow capacity. The multiple capillary passages in the restriction tube of this invention may be as small as 2 microns. However the size of the capillary passages will usually be set to use not more than 19 and not less than 7 capillary passages to provide numerous passages while still allowing gas release under reasonable pressures.
A useful feature of this invention is the provision of the essentially round outer cross section of the tube with the relatively uniform internal capillary passages. The internal open flow area through the tube will be defined almost entirely by the regular capillaries, i.e. those with cross sections in the form of the same regularly recurring shape. The regular capillaries preferably have a round cross section. The roundness of the individual capillary passages may be defined by the variation in diameter, taken along any two lines of direction across the substantially circular cross section of each capillary passage, not exceeding 15%. The uniformity of the different uniform capillary passages may be defined by the variation in average diameter between capillaries not exceeding 15%. Any remaining flow area through the tube is typically in the form of irregular capillary sized passages having individual cross sectional areas that are less than the individual cross sectional areas of the regular capillary passages. Typically the irregular capillaries will have an average cross sectional area that equals 50% or less of the average flow area of the regular capillaries. The relatively small diameter of the irregular capillaries minimizes the detrimental effect that the presence of the irregular capillaries may have on the regulation of the flow rate through the restrictor.
The preferred structure of this invention is a uniform multi-capillary assembly that virtually eliminates the presence of irregular capillaries. In this preferred structure the internal open area defined by regular capillaries will equal at least 95% and more preferably at least 99% of the total internal open area through the assembly. The most preferred form of this structure eliminates all irregular capillaries. Furthermore, any irregular capillaries that are found in the preferred structure will have minimal affect. Any such irregular capillary will have an open area equal to 10% or less than the open area of any regular capillary .
The outer wall and the inner walls of the multicapillary assembly may be made from any material that is suitably formed into the required structure. Thus the resulting capillary structure has an operating temperature that is limited by the stability or transition temperature of the material defining the capillaries. Capillaries of this size may be made from various glass materials. Drawing techniques used for forming glass fibers and tubes lend themselves most readily to the production of the tube structure of this invention. Suitable glass materials include lead silicate, borosilicate, conventional glasses (soda lime silicate), and other forms of high purity silica such as quartz or fused silica. A particularly preferred glass material is an alumino-silicate.
A variety of suitable capillary structures may be created. The capillary structure may be wound as shown in FIG. 1 to provide extra length. Alternately, FIG. 3 shows a tank that uses a modified form of a capillary defined by a straight capillary tube arrangement 13' with its inlet 14' centered at the radial and axial midpoint of cylinder 10.
As also shown by FIG. 4, the thickness of the glass wall relative to the capillary diameter may be made quite large to overcome any fragility of the glass. Proper containment can further overcome any fragility of glass. As shown more clearly by the cross-sectional view in FIG. 4, tube 46 preferably defines a hexagon arrangement of six capillary passages 43 that surround a central capillary passage 44 and wherein all of the capillaries have the same relatively smaller diameter with respect to the inside diameter of the glass tube 46.
Once formed, an outer sleeve may surround the tube to provide additional support and structural integrity. Metallic materials will work well as outer sleeves. An optional metal tube 42, typically constructed from stainless steel when provided, may protectively surround the glass tube 46. Metal tube 42 adds further rigidity and durability when optionally shrunk around tube 46 to provide a reinforced unit. With the optional reinforcement of metal tube 42, fracture of the glass tube would again leave the function of the restricted flow path through capillary arrangement 13' substantially unchanged. An especially beneficial arrangement may shrink a metallic sleeve around a glass multi-capillary assembly to compress the tube into the sleeve. An arrangement of this may provide the needed structural support for imposing the necessary ultra-high pressures that are required to push many fluids through capillaries that approach 2 micrometers in diameter.
This invention uses a forming method that readily provides the assembly of the structure of this invention and in particular the uniform multi-capillary assembly of this invention. The method forms the multi-capillary tube or conduit with a substantially circular perimeter that surrounds a plurality of regular capillary passages defined by internal walls within an outer wall. The method starts with inserting a plurality of smaller conduits into a surrounding tube to form a tube and conduit assembly. The conduits may be formed by drawing down the tube stock to the desired conduit size. The number of inserted conduits will correspond with the number of regular capillaries obtained by the forming method. Common openings of the conduits are sealed about one end of the tube and conduit assembly to form a drawing stock having a closed end about which all conduits are sealed from fluid flow and an opposite open end about which all conduits are open for fluid flow. The drawing stock is then heated to a softening temperature in a suitable drawing apparatus. Simultaneously drawing the heated drawing stock while restricting fluid flow from the open conduit ends of the drawing stock reduces the interiors of the conduits to capillary size while preventing collapsing closure of the conduit interiors. A multi-capillary tube that has a number of capillary passages substantially equal to the number of conduits may be recovered from the stretched and cooled drawing stock. In many cases the reduction of the diameter of the conduits during the drawing of the heated drawing stock provides sufficient reduction in the diameter at their open ends to suitably restrict gas flow out of the interiors of the conduits to a rate that maintains the desired final diameter of the capillary passages formed from the conduits.
Preferably the conduits will again have a round cross section. Prior to drawing, the conduits in the tube and conduit assembly will preferably have a diameter in a range of from 0.5 to 1 mm and a wall thickness of from 100 to 300 micrometers. The multi-capillary assembly will usually contain at least 7 regular capillary passages. The thickness of the outer tube will usually average from 1 to 10 mm. The inner diameter of the outer tube will be determined by the number and outer diameter of the inner conduits. The most effective packing arrangement for the inner conduit has been found to be a number of circular rings of conduits that surround a central conduit. Jacques Dutka, in Machinery Journal, October 1956, gives the maximum number of small circles that may be packed into a larger circle for a number of different packing arrangements. Based on these formulas it has been found that for this invention the typical number of total passageways in a given number of passageway rings is best given by the formula for maximizing circles as presented in the foregoing reference. Therefore, where the desired arrangement for round conduits is as an assembly of rings about a central tube, the number of conduits in the assembly is determined by:
N=3n.sup.2 +3n+1;
where,
N=the total number conduits, and
n=the number of rings of conduits around the central conduit.
Where all of the inner conduits have the same outer diameter the preferred inner diameter of the outer tube is calculated in terms of a "K" factor defined by the above reference. Accordingly the outer tube has an inner diameter "D" determined by the outer diameter "d" of the inner conduits where:
D=K*d
The factor K varies mathematically with the number of inner conduits. Values for K are set forth in the above reference. Examples of specific "K" values are set forth in Table 1 for arrangements that wrap rings of conduits around a central conduit.
TABLE 1______________________________________# of inner conduits I.D. of Outer tube______________________________________2-7 3 8-13 4.465 13-19 5 20-31 6.292 32-37 7.001 38-43 7.929 44-55 8.212______________________________________
An important parameter when seeking to minimize irregular channel formation is temperature uniformity during the drawing process. It has been found that the drawing apparatus should not permit substantial temperature variations during the drawing operation. Temperature variations should be held to less than 5° C. over the length of the draw. A number of other forming techniques and material properties can be important to obtaining a uniform multi-capillary structure. Drawing the structure from conduits that themselves have very uniform bores and walls enhances the uniformity of the resulting structure. Uniformity of the individual conduits may be enhanced by drawing the starting conduits down in several stages from large conduits. Uniformity of the resulting capillaries also improves as the alignment of the conduits in the drawing stock becomes more parallel. For a glass material comprising aluminosilicate glass the glass melting point used in the draw is typically 1120° C. The starting conduits have their top ends capped to inhibit gas flow in the tubing. This prevents the tubes from collapsing and forming a solid rod during the drawing process. The structure for the drawing stock is assembled one row of conduits at a time using glue or rubber bands to hold each row in place. The assembly is mounted in the drawing tower and allowed to slowly equilibrate at the softening temperature of the glass. This begins to establish the surface forces on the initial part of the assembly and corrects for slight packing errors. The tip of the preform is then dropped and a tractor is used to draw the preform structure from the furnace. The drawing furnace is usually operated at a top feed rate of 1 mm/min, a bottom feed rate of 190 mm/min with a helium carrier gas flow of 6 L/min and a furnace temperature of 983° C. Capillaries of other sizes may be produced in varying numbers using the same formula and similar techniques. Additional details of drawing multiple capillary tubes is disclosed in the copending application 067,109, filed, Mar. 27, 1998, the contents of which are incorporated by reference.
Where the capillary is the only entrance, arsine for filling the cylinder must enter through the capillary size opening. Cylinder filling normally requires the pumping of liquid arsine into the cylinders. Liquid arsine has a density about 500 times greater than gaseous arsine. Consequently for most liquid-fill, gas-withdrawal systems, filling will take orders of magnitude less time than the emptying of the cylinder.
In applications where fill time needs reduction, a larger port dedicated exclusively to cylinder filling may reduce times for recharging cylinders when desired or necessary for filling/delivery of other gas/gas or fluid/gas systems. In such arrangements the cylinder or valve may contain a separate entry port that by-passes the capillary or other flow restriction. Flow into the by-pass port may be controlled by a pressure, electrical or magnetic, or mechanical means to mention only a few possibilities.
It is also possible to fill the cylinder by using a displaceable restriction. Such a system is disclosed in copending provisional application 60/044107 filed Apr. 24, 1997. In this arrangement a filter element that can serve as a restriction element reciprocates between different positions, one for filling the container and another for withdrawing gas from the container. In the case of a restrictor, it may be in the form of a sealing body wherein the sealing body is adapted for displacement away from the seal surface to establish a fluid flow path from the container that inhibits fluid flow through the valve body and for displacement toward the seal surface to establish a fluid flow path from the container to the valve outlet port that passes fluid through the restrictor and restricts fluid flow from the container. In this manner a single port may be used to move fluid in and out of the container at automatically differing rates. The use of a single port through the tank inlet permits the port to have a large flow area through the narrow neck of most containers that facilitates filling of the tank with gases. A displaceable restrictor element may further incorporate valve sealing elements that move with the restrictor element to block any discharge of gas unless the restrictor is fully in contact with the seal surface.
|
The present invention uses a flow restrictor in the form of a tube containing multiple capillary sized passages to minimize any discharge of toxic gases from compressed gas cylinders in the unlikely event of the control valve or regulator failure. The use of this arrangement to provide a flow restriction in combination with a regulator in the form of dispensing check valve provides a virtually fail safe system for preventing hazardous discharge of fluid from a pressurized cylinder or tank. The multiple capillary passage structure provides carefully sized openings that minimize any discharge of gas. Location of the inlet to the capillary tube at the midpoint of the cylinder can also prevent the discharge of liquid from the cylinder if the control valve system fails. Limiting the accidental discharge of fluid from the cylinder to gas phase fluids greatly reduces the uncontrolled mass flow rate at which fluid can escape from the cylinder. A diaphragm can control the movement of a check valve element to prevent discharge of gas from a tank unless a predetermined vacuum condition exists downstream of the check valve. This system is particularly useful in the delivery of arsine gas and provides multiple safeguards against accidental discharge.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. Ser. No. 12/503,505 filed Jul. 15, 2009, which is a divisional of U.S. Ser. No. 11/486,748 filed Jul. 14, 2006, which is a continuation of international application PCT/EP2004/053137 filed Nov. 26, 2004, which claims priority to German Patent Application No. DE 102004002181.3 filed Jan. 15, 2004, all of which are incorporated in their entirety by reference herein.
FIELD OF THE INVENTION
The present invention relates to an integrated transistor and method for the production thereof.
BACKGROUND
Generally, bipolar transistors include connection regions referred to as the emitter region and base region. In a bipolar transistor, the reverse doping region is referred to as the base region. In field effect transistors, by contrast, the connection regions are referred to as the source region and drain region. In a field effect transistor, the reverse doping region serves for forming an inversion channel.
In so-called high-voltage transistors, a drift path is present in order to switch voltages of more than 40 volts, more than 50 volts or even more than 100 volts between the connection zones during normal operation.
A multiplicity of high-voltage transistors have been proposed heretofore whose electrical properties are improved by constructive measures, for example by field plates or by field rings. In particular, the breakdown voltage is increased or the chip area requirement is reduced by means of these measures. However, these transistors may have increased complexity with regard to design and manufacture.
SUMMARY
The invention relates to an integrated transistor having a semiconductor substrate, which is preferably monocrystalline or contains monocrystalline layers, a connection region remote from the main area and contained in the semiconductor substrate, said connection region being doped in accordance with a basic doping type and being arranged at a distance from a main area of the semiconductor substrate, a drift region contained in the semiconductor substrate, said drift region being doped in accordance with the basic doping type with a lower dopant concentration than the connection region remote from the main area, and said drift region being arranged between the connection region remote from the main area and the main area, a connection region near the main area, said connection region being doped in accordance with the basic doping type and being arranged, for example, at the main area of the substrate, a reverse doping region, which is doped in accordance with a different doping type than the basic doping type and separates the drift region from the connection region near the main area.
It is nevertheless one aspect of the invention that specifies an improved transistor which, in particular, is simple to produce, which, in particular, has outstanding electrical properties and which, in particular requires only a small chip area. Moreover, a production method is specified by means of which a transistor can be produced in a simple manner.
The invention is based on the consideration that the number of trenches does not influence, or influences only slightly, the production outlay for an integrated circuit arrangement. Even different trench depths and different trench fillings can be produced with little outlay. Furthermore, the invention is based on the consideration that diffusion zones for the connection of the connection region remote from the main area easily exceed a lateral dimensioning of greater than 20 micrometers on account of the all-around diffusion in the case of high-voltage transistors. Trenches are particularly suitable for avoiding long diffusion paths or for laterally delimiting a deep diffusion. A further function which can be provided by trenches in a simple manner is the isolating function, which can likewise be used for reducing the chip area for a transistor. However, specific functions cannot be performed simultaneously by trenches, for example the connection function and the isolating function. Consequently, only double trenches or triple trenches per component are suitable for improving the electrical properties in conjunction with a small chip area.
In addition to the features mentioned in the introduction, therefore, a transistor in one embodiment of the invention has an electrically insulating isolating trench extending from the main area in the direction of the connection region remote from the main area and consequently having an isolating function, and an auxiliary trench extending from the main area as far as the connection region remote from the main area and serving for connection of the connection region remote from the main area, for example the auxiliary trench offers access for a doping material that diffuses into the surroundings of the trench, or the auxiliary trench forms the lateral boundary of a diffusion process.
In one development, the isolating trench and/or the auxiliary trench has at least one of the following features: a trench width greater than one micrometer or greater than two micrometers, so that a sufficient dielectric strength is provided in the case of an isolating trench, a trench width less than ten micrometers or less than five micrometers, so that an excessively large amount of chip area is not required for the trench, a trench depth greater than ten micrometers or greater than fifteen micrometers, a sufficient voltage drop across the drift path being achieved only through these depths.
In another development, the isolating trench contains an electrical isolation that completely fills the trench. As an alterative, the isolating trench contains an electrically insulating isolation on the trench walls and on the trench bottom and also an electrically conductive region in the trench. By way of example, deep trenches can be filled with doped polycrystalline silicon, with undoped silicon, with an oxide, or be filled with some other material.
In another development, the isolating trench has the same depth as the auxiliary trench, so that it is not necessary to take measures for producing different depths. As an alternative, the auxiliary trench is deeper than the isolating trench. By way of example, the isolating trenches are covered at the beginning or at the end of the etching of the auxiliary trenches, only one additional photolithographic step being required, for example.
In a development with different trench depths, the distance between the bottom of the isolating trench and the connection region remote from the main area is in the range of ⅕ to ⅘ or in the range of ⅓ to ⅔ relative to the distance between the main area and the connection region remote from the main area. If, in the same depth as the already mentioned connection region remote from the main area, a further connection region remote from the main area is present, as far as which a further isolating trench extends, which has the same depth as the auxiliary trench, then an ESD protection element (electrostatic discharge) can be produced in the region of the shortened isolating trench in a simple manner, said protection element avoiding damage to the other component by means of its own early breakdown.
In another development, the auxiliary trench has the same trench filling as the isolating trench. Consequently, measures for introducing different trench fillings are not necessary. In an alternative configuration, by contrast, the auxiliary trench has a different trench filling than the isolating trench. In particular, the auxiliary trench is filled with an electrically conductive material, e.g. with doped polycrystalline silicon or with a metal, which is electrically conductively connected to the connection region remote from the main area. Different trench fillings can be achieved in a simple manner by the covering or the later formation of the other type of trench.
In a next development, a doping of the basic doping type with a higher dopant concentration than in the drift region is present between the isolating trench and the auxiliary trench, the doping filling the region between the isolating trench and the auxiliary trench completely—for example in the case of a vertical diffusion delimited by the two trenches—or only in the vicinity of the auxiliary trench and not in the vicinity of the isolating trench—for example in the case of a diffusion proceeding from the auxiliary trench.
In another development, the auxiliary trench is electrically insulating. The auxiliary trench extends into the substrate main region more deeply than the connection region remote from the main area and is arranged at the edge of an electronic component, so that it insulates the component from other components into the depth as well.
In a next development, a substrate main region is doped in accordance with the reverse doping type. A substrate trench extends from the main area as far as the substrate main region and serves for connection of the substrate main region. Consequently, three types of trench are present, namely the isolating trench, the auxiliary trench and the substrate trench. The substrate trench enables a simple and area-saving connection of the substrate, for example as access for a doping material that is introduced into the surroundings of the substrate trench, or as a lateral boundary of a diffusion process.
The technical effects discussed above for the auxiliary trench and the isolating trench also apply to the formation of the substrate trench, in particular with regard to the same depth of trenches and with regard to the same trench filling of trenches.
In a next development, a connection of the transistor is electrically conductively connected to the reverse doping region, so that the transistor is a bipolar transistor having a pnp layer sequence or an npn layer sequence. As an alternative, an insulating layer is present that is electrically insulating, adjoins the reverse doping region and isolates the reverse doping region from an electrically conductive control electrode of the transistor, so that a field effect transistor is formed which operates as an n-channel transistor or as a p-channel transistor.
The invention additionally relates to a method having the steps specified in the independent or coordinate method claim, the order in which the steps are specified not constituting any restriction. In the case of the method, similarly, a transistor with a multiple trench arises, so that the technical effects specified above also apply to the method.
Further objects, features and advantages of this invention will become readily apparent to persons skilled in the art after a review of the following description, with reference to the drawings and claims that are appended to and form a part of this specification.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows two bipolar transistors each having two trenches, a substrate connection being produced with the aid of a substrate trench;
FIG. 2 shows a bipolar transistor having two trenches, a substrate connection being produced by means of a large-area diffusion;
FIG. 3 shows a bipolar transistor having two trenches, a substrate connection being delimited by two substrate trenches;
FIG. 4 shows a field effect transistor having two trenches; and
FIG. 5 shows a bipolar transistor having two trenches with different lengths.
DETAILED DESCRIPTION
Exemplary embodiments are explained below which apply in principle both to bipolar transistors and to field effect transistors. In the exemplary embodiments, only one emitter or source connection and one base or gate connection are provided per component. In order to increase the switching current, other exemplary embodiments use, in one component, a sequence of emitter-base pairs which are respectively assigned a collector region, or source-gate pairs which are respectively assigned a drain region. By way of example, the collector or drain connection and/or the substrate connection encloses the emitter-base pairs or the source-gate pairs, respectively, of a component.
FIG. 1 shows two bipolar transistors T 1 and T 2 , a substrate connection of a substrate main part 10 being produced with the aid of a substrate trench 12 . The substrate main part 10 contains lightly p-doped silicon and is contained in a commercially available wafer, by way of example. Buried doping regions 14 and 16 have been introduced into the wafer, said doping regions being heavily n-doped and belonging to a buried layer 18 . A lightly n-doped epitaxial layer 20 has a layer thickness D 1 of twenty micrometers in the exemplary embodiment. The epitaxial layer 20 is adjacent to the substrate main area 10 and contains an upper layer part of the buried layer 18 .
The substrate trench 12 penetrates through the epitaxial layer 20 and ends in the substrate main part 10 . The substrate trench 12 is surrounded at its sidewalls 22 and at the trench bottom 24 by a substrate connection doping 26 , e.g. a high p-type doping, which surrounds the substrate trench 12 with a layer thickness of e.g. greater than 500 nanometers or of one micrometer. In particular, the layer thickness of the substrate connection doping 26 is less than three micrometers.
Heavily p-doped doping regions 32 and 34 extend from the surface 30 of the epitaxial layer 20 on both sides of the substrate trench 12 , said doping regions being electrically conductively connected to a metallic or polycrystalline substrate connection 36 . The doping regions 32 and 34 in each case have e.g. a depth of one micrometer and a width of one micrometer.
The two transistors T 1 and T 2 lie e.g. on both sides of the substrate trench 12 . The transistor T 1 contains a collector connection 40 , a base connection 42 , and an emitter connection 44 .
In another exemplary embodiment, further base connection-emitter connection pairs 45 of the transistor T 1 are present, indicated by dots. The collector connection 40 , the base connection 42 and the emitter connection 44 are electrically conductive and contain e.g. a metal or highly doped polycrystalline silicon.
In the transistor T 1 , there is an auxiliary trench 46 . The auxiliary trench 46 encloses an isolating trench 48 , which laterally isolates a drift zone 50 formed in the epitaxial layer 20 .
The auxiliary trench 46 penetrates through the epitaxial layer 20 and ends in the doping region 14 of the buried layer 18 . The auxiliary trench 46 is surrounded at its sidewalls and at the trench bottom by a collector connection doping 52 , for example a high n-type doping, which surrounds the auxiliary trench 46 with a layer thickness of e.g. 500 nanometers or of one micrometer. In particular, the layer thickness of the collector connection doping 52 is less than three micrometers.
A heavily n-doped doping region 54 extends from the surface 30 of the epitaxial layer 20 at the inner trench edge of the substrate trench 12 , said doping region being electrically conductively connected to the collector connection 40 . The doping region 54 has e.g. a depth of one micrometer and a width of e.g. greater than three micrometers, e.g. five micrometers. In another exemplary embodiment, there are doping regions for the collector connection 40 on both sides of the auxiliary trench 46 along the peripheral trench edge. As an alternative, there is only one outer doping region for the collector connection 40 on the right-hand side of the auxiliary trench 46 relative to the trench section illustrated in FIG. 1 .
A region of the epitaxial layer 20 lies between the substrate connection doping 26 and the collector connection doping 52 . By way of example, the minimum distance between the substrate connection doping 26 and the collector connection doping 52 is greater than ten micrometers, e.g. twenty micrometers.
The isolating trench 48 likewise penetrates through the epitaxial layer 20 and ends in the doping region 14 of the buried layer 18 . The isolating trench 48 is not surrounded by a doping region introduced with the aid of the isolating trench 48 .
A p-doped base region 56 extends from the surface 30 of the epitaxial layer 20 within the zone enclosed by the isolating trench 48 , said base region being electrically conductively connected to the base connection 42 . The base region 56 has e.g. a depth in the range of one micrometer up to three micrometers, e.g. of two micrometers, and a width of e.g. greater than four micrometers, e.g. ten micrometers.
The base region 56 encloses an n-doped emitter region 58 , which likewise extends from the surface 30 of the epitaxial layer 20 in the direction of the doping region 14 . The emitter region 58 is electrically conductively connected to the emitter connection 44 .
In the exemplary embodiment, the substrate trench 12 , the auxiliary trench 46 and the isolating trench 48 are completely filled with an electrically insulating material, namely with silicon dioxide. In the exemplary embodiment, the trench width B of the substrate trench 12 , of the auxiliary trench 46 and of the isolating trench 48 is 1.5 micrometers in each case. The trench depth is identical for all three trenches 12 , 46 and 48 and is 21 micrometers, by way of example.
The transistor T 2 is constructed like the transistor T 1 , so that reference is made to the explanations above. Elements of the transistor T 2 having the same construction and the same function as elements in the transistor T 1 bear the same reference symbol in FIG. 1 , but followed by the lower-case letter b, see e.g. a base region 56 b corresponding to the base region 56 , an auxiliary trench 46 b and an isolating trench 48 b.
By virtue of the construction of the transistors T 1 and T 2 that is illustrated in FIG. 1 , only a small chip area is required because the connection of the doping region 14 and 16 via the collector connection doping 52 and 52 b , respectively, lies very near to the base region 56 and 56 b , respectively, on account of the isolating trench 48 and 48 b , respectively. FIG. 2 shows a bipolar transistor T 3 , which is constructed like the bipolar transistor T 1 apart from the deviations explained below, so that like elements are designated by the same reference symbols but followed by the lower-case letter c, see:
Substrate main region 10 c,
Doping region 14 c in a buried layer 18 c,
Epitaxial layer 20 c,
Surface 30 c,
Collector connection 40 c,
Base connection 42 c,
Emitter connection 44 c,
Auxiliary trench 46 c,
Isolating trench 48 c,
Drift region 50 c,
Collector connection doping 52 c,
Doping region 54 c,
Base region 56 c , and
Emitter region 58 c.
In the case of the bipolar transistor T 3 , in contrast to the transistor T 1 and T 2 , the substrate connection was produced by means of a high p-type doping and a subsequent large-area diffusion in relation to the required chip area as far as the substrate main part 10 c . A smallest lateral dimensioning L 1 of a substrate connection doping 26 c is approximately equal to the diffusion depth at the surface 30 c , that is to say that the dimensioning L 1 is more than twenty micrometers in the exemplary embodiment. The required chip area is nevertheless smaller than in the case of previously known transistors on account of the use of the trenches 46 c and 48 c . Moreover, the large-area substrate connection does not have to be embodied separately for each transistor.
The substrate connection doping 26 c is electrically conductively connected via a p-type doping region 32 c to a substrate connection 36 c corresponding to the substrate connection 36 . The substrate connection doping 26 c is again separated from the collector connection doping 52 c by a zone of the epitaxial layer 20 c in which the original dopant concentration of the epitaxial layer is present.
FIG. 3 shows a bipolar transistor T 5 , which is constructed like the bipolar transistor T 1 apart from the deviations explained below, so that identical elements are designated by the same reference symbols but followed by the lower-case letter d, see:
Substrate main region 10 d,
Doping region 14 d in a buried layer 18 d,
Epitaxial layer 20 d,
Surface 30 d,
Collector connection 40 d,
Base connection 42 d,
Emitter connection 44 d,
Auxiliary trench 46 d,
Isolating trench 48 d,
Drift region 50 d,
Collector connection doping 52 d,
Doping region 54 d,
Base region 56 d , and
Emitter region 58 d.
In the case of the bipolar transistor T 5 , in contrast to the transistors T 1 , T 2 and T 3 , a substrate connection doping 26 d was produced by a diffusion that was laterally delimited by two substrate trenches 60 and 62 . The substrate trenches 60 and 62 have the width B, that is to say the same width as the auxiliary trench 46 d and the isolating trench 48 d . The depth of the substrate trenches 60 , 62 also matches the depth of the auxiliary trench 46 d and the isolating trench 48 d , that is to say that the depth is 21 micrometers in the exemplary embodiment. The substrate trenches 60 and 62 contain the same filling material as the auxiliary trench 46 d and the isolating trench 48 d.
Although the substrate connection doping 26 d has been outdiffused into the depth over ten micrometers as far as the substrate main region 10 d , the smallest lateral dimensioning L 2 or the width of the substrate connection doping 26 d is less than five micrometers. The lateral dimensioning L 2 is prescribed by the distance between the walls of the substrate trenches 60 and 62 bearing against the substrate connection doping 26 d and is three micrometers in the exemplary embodiment.
The substrate connection doping 26 d is electrically conductively connected via a p-doped doping region 32 d to a substrate connection 36 d corresponding to the substrate connection 36 . A region in which the original doping of the epitaxial layer 20 d is retained lies between that wall of the substrate trench 60 which faces the auxiliary trench 46 d and the collector connection doping region 52 d . By way of example, a distance A between the collector connection doping region 52 d and the trench wall of the substrate trench 60 is less than five micrometers, one micrometer in the exemplary embodiment.
The connection variant of the substrate main region 10 d illustrated in FIG. 3 is thus space-saving and has very low impedance. On account of the good connection of the substrate main region 10 d , the high-voltage transistor T 5 also has good switching properties.
FIG. 4 shows a field effect transistor T 6 , a substrate connection of a substrate main part 110 being produced with the aid of a substrate trench 112 . The substrate main part 110 contains lightly p-doped silicon and is originally contained in a commercially available wafer, by way of example. Doping regions have been introduced into the wafer, e.g. a doping region 114 , said doping regions being heavily n-doped and belonging to a buried layer 118 . In the exemplary embodiment, a lightly n-doped epitaxial layer 120 has a layer thickness D 2 of twenty micrometers. The epitaxial layer 120 is adjacent to the substrate main region 110 and contains an upper layer part of the buried layer 118 .
The substrate main region 110 is connected like the substrate main region 10 , that is to say by the substrate trench 112 , which is formed like the substrate trench 12 , a substrate connection doping 126 corresponding to the substrate connection doping 26 , heavily p-doped doping regions 132 and 134 corresponding to the doping regions 32 and 34 , respectively, and by a substrate connection 136 having the same construction and the same function as the substrate connection 36 .
The transistor T 6 contains a drain connection 40 , a gate connection 42 , and a source connection 44 .
The drain connection 40 , the gate connection 42 and the source connection 44 are electrically conductive and contain e.g. a metal of highly doped polycrystalline silicon.
In the transistor T 6 , there is an auxiliary trench 146 enclosed by the substrate trench 112 , for example. The auxiliary trench 146 , for its part, encloses an isolating trench 148 , which laterally isolates a drift zone 150 formed in the epitaxial layer 120 .
The buried doping region 114 is connected like the doping region 14 , that is to say by the auxiliary trench 146 , which is formed like the auxiliary trench 46 , a drain connection doping 152 corresponding to the collector connection doping 52 , and a heavily n-doped doping region 154 , which is formed like the doping region 54 .
A region of the epitaxial layer 120 lies between the substrate connection doping 126 and the drain connection doping 152 . By way of example, the minimum distance between the substrate connection doping 126 and the drain connection doping 152 is greater than ten micrometers, typically equal to the thickness of the epitaxial layer 120 .
The isolating trench 148 likewise penetrates through the epitaxial layer 120 and ends in the doping region 114 of the buried layer 118 . The isolating trench 148 is not surrounded by a doping region introduced with the aid of the isolating trench 148 , but rather directly adjoins the epitaxial layer 120 .
A p-doped channel doping region 156 extends from the surface 130 of the epitaxial layer 120 within the zone enclosed by the isolating trench 148 , said channel doping region serving for forming an inversion channel. The channel doping region 156 has e.g. a depth in the range of one micrometer up to three micrometers, e.g. of two micrometers, and a width greater than four micrometers, e.g. ten micrometers.
The channel doping region 156 encloses an n-doped source region 158 which likewise extends from the surface 130 of the epitaxial layer 120 in the direction of the buried doping region 114 . The source region 158 is electrically conductively connected to the source connection 144 . A lightly n-doped extension region 160 of the source region 158 is optionally situated between the channel doping region 156 and the source region 160 .
A dielectric 162 made of silicon dioxide, for example, is situated on the surface of the channel doping region 156 that lies between the source region 158 and the isolating trench 148 . The thickness of the dielectric 162 is more than 10 nanometers, in particular 15 nanometers. A gate region 164 made e.g. of a metal or highly doped polycrystalline silicon is arranged on that side of the dielectric 162 which is remote from the epitaxial layer 120 . The gate region 164 is electrically conductively connected to the gate connection 142 .
In the exemplary embodiment, the substrate trench 112 , the auxiliary trench 146 and the isolating trench 148 are completely filled with electrically insulating material, namely with silicon dioxide. In the exemplary embodiment, the trench width B of the substrate trench 112 , of the auxiliary trench 146 and of the isolating trench 148 is 1.5 micrometers in each case. The trench depth is identical for all three trenches 112 , 146 and 148 and is 21 micrometers, by way of example.
The field effect transistor T 6 is a field effect transistor in which the channel length is determined by the dimensions of the gate. In an alternative exemplary embodiment, the field effect transistor T 6 is a doubly diffused field effect transistor in which the channel length is set by way of a diffusion length. The field effect transistor T 6 can also be produced on a small chip area and is nevertheless suitable for switching voltages of greater than 40 volts, greater than 50 volts or even greater than 100 volts.
FIG. 5 shows a bipolar transistor T 8 , which is constructed like the bipolar transistor T 1 apart from the deviations explained below, so that identical elements are designated by the same reference symbols but followed by the lower-case letter e, see:
Substrate main region 10 e,
Doping region 14 e in a buried layer 18 e,
Epitaxial layer 20 e,
Surface 30 e,
Collector connection 40 e,
Base connection 42 e,
Emitter connection 44 e,
Auxiliary trench 46 e,
Isolating trench 48 e,
Drift region 50 e,
Doping region 54 e,
Base region 56 e , and
Emitter region 58 e.
The substrate trench 12 e and the isolating trench 48 e have the same depth of e.g. 21 micrometers. By contrast, the auxiliary trench 46 e is made deeper, e.g. by more than three micrometers, in comparison with the substrate trench 12 e or isolating trench 48 e . The trench bottom of the auxiliary trench 52 e is situated more deeply than that interface of the doping region 14 e which is furthest away from the surface 30 e , for example by more than one micrometer, see overhang dimension U.
The auxiliary trench 46 e preferably adjoins the doping region 14 e . The auxiliary trench 46 e is preferably arranged in such a way that the doping region 14 e is completely enclosed laterally by the auxiliary trench 46 e . In another exemplary embodiment, the auxiliary trench 46 e subdivides the doping region 14 e into an inner region, which is electrically conductively connected to the collector connection 40 e , and into an outer doping region, which is electrically insulated from the inner doping region and does not belong to a component.
The auxiliary trench 46 e is not surrounded by a doping region introduced with the aid of the auxiliary trench 46 e . A trench intermediate region 98 between the auxiliary trench 46 e and the isolating trench 48 e was heavily n-doped in its entirety, for example by an implantation with subsequent outdiffusion. The distance between the auxiliary trench 46 e and the isolating trench 48 e is e.g. less than five micrometers or even less than three micrometers. Despite a diffusion depth of more than ten micrometers, the lateral diffusion during the doping of the trench intermediate region 98 is effectively delimited by the auxiliary trench 46 e and the isolating trench 48 e , thereby likewise giving rise to a transistor which requires only a small chip area and is nevertheless suitable for switching voltages of greater than 40 volts.
In other exemplary embodiments, the isolating trench 48 , 48 c , 48 d , 148 or 48 e is embodied in a shortened manner, so that it does not reach as far as the buried doping region 14 , 14 c , 14 d , 114 or 14 e , respectively, see dashed lines 170 to 178 . By way of example, the distance between the trench bottom of the isolating trench and the buried doping region is greater than one micrometer or greater than three micrometers. The breakdown voltage U CE of the transistor T 1 , T 3 , T 5 , T 8 or the breakdown voltage Ups of the transistor T 6 is thereby reduced. By way of example, the transistor T 1 , given a shortened isolating trench 48 , can be used as an ESD protection element for the transistor T 2 with an unshortened isolating trench 48 b if the isolating trench 48 b has the depth illustrated in FIG. 1 , that is to say reaches as far as the buried doping region 16 . The breakdown voltage of the ESD protection element can be set by way of the distance between the trench bottom of the isolating trench 48 and the surface 30 , see arrow 180 in FIG. 1 . Particularly in the case of a bipolar transistor, an ESD protection effect can be achieved even if, in the transistor to be protected, the isolating trench is shortened only in one section.
In other exemplary embodiments, field effect transistors constructed like the field effect transistor T 6 are used instead of the bipolar transistors T 1 , T 2 , T 3 , T 5 and T 8 elucidated in FIGS. 1 , 2 , 3 and 5 .
To summarize, it holds true that a vertical drift path that saves chip area arises as a result of the introduction of the isolating trench. The drift path runs firstly into the depth along the isolating trench and then on the other side of the isolating trench vertically to the surface along the isolating trench. The required chip area can thereby be drastically reduced compared with transistors with a lateral drift path.
Moreover, the possibility is afforded of setting, by way of the depth of the trench, the collector-emitter breakdown voltage U CE in the case of bipolar transistors or the drain-source breakdown voltage U DS in the case of MOS transistors (metal oxide semiconductor) in a targeted manner in conjunction with laterally unchanged dimensions.
The doping of the trench walls for the collector connection or drain connection and also for the substrate connection may be effected e.g. by implantation with subsequent outdiffusion or by coating. The trenches are etched e.g. by means of a trench etching process, e.g. in dry-chemical fashion.
The isolating trench, the auxiliary trench and, if appropriate, also the substrate trench are produced simultaneously in one exemplary embodiment. Different depths can also be achieved during simultaneous etching if different trench widths are chosen. At least one of the following steps is also performed simultaneously and thus in a simple manner: filling of the trenches of the two or three types of trench, doping of the sidewalls of an auxiliary trench and of a substrate trench.
As a person skilled in the art will readily appreciate, the above description is meant as an illustration of implementation of the principles this invention. This description is not intended to limit the scope or application of this invention in that the invention is susceptible to modification, variation and change, without departing from the spirit of this invention, as defined in the following claims.
|
Integrated transistor and method for the production is disclosed. An explanation is given of, inter alia, a transistor having an electrically insulating isolating trench extending from a main area in the direction of a connection region remote from the main area. Moreover, the transistor contains an auxiliary trench extending from the main area as far as the connection region remote from the main area. The transistor requires a small chip area and has outstanding electrical properties.
| 7
|
RELATED APPLICATIONS
[0001] This Application claims priority of U.S. Provisional Patent Application No. 61/472,590, filed on Apr. 6, 2011, and entitled “Method and Apparatus for Planting Raspberries, Blackberries, and other plants in the Rubus Genus,” which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention relates generally to a method of planting, and more specifically to a method of planting root material from suckering or runner-producing plants, for example, plants of the genus Rubus.
[0003] The disclosed method and apparatus relates generally to the planting of raspberry, blackberry and other species and hybrids in the Rubus genus, as well as asparagus, strawberries, or other suitable plants, and more specifically to methods of planting suckering plants, or plants producing runners, where the plant develops from planting of root material, as opposed to seeds, whole plants, or other planting methods. While the present invention has application to other species and hybrids, particularly in the Rubus genus, but among other suckering plants, as well as those producing runners, because of the broad application of the present application to raspberries in particular, the term “raspberries” will be used in this disclosure with the understanding that the claimed method and apparatus are applicable to those other plants, species and hybrids, notwithstanding the specific reference to raspberries.
[0004] Raspberries are a small-fruit crop produced by large and small scale farming operations. Initial investment for raspberry farming is high, primarily a result of the costs associated with land preparation, planting, and installation of trellis and irrigation systems. Raspberry cultivars readily produce new shoots from the roots, in a planting process called “suckering.” New plantings are established by taking advantage of the plants' ability to produce these suckers. As the plants go dormant in the fall they are harvested and the harvested roots are used to produce subsequent plantings. Future planting can be established using the roots only or by using a complete plant consisting of the roots, the crown and a portion of a stem. In either style of planting, (root only or root, crown & stem), large amounts of hand labor are expended to sort, clean, package, warehouse and replant the root material. Of these, the planting process consumes the largest amount of labor.
[0005] The current state of the art for replanting raspberry roots consists of the following operations: (1) preparing the harvested crop for cold storage; (2) cleaning, sorting and packaging; and (3) prior to planting, preparing the fields to receive the roots. This last step involves multiple operations using specialized ground-working equipment to create a defined bed top with longitudinal grooves in the surface of the bed-top. These grooves are designed to receive the root plantings.
[0006] Once the bed has been prepared, the plants are removed from cold storage and transported to the field immediately prior to planting. The roots are unpacked and weighed into totes that are then placed along the bed top at spacings which will yield the desired plant density. Laborers then separate the bunches of roots and lay them by hand into the grooves atop the bed. Finally, specialized ground-working equipment is used to cover the roots with an even layer of soil. It should be mentioned that the previously described process is more art than science. Many variables can affect the quality and success of the finished plantings, such as soil and weather conditions, and the availability of skilled laborers to perform the planting and tractor work. A few acres planted in this fashion create a stressful fast paced operation that must be overseen by a skilled supervisor to insure that the work is done correctly. Large plantings of 100 acres or greater are even more problematic and are labor intensive undertakings. Management, logistical and labor costs are extremely high, cumulatively requiring 100+ man-hours per acre planted.
SUMMARY OF THE INVENTION
[0007] One aspect of the present invention provides a device for producing a root rope. The device includes a carrier line suspended above a transport path for suspending a carrier line thereabove, and on which root material is deposited. A winding apparatus receives the carrier line and also receives at least one wrapping material. The winding apparatus uses a winding motion to wrap the wrapping material around the root material and carrier line, securing the root material to the carrier line and creating the “root rope.” A reel receives the root rope from the winding apparatus, the reel using a rotating motion to wrap the root rope around the reel.
[0008] In another aspect of the invention, the winding apparatus is a rotating drum that includes a funnel adapted to receive the carrier line and wrapping material, the rotation of the rotating drum causing the wrapping material in the funnel to wrap around the root material and carrier line to create the root rope.
[0009] In another aspect of the invention, the funnel includes two openings, one having a larger diameter than the other. The carrier line and root material is received into the larger opening of the funnel, while the root rope is dispensed from the smaller opening of the funnel.
[0010] In another aspect of the invention, the device also includes a drive wheel assembly that engages the winding apparatus, a rotating motion of the drive wheel assembly translating to rotation of the winding apparatus.
[0011] In still another aspect of the invention, the device includes a drive wheel assembly engaging a rotating drum, a rotating motion of the drive wheel assembly translating to rotation of rotating drum.
[0012] In another aspect of the invention, the device further includes a conveyor that defines a transport path for transporting root material along a transport path. The carrier line is suspended above the conveyor.
[0013] In another aspect of the invention, the device further includes at least one pulley in communication with the exit of the funnel. The pulley is adapted to receive the completed root rope from the funnel.
[0014] In another aspect of the invention, the pulley is in electronic communication with a controller, the controller adapted to regulate the speed of the reel.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 shows a perspective view of one embodiment of a conveyor and winding apparatus of the present invention.
[0016] FIG. 2 shows a side view of the conveyor and winding apparatus shown in FIG. 1 .
[0017] FIG. 3 shows a top view of the conveyor and winding apparatus shown in FIG. 1 .
[0018] FIG. 4 shows a top view of the conveyor shown in FIG. 4 .
[0019] FIG. 5 shows a side view of the conveyor shown in FIG. 4 .
[0020] FIG. 6 shows a perspective view of one embodiment of a winding apparatus of the present invention, viewed from the side into which the carrier line and attached root material are fed into the apparatus (henceforth, the “front”).
[0021] FIG. 7 shows a perspective view of one embodiment of a winding apparatus, viewed from the side from which completed root rope is dispensed (henceforth, the “rear”).
[0022] FIG. 8 shows a front view of one embodiment of a winding apparatus of the present invention.
[0023] FIG. 9 shows a side view of one embodiment of a winding apparatus of the present invention.
[0024] FIG. 10 shows a sectional view of one embodiment of a winding apparatus of the present invention.
[0025] FIG. 11 shows a front perspective view of one embodiment of a funnel that is utilized in one embodiment of the winding apparatus of the present invention.
[0026] FIG. 12 shows a rear perspective view of an embodiment of a funnel that is utilized in an embodiment of the winding apparatus.
[0027] FIG. 13 is a front view of the funnel depicted in FIG. 11 .
[0028] FIG. 14 is a side view of the funnel depicted in FIG. 11 .
[0029] FIG. 15 is a sectional view of the funnel shown in FIG. 11 .
[0030] FIG. 16 shows one embodiment of a reeling apparatus of the present invention which may be utilized with the present invention, the reeling apparatus including a guide assembly.
[0031] FIG. 17 shows an alternative embodiment of a reeling apparatus of the present invention.
[0032] FIG. 18 shows the relative disposition of a conveyor, winding apparatus, and reeling apparatus in one embodiment of the present invention.
[0033] FIG. 19 shows one embodiment of a root rope constructed in accordance with the teachings of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0034] Embodiments of the presently disclosed method and apparatus reduce costs and time associated with the preparation of plant beds and planting raspberry plants or other plants producing suckers, runners, and the like. The planting methodologies developed through use of this invention have application across the full spectrum of plant and fruit production, including commercial growers, nursery operations, and retail or wholesale outlets which sell plants to the hobby farm and the gardening/home improvement market. While the discussion below refers specifically to raspberries, it is contemplated that the principles of the present invention are applicable to any suitable plant.
[0035] Due to the fibrous nature of raspberry roots it is possible to weave the roots into a “rope” configuration, where the roots are preferably disposed onto a carrier line. The carrier line and attached roots are fed through a winding apparatus which wraps one or more wrapping members around the roots/carrier line, to form the rope configuration. The carrier line and wrapping member(s) are preferably fabricated from organic materials, (e.g., sisal, jute and bamboo) which will breakdown quickly once placed in the microbial soil environment so as not to impede the harvest process later in the season.
[0036] The roping machine apparatus utilized in the present invention includes a feed conveyor, a winding apparatus for winding wrapping material around the roots, and a reeling apparatus for winding the root rope onto a reel. The feed conveyor and winding apparatus may be synchronized together such that the conveyor and winding apparatus are in operation at the same time. The reeling apparatus takes up root rope as it is dispensed from the winding apparatus, with slight tension maintained on the root rope. Root rope is guided onto the reel for uniform distribution on the reel. Once wound on a reel, the root rope is placed into cold storage until ready to be planted.
[0037] The feed conveyor will typically be placed alongside a work surface containing root material, either fresh from the field, or taken from cold storage. The carrier line is preferably axially disposed above the feed conveyor, such that workers may manually place root material on the carrier line as it passes along above the conveyor. An acceptable size for the feed conveyor is six inches wide and twelve feet long, which allows provides sufficient space for workers to attach root material to the carrier line. Although in the embodiments of the invention described herein the root material is preferably hand-disposed onto a carrier line, it is contemplated that automated methods of disposing the root material onto the carrier line may be utilized. Further, in some embodiments of the invention, the carrier line may be omitted, with the root material being contained within the wrapping material without first being disposed onto a carrier.
[0038] The carrier line and attached root material are fed into the winding apparatus. As the carrier line and the root material attached to the carrier line are fed through the winding apparatus, wrapping material (the “wrapping twine”) is wrapped around the carrier line and root material to secure the root material, forming the root rope. One embodiment of the winding apparatus includes a winding drum having a center axial opening, a support frame, rotation means, a wrapping material source for providing the wrapping material, and rotation means for rotating the winding drum. The root rope is axially dispensed from the winding apparatus and spooled onto a reel attached to the reeling apparatus, with the root rope guided onto the reel. Full reels are transported to cold storage, where the root rope is stored until required for planting.
[0039] When required for planting, the rope storage reels are attached to bedshaping equipment modified to accept the rope storage reels. The rope is fed into the bed by being spooled off of the storage reel, and guided into the proper bed location by an adjustable injection tool. Correct density and correct plant location are controlled respectively by using the proper root mass density during the roping process, and proper placement of the rope during the bedshaping process. At harvest, the root from the plants are reclaimed and the process repeated.
[0040] In utilizing the method disclosed herein, substantial savings will be realized from the reduction in the size of the planting crew. The utilization of the root rope eliminates the manual labor steps of sorting, separating, and planting the root material.
[0041] FIGS. 1 through 19 depict exemplary embodiments of the present invention, or of various components thereof. FIGS. 1 through 5 depict an embodiment of a feed conveyor 10 which feeds into winding apparatus 12 in some embodiments of the present invention. FIG. 1 , for example, shows a perspective view of one embodiment of a conveyor and winding apparatus of the present invention. A carrier line supply, such as spool 14 may provide carrier line 16 (not shown), which is preferably suspended above a transport path defined by continuous belt 18 . Root material is preferably hand placed on carrier line 16 , and the combination of root material and carrier line 16 is fed into the winding apparatus 12 . FIG. 2 illustrates a side view of the conveyor 10 and winding apparatus 12 of FIG. 1 . FIG. 3 provides a top view of the same, while FIG. 4 provides a bottom view of conveyor 10 , alone. FIG. 5 is a side view of conveyor 10 .
[0042] As best shown in FIGS. 2 and 5 , feed conveyor 10 comprises a continuous belt 18 which extends between idler roller 19 and is powered by a drive roller 21 , which is driven by a motor 23 . A work surface, such as a table, counter, or the like (not shown), is preferably disposed adjacent to feed conveyor 10 , where root material is placed on the work surface for easy access by workers, who deposit the root material onto the carrier line 16 .
[0043] Exemplary embodiments of winding apparatus 12 are shown in greater detail in FIGS. 6 through 10 . As shown in FIG. 6 , winding apparatus 12 preferably includes a drive motor 20 which is mechanically linked to a drive wheel assembly 22 . Drive wheel assembly 22 rotates drum 24 , which is cradled within frame 26 . As seen in FIG. 7 , frame 26 comprises lower idler wheel assembly 28 and upper idler wheel assembly 30 , both which retain and guide drive wheel assembly 22 within frame 26 . Lower idler wheel assembly 28 may be located on the opposite side of frame 26 from drive wheel assembly 22 . Upper idler wheel assembly 30 may be disposed on a pivoting arm assembly 32 which is biased downwardly by tension member 34 . Winding apparatus 12 further preferably includes wrapping material spools 36 which provide wrapping material to the root rope as the drum 24 is rotated.
[0044] FIG. 8 shows a side view of winding apparatus 12 , and the relative positions of upper idler wheel assembly 30 , lower idler wheel assembly 28 , and drive wheel assembly 22 in this embodiment of the invention are clearly shown. It should be noted, however, that any suitable means of rotating drum 24 may be employed. FIG. 9 provides a side view of the same embodiment of winding apparatus 12 shown in FIG. 8 .
[0045] As shown in FIG. 10 , drum 24 preferably comprises a funnel member 38 , into which the combination of root material and carrier line 16 are drawn, entering the larger diameter opening. As root material 82 and carrier line 16 are drawn into funnel member 38 , wrapping material 40 (not shown) is applied by rotation of drum 24 . Wrapping material 40 is preferably in the form of two strands of material wound onto or around the root material 82 and carrier line 16 from opposing directions. The wrapping material 40 preferably passes through tension eyelets 45 , which guide the wrapping material 40 and maintain the required tension in the wrapping material. Finished root rope 44 is dispensed from the smaller diameter opening of funnel member 38 as shown in FIG. 14 . Wrapping material 40 is preferably spooled off of wrapping spine spools 36 as the drum 24 rotates. Tension of the completed root rope 44 is preferably regulated as the rope emerges from funnel 38 . Root rope 44 preferably passes through a series of pulleys 84 , 86 , and 88 , that serve to regulate the tension of root rope 40 and to provide feedback to reel 52 if the tension is too great or not great enough. Pulley 86 is preferably the load cell that measures the tension on root rope 44 . Feedback is provided to a motor controller that adjusts the rotational speed of reel 52 based on the measured tension of root rope 44 . If the tension of root rope 44 is too low, the rate of rotation of reel 52 is increased. Conversely, if the measured tension of root rope 44 is too high, the rate of rotation of reel 52 decreases.
[0046] While it is preferred that pulleys 84 , 86 , and 88 are used to measure, regulate, and adjust the tension of root rope 44 , it is contemplated that the present device may be utilized without these pulleys. A user of the present device may seek to maintain a more or less constant tension of root rope 44 solely through a set rotational speed of reel 52 , and when tension has to be adjusted the user may, for example, adjust the rotational speed of reel 52 based on manual observation of root rope 44 as it leaves funnel 38 .
[0047] FIGS. 11 through 15 show an exemplary embodiment of a funnel member.
Example
Funnel Member
[0048] An exemplary embodiment of funnel member 38 of the present invention is now described. It is to be understood that the dimensions of exemplary funnel member 38 provided here are exemplary and provided for purposes of illustration, and should not be considered limiting. Any suitable size of shape of funnel member 38 may be used.
[0049] An exemplary funnel member 38 , as shown in FIGS. 11 through 15 , includes a generally cylindrical body 68 that is about eight inches in length. Flanges 64 and 66 of about one inch in width each are provided at either end of funnel member 38 . Thus, the overall length of exemplary funnel member 38 is about ten inches. Openings are defined at either end of the funnel member 38 . At one end, a smaller opening is defined, preferably being about one inch in diameter. At the other end of funnel member 38 , a larger opening is defined, the larger opening preferably being about six inches in diameter. Interior walls 60 and 62 , shown in FIG. 15 , extend between the smaller opening and the larger opening, the interior walls preferably slanting at about an 11.3° angle 70 from an imaginary longitudinal axis 72 drawn through the center of funnel member 38 and extending across the length thereof. Flange 64 at the end of funnel member 38 having the larger opening preferably extends slightly beyond body 68 , giving that end of funnel member 38 an overall diameter of about seven and a half inches. Flange 66 at the end of funnel member 38 having the smaller opening is preferably set in from the edges of body 68 , giving that end of funnel member 38 a diameter of about four and a half inches. It is contemplated that the dimensions provided herein apply to one exemplary embodiment of funnel member 38 , and that any suitable size or shape of funnel member 38 may be used without departing from the spirit or scope of the present invention.
[0050] Once the finished root rope 44 is dispensed from the winding apparatus 12 , it is preferably pulled by a reeling apparatus 50 . Exemplary embodiments of a reeling apparatus are depicted in FIGS. 16 and 17 . Reeling apparatus 50 preferably includes a reel 52 which is suspended between a locking arm 54 and a support column 60 . The reeling apparatus 50 comprises a motor 58 (either electric or hydraulic) which rotates reel 52 to take up finished root rope 44 (not shown) dispensed from the winding apparatus 12 . A slight tension is maintained on the finished root rope. Some embodiments of reeling apparatus 50 comprise a guide assembly 56 which guides finished root rope 44 onto the reel 52 by laterally traversing back and forth along the axial length of the reel such that the rope is evenly wound across the width of the reel. An exemplary embodiment of a reeling apparatus 50 having a guide assembly 56 is shown in FIG. 16 .
[0051] FIG. 18 depicts the relative disposition of components of an exemplary root rope assembly and reeling system of the present invention. As shown in the figure, conveyor 10 is preferably located in proximity to winding apparatus 12 , which winds the wrapping material around the root material and carrier line to form a completed root rope. Reeling apparatus 50 is preferably further removed from conveyor 10 and winding apparatus 12 and maintains a constant tension on the finished root rope as it is being reeled. It is contemplated, however, that any suitable disposition of the various components of the present invention may be employed. FIG. 18 also shows an exemplary shield 90 that may be associated with some embodiments of the present invention. Shield 90 encloses a space around winding apparatus 12 , ensuring that the space is kept free of debris and also preventing harm to workers and others in the vicinity of winding apparatus 12 who may be harmed by the rotational movement thereof.
[0052] FIG. 19 shows an exemplary embodiment of a root rope 44 constructed in accordance with the teachings of the present invention. The root rope includes a carrier line 16 and root material 82 disposed along carrier line 16 . At least one wrapping line or length of wrapping material 40 is also included. A second wrapping material 41 is also preferably provided, though it is contemplated that a single wrapping material, or more than two wrapping materials, may be used so long as root material 82 is secured to carrier line 16 .
[0053] Carrier line 16 and wrapping materials 40 and 41 are preferably produced from organic materials such as jute, sisal, bamboo, or combinations of these. It should be noted that the first wrapping material 40 and the second wrapping material 41 may be composed of the same material. The use of two element numbers herein to refer to two separate lengths of wrapping material does not necessarily indicate different composition, though wrapping materials of differing composition may be used if desired.
[0054] While the above is a description of various embodiments of the present invention, further modifications may be employed without departing from the spirit and scope of the present invention. It is contemplated that such modifications will be readily apparent to those of ordinary skill in the art upon reading this disclosure. Thus the scope of the invention should not be limited according to these factors, but according to the claims to be filed in the forthcoming utility application.
[0055] Having thus described the preferred embodiment of the invention, what is claimed as new and desired to be protected by Letters Patent includes the following:
|
A device for producing a root rope includes a transport path for suspending a carrier line thereabove, root material being deposited on the carrier line. A winding apparatus receives the carrier line and also receives at least one wrapping material. The winding apparatus uses a winding motion to wrap the wrapping material around the root material and carrier line, securing the root material to the carrier line and creating the “root rope.” A reel receives the root rope from the winding apparatus, the reel using a rotating motion to wrap the root rope around the reel.
| 3
|
REFERENCE TO RELATED APPLICATION
This application is directed to the utility aspects of the chair design disclosed in the copending design Patent Application, Ser. No. 665,730, filed Mar. 10, 1976.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to furniture and methods of furniture construction. More particularly, the present invention relates to a method of furniture manufacturing and an article of furniture, the method utilizing standardized unitized structural components, standardized fasteners and a geometrically balance assembly plan.
2. General Background and Prior Art
The construction of furniture and the like requires generally that materials be cut and/or formed to meet specifications prior to their assembly into a finished article of manufacture. Generally, the structural integrity of a given piece of furniture is insured by varying the configuration of individual structural components which form the final product. The cross-sectional dimensions of some members which receive greatest stress in use are generally larger than the dimensions of structural components which receive lesser stress. Additionally, variation in structural component configuration are necessary to give an aesthetically pleasing appearance to the final product to thereby enhance its saleability. Thus, when a particular article of furniture is manufactured, it is generally necessary to sacrifice efficiency and economy in order to achieve both an attractive and structurally worthy product. This sacrifice while producing perhaps a saleable item, usually results in an increase in price to the consuming public.
Patents have been issued for furniture construction methods and more specifically for the construction of chairs. Examples of two prior art devices which have been patented are provided by U.S. Pat. No. 1,813,020 issued to N. N. Brown on July 7, 1931 and U.S. Pat. No. 3,873,154 issued to R. E. Baker, Jr. on Mar. 25, 1975.
The present invention utilizes the uniform structural components in a balanced geometric assembly configuration which distributes stresses properly to all the members, thereby allowing individual components to be of a standard uniform and smaller size. The joints between members is a face-to-face pinned connection which allows the chair to be totally prefabricated before its final assembly which could be, for example, performed by the consumer himself. Since the individual structural components have a constant square cross-section, they can be drilled in manufacture without regard to orientation as to length or width. Likewise, once the individual component is predrilled for assembly, the final assembly requires a minimum amount of orientation of the member itself before assembly by the consumer.
Thus, the present invention lends itself to a total kit type operation whereby the manufacturer only provides individual structural components of a single uniform cross-section throughout their length, predrilled with necessary uniform diameter connection holes and a plurality of constant diameter binding fasteners to make a complete kit for assembling a chair. Other than these easily manufactured and economical components, only the balanced frame geometry and a set of assembly instructions is required.
GENERAL DISCUSSION OF THE PRESENT INVENTION
The present invention provides an attractive, comfortable, heavy load bearing, and efficient article of furniture utilizing a minimum volume/mass of standard materials and processing.
The present invention provides individual structural components which are standardized to a substantially identically cross sectional dimension with varying lengths for individual furniture articles. Each furniture article is constructed utilizing a balanced geometric assembly plan which properly distributes the load to the various structural components of the furniture article. The individual structural components are pin joined using standardized fasteners which are attached through the pin joints at pre-drilled holes which are sized so as to properly accomodate the standard fasteners. Each pinned joint where a given plurality of structural components is connected is oriented in such a manner as to form a rigid and structurally sound connection.
The joint connections are rigid structurally, but some joints additionally can pivot upon the removal of certain fasteners, allowing the furniture article to fold.
BRIEF DESCRIPTION OF THE DRAWINGS
For a further understanding of the nature and objects of the present invention, reference should be had to the following detailed description, taken in conjunction with the accompanying drawings, in which like parts are given like reference numerals and wherein:
FIG. 1 is a perspective, front view of the preferred embodiment of the furniture article of the present invention;
FIG. 2 is a perspective, rear view of the preferred embodiment of the furniture article of the present invention;
FIG. 3 is a perspective view of the article of furniture of FIG. 1 in a folded position;
FIG. 4 is a side view of the preferred embodiment of the article of furniture of the present invention illustrating an exemplary geometric assembly plan and having certain limited areas cut away to show the position of some of the fasteners; and
FIG. 5 is a partial, perspective view of the preferred embodiment of the article of furniture of the present invention illustrating a special pinned joint used in the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 illustrates the preferred embodiment of the article of furniture of the present invention comprised generally of a plurality of structural component members 10-17 which are connected at their end portions (as can best be seen in FIG. 1) by a plurality of fasteners 31. The preferred embodiment illustrated in FIG. 1 is a chair designated generally by the numeral 5. The seat portion of the chair designated by the numeral 25 can be of a strong but flexible type material such as canvas, leather, vinyl or the like. The back portion of the chair provides support by means of two, like flexible supports 20, 21.
Structural supports 10-17 are of a substantially identical cross-sectional dimension. In the preferred embodiment, structural supports 10-17 are provided with square cross-sections which can be for example, 11/2" by 11/2". A rectangular cross-section would also be suitable, as preferably a cross-section providing squared sides and right angular corners if desired. The cross-sectional dimension would be preferably uniform throughout the length of an individual structural support 10-17 which would then provide an easily manufactured and economical component 10-17. With this uniformity, a large number of structural components 10-17 could be premanufactured and later cut and pre-drilled with connection openings where necessary.
In the preferred embodiment, component members 10-17 can be of any rigid, structural yet economical material, such as for example, wood.
Since the structural component members 10-17 of the chair 5 will be utilized in different portions of the chair which will necessarily sustain differing stresses during use, the present invention provides that the chair be assembled using a balanced and supportive frame geometry. FIG. 4 illustrates an inventive example of such a workable frame geometry for the chair 5 which will assure a structurally sound and rigid piece of furniture that can withstand the stresses applied during use by the consumer. This feature is important since all the component members of the chair are manufactured of a substantially identical cross-sectional dimension, with members experiencing greatest stress being afford no greater structural integrity than other members of the chair. FIG. 4 represents a side view of chair 5 and illustrates the preferred geometric relationships between the support components 10-17. Although the particular angles shown have been found to be suitable and are preferred, a little variation of a few degrees is possible in the non-orthogonal joints, but the angles should at least be of the order of the angles illustrated (namely of the order of 100° and 80°.
As can best be seen in FIGS. 1 and 2, there is provided for chair 5 a base, a seat, a back portion, an arm rest portion and a front represented generally by the numerals 40, 42, 44, 46 and 48 respectively, in FIG. 2. Base 40, which can contact the floor or other support surface along its full length, forms an angle of 90° with front portion 48. An angle of 100°, for example, is formed between base 40 and back portion 44. Back portion 44 forms an angle of 90° with seat 42 and an exemplary angle of 100° with arm rest portion 46. Seat 42 additionally forms an exemplary angle of 80° with front portion 48. The side portions formed by elements 10, 11, 12 and 13 are parallel and form an angle of 90° with respect to the base section 40.
It can be seen by one skilled in the art by an inspection of FIG. 4 that the geometric configuration provided to the structural components 10-17 produces a rigid structure. However, the chair 5 can be folded by the removal of the pins 31 at the joints between upper arms 10 and front legs 11, the joints being designated by the numeral 50 in FIG. 4 illustrates the folded position of chair 5 after the removal of fasteners 31 from joint 50 on each side of the chair 5 respectively. A further collapsible feature of chair 5 can be utilized for storage by the removal of three cross-braces 14, 15 and 16. With the removal of these braces, the chair will then comprise two rigid sections connected together by the flexible seat portion 25 and back portions 20, 21 which can be collapsed and rolled together into a tight compact disposition for storage.
The exemplary frame geometry for chair 5 provides a proper distribution of forces allowing the chair 5 to be constructed with highly standardized construction parts while still maintaining the structural integrity of the chair itself. Thus, it can be seen that chair 5 could be manufactured with a minimum amount of labor and materials while still providing a structural sound and aesthetically pleasing unit for consumer use at a considerable savings in cost.
Fasteners 31, which can be for example nut and bolt type fasteners, are provided to make rigid pinned connections at the joints between the various component supports 10-17. FIG. 1 more particularly illustrates the construction of chair 5. Base portion 40 is provided with a pair of bottom braces 13 connected at the upper surfaces of their rear portions by lower cross-bar 14. Front legs 11 are connected to base 40 by means of fasteners 31 at the front tip portions 13A of bottom braces 13 and at the lower tip portion 11A of legs 11. It can be seen that the tip portions 13A of bottom braces 13 substantially align flush with the lower front bases 11A of legs 11. This results, because openings are provided in the end portions of all structural supports 10-17 which are substantially symmetrically placed about the cross-sectional axis of each support member 10-17.
Thus, as can be seen in FIG. 1, all the jointed connections which result in 90° angular connections will provide an aesthetically pleasing, smooth, face-to-face orthogonal joint. Note that the same connection formed by bottom braces 13 and legs 11 is achieved at the joints 50 of legs 11 and arms 10.
A like face-to-face, orthogonal connection is provided by the connection at the lower, rear cross-bar 14 and bottom braces 13. A like connection is formed at the joints of front, upper cross-bar 15 and seat stretcher members 17, as well as at the joints between seat stretcher members 17 and rear, upper cross-brace 16. In the former connection, it is highly desirable that the front cross-bar 15 is connected to the underside of the members 17 and inboard of the angled connection between the front legs 11 and the members 17.
FIG. 5 illustrates a three piece, partially orthogonal joint designated generally by the numeral 60, the joint represented in FIG. 5 illustrating the three-way joint 60 which is formed at the rear joints of seat structure member 17, rear, upper cross-bar 16 and rear leg 12. As can be seen by an examination of FIG. 5, rear, upper bar 16 is connected to seat stretcher member 17 by means of fastener 31A. Seat stretcher member 17 is then attached by fastener 31A to rear leg 12. Since the connection hole (not shown) at the end portion of each structural component is always symmetrically placed at about the centroidal axis of a given component, it can be seen that the junction of rear, upper cross-bar 16 and seat stretcher member 17 provides an orthogonal connection at joint 60 which places the outer face 17A of stretcher member 17 substantially flush with the side face 16B of rear, upper cross-bar 16. The orthogonal joint thus formed is both structurally sound and aesthetically pleasing. Additionally, the portion of the end face of cross-bar 16 preferably contacts and engages face-to-face the side surface of the rear leg 12.
The chair 5 of the present invention could be provided to the consumer in the form of a unassembled kit. Such a kit would greatly reduce the cost of the chair to the consumer with the individual consumer providing the labor necessary to assemble the chair into its final configuration. A kit form while used in many instances, lends itself especially to the present invention. This is a fact because the present invention provides component structural members which are highly unitized and easy to manufacture at a low cost. As has been more fully discussed, since each member is of a constant, square cross-sectional dimension and since constant diameter connecting holes and fasteners are utilized, a very minimal amount of manufacturing is in fact necessary. If a proper and well designed geometric assembly plan is provided to the individual, he can easily assemble the furniture article of the present invention in his spare time.
The following table provides a listing of parts which would be exemplary of a kit form which could be supplied to the consumer for assembly thereafter.
__________________________________________________________________________PARTS LISTDRAWING INDICATOR NO. PART DESCRIPTION QUANTITY__________________________________________________________________________12 Rear legs (31" × 1 1/2" × 1 2/2")11 Front legs (22 1/2" × 1 1/2" × 1 2/2")10 Arm Rests (22 1/2" × 1 1/2" × 1 2/2")15 Front Upper Cross-bar 1 (22 1/2" × 1 1/2" × 1 1/2")17 Stretcher bar (21 3/4" × 1 1/2" 2 × 1 1/2")14 Lower rear cross-bar 1 (22" × 1 1/2" × 1 1/2")16 Upper rear cross-bar 1 (22" × 1 1/2" × 1 1/2")13 Bottom Braces (22 1/2" × 1 1/2" × 1 2/2")31 1/4" diameter × 3" length 18 threaded hex head/cap nut- head bolts 1/4" diameter × 7/16" shaft tee nuts with 3 knobs, each flange. Split lock washers, 1/4". Flat washer, 1/4".20 Sewn canvas back (14.75 oz. or 1 greater weight/yard)25 Sewn canvas seat (14.75 oz. or 1 greater weight/yard)__________________________________________________________________________
As exemplary materials for construction, all metal parts (which would be fasteners 31) could be chromed or brass plated. The woods could be high density hard wood, having a soaked natural oil finish.
For aesthetics, the structural members 10-17 could be provided with bevels on the edges and on the end portions. For example, a 1/16" bevil on all edges could be provided throughout the length of a structural component 10-17, and a 3/8" bevil on the end portions of each structural component could be provided. In order to economize the manufacture, all holes would be drilled at a constant diameter, preferably 1/4" in order to correspondent with with a 1/4" diameter as given in the exemplary table above for fasteners 31. The dimensions as given in the exemplary table would be dimensions for sanded wood finishes.
It is noted that joints 60 and joints 50 are typical examples of face-to-face joints which could be utilized to manufacture several different types of furniture using structural components of substantially identical, square cross-sections, the square cross-sectional members forming face-to-face and in some cases orthogonal joints as is shown in the figures. Thus, in addition to chairs, the present method of furniture manufacture could be used to produce other supporting furniture such as for example, sofas, ottomans, tables, desks, wall units, and the like. An entire line of furniture could be manufactured utilizing the same identical cross-sectional dimensioned components, the same diameter fasteners, and the same face-to-face joint technology as is taught by the present invention.
Because many varying and different embodiments may be taught within the scope of the inventive concept herein taught, and because many modifications may be made in the embodiment herein detailed in accordance with the descriptive requirements of the law, it is to be understood that the details herein are to be interpreted as illustrative and not in a limiting sense.
|
An arm chair and its method of manufacture provides a plurality of standardized, build-up, structural components, the components being joined by means of pin joinings at the appropriate joints, the individual structural components predrilled to accommodate standardized fasteners of substantially identical diameter. The chair is constructed in a method which provides a balanced seating geometry to equally distribute stresses applied to the chair. Structural components are of substantially identical cross-sectional dimensions and of substantially identical material. The chair can be folded into a compact, space saving position.
| 0
|
TECHINICAL FIELD
[0001] The present invention is related to a method for measuring fluid medium velocities, and more concretely to a method and system for measuring flow layer velocities using correlation velocity measuring sonar.
PRIOR ART
[0002] At present, methods for measuring flow layer velocities using correlation velocity measuring sonar are summarized as follows.
[0003] (1) U.S. Pat. No. 5,315,562, titled “Correlation Sonar System” invented by S. E. Bradley et al. discloses correlation sonar used for measuring current profile and velocities of a vessel in water relative to the bottom. This invention includes the following four aspects:
[0004] (A) A complex signal is transmitted. The complex signal's autocorrelation function has two different peaks at delay τ=0 and τ=τ c . The previous technology of transmitting two pulses that may cause interferences between medium layers of the fluid is eliminated.
[0005] (B) A theoretical expression for sonar array temporal and spatial correlation function for fluid medium and bottom medium is introduced in series forms, wherein bessel function and Legendary function are included, and a simplified expression based on experiences is proposed and adopted for signal processing because of its simplicity
[0006] (C) Based on the maximum likelihood principle, by using the simplex method, the current velocities and the vessel's velocity relative to the bottom are derived by optimally fitting the theoretical and experimental sonar array time-spatial correlation functions.
[0007] (D) A matched filter approach is used for detecting the seabed echoes.
[0008] (2) U.S. Pat. No. 5,422,860, titled “Correlation Sonar System” invented by S. E. Bradley et al. discloses a method to generate correlation sonar signals. Pseudo random phase-coded signal, whose autocorrelation function has two different peaks at delay τ=0 and τ=τ c , is transmitted.
[0009] The methods for measuring current velocities has obvious shortcomings: (1) The theoretical expression for sonar array temporal and spatial correlation function is so complex that it is difficult to use in practice; but the simplified expression derived from experience does not have sufficient physical foundation. This is the most important technology of correlation velocity-measuring sonar system. (2) It is not the best method to fit the theoretical and experimental temporal and spatial correlation function by using simplex method based on the maximum likelihood principle. (3) It is also not the best method to use a velocity corresponding to the maximum value of the sonar array temporal and spatial correlation function as an initial value of velocity estimation.
SUMMARY OF THE INVENTION
[0010] The main objective of the invention is to provide a preferred theoretical fluid medium sonar array temporal and spatial correlation function for fitting with experimental data. Another objective of the invention is to improve the data processing method for data temporal and spatial correlation function.
[0011] In order to achieve the objectives mentioned above, the present invention provides a method for measuring flow layer velocities using correlation velocity measuring sonar, the method comprising steps of
[0012] (1) Select transmit code for acoustic pulses, whose autocorrelation has a peak at a non-zero time delay;
[0013] (2) According to the transmit code, transmit acoustic pulses into fluid medium, and receive echo signals backscattered by flow layers;
[0014] (3) Demodulate and filter the echo signals of flow layer, and calculate a data temporal and spatial correlation function matrix of flow layer;
[0015] (4) extract a data matrix for fitting from the data temporal and spatial correlation function matrix of flow layer derived from the step (3), wherein the data matrix for fitting is the data temporal and spatial correlation function matrix of flow layer, or is a localized data temporal and spatial correlation function matrix of flow layer, and the localized data temporal and spatial correlation function matrix of flow layer is derived from steps of
[0016] (a) operate absolute value of the data temporal and spatial correlation function matrix of flow layer to attain a data temporal and spatial correlation function absolute value matrix of flow layer, and elements of said data temporal and spatial correlation function absolute value matrix have a maximum value E Max ;
[0017] (b) set a threshold value χ, wherein 0<χ≦1, preferably 0.7<χ≦1, those elements in the absolute value matrix with numerical value less than χE Max is set to zero, those elements with numerical value equal to or larger than χE Max is retained, and the localized temporal and spatial correlation function absolute value matrix of the flow layer can be derived by operating all the elements;
[0018] (5) set a search range for the unknown parameter ensemble ={ V x , V y , σ vx , σ vy , γ}, wherein V x , V y are average values of relative velocities of flow layer in x, y directions respectively, σ vx , σ vy are standard deviation of velocities in x, y directions respectively, γ is width factor;
[0019] (6) fit the data matrix derived from the step (4) with a theoretical function in the search range of the unknown parameter ensemble ; the fitting algorithm uses a sequential quadratic programming method based on the maximum likelihood principle or on the nonlinear least square principle;
[0020] The theoretical function is
φ ( τ , ϑ , d ) = C { exp ( γβ θ ) - ζ 2 2 [ θ e 2 2 π 1 F 1 ( 2 ; 1 ; β θ ) - cos 2 ( α 3 - α 2 ) B 2 2 θ e 4 8 π 2 F 1 1 ( 3 ; 3 ; β θ ) ] }
where C is a constant, τ is time delay, d is the distance between receive elements of the sonar array, 1 F 1 (·) is Kummer function,
β θ = - β 2 2 θ e / 4 π ,
β 2 = ω 0 c ( ( τ V _ x + d x ) 2 + ( τ V _ y + d y ) 2 ) 1 / 2 , ξ 2 = ω 0 τ c ( σ vx 2 + θ vy 2 ) 1 / 2 ,
α 2 = tg - 1 τ V _ y + d y τ V x + d x , α 3 = tg - 1 σ vy σ yx , θ e 2 = 1 2 θ b 2 θ c 2 θ b 2 + θ c 2 ;
where ω 0 is the central frequency of the transmit signal, c is the velocity of sound, dx and dy are component of d in x and y direction respectively, and θ b and θ c are transmit beam width and receive beam width respectively;
[0021] (7) Cooperate the vessel's velocity relative to the bottom with average values of the relative velocities { V x , V y ,} obtained from the step (6) to calculate the absolute velocities of flow layer.
[0022] The steps (1)˜(7) can be repeated for the next measurement of flow layer velocities. When repeating the step (5), a previous measured relative velocity or an average value of multiple previous measured relative velocities is used as the initial value of the search range of the unknown parameter ensemble .
[0023] The present invention further provides a correlation velocity measuring sonar system including a sonar array ( 200 ) and an electronic subsystem, the electronic subsystem includes a computer ( 406 ), characterized in that the computer ( 406 ) comprises:
[0024] An initialization module for initializing software and hardware;
[0025] A signal coding module for selecting transmits code for acoustic pulse, whose autocorrelation has a peak value at a non-zero time delay;
[0026] a transmit/receive module for transmitting acoustic pulses into fluid medium, and receiving echo signals backscattered by flow layers;
[0027] A demodulation and filter module for demodulating and filtering the echo signals of flow layer received by the transmit/receive module;
[0028] A matrix calculation module for calculating data temporal and spatial correlation function matrix of flow layer according to the demodulated and filtered echo signals of the flow layer;
[0029] a matrix extraction module for extracting a data matrix for fitting from the data temporal and spatial correlation function matrix of flow layer derived from the matrix calculation module, wherein the data matrix for fitting from the matrix extraction module can be the data temporal and spatial correlation function matrix of flow layer, or a localized data temporal and spatial correlation function absolute value matrix of flow layer; when the localized data temporal and spatial correlation function absolute value matrix of flow layer is used as the data matrix for fitting, the matrix extraction module comprises:
[0030] an absolute value calculation unit for performing an absolute value operation on the data temporal and spatial correlation function matrix to attain a data temporal and spatial correlation -function absolute value matrix of the flow layer; and
[0031] a localization unit for selecting a maximum value E Max in the data temporal and spatial correlation function absolute value matrix, and setting a threshold value χ, wherein 0<χ≦1, and for setting those elements in the absolute value matrix with numerical value less than χE Max to zero and retaining those elements with numerical value equal to or larger than χE Max to obtain the localized temporal and spatial correlation function absolute matrix of the flow layer by operating all the elements;
[0032] a parameter module for storing the search range of the unknown parameter ensemble ={ V x , V y , σ vx , σ vy , γ}, wherein V x , V y are average values of relative velocities of flow layer in x, y directions respectively, σ vx , τ vy are standard deviation of velocities in x, y directions respectively, γ is width factor, wherein the initial value of the search range of the unknown parameter ensemble stored in the parameter module is a previous measured relative velocity or an average value of multiple previous measured relative velocities;
[0033] A fit module for fitting the data matrix derived from the matrix extraction module with a theoretical function in the search range of the unknown parameter ensemble ; wherein the fit module is a calculation module using a sequential quadratic programming method based on the maximum likelihood principle or on the nonlinear least square principle, the theoretical function being
φ ( τ , ϑ , d ) = C { exp ( γβ θ ) - ζ 2 2 [ θ e 2 2 π 1 F 1 ( 2 ; 1 ; β θ ) - cos 2 ( α 3 - α 2 ) B 2 2 θ e 4 8 π 2 F 1 1 ( 3 ; 3 ; β θ ) ] }
wherein, C is a constant, τ is delay, d is the distance between receive elements of the sonar array, 1 F 1 (·) is Kummer function,
β θ = - β 2 2 θ e / 4 π ,
β 2 = ω 0 c ( ( τ V _ x + d x ) 2 + ( τ V _ y + d y ) 2 ) 1 / 2 , ξ 2 = ω 0 τ c ( σ vx 2 + θ vy 2 ) 1 / 2 ,
α 2 = tg - 1 τ V _ y + d y τ V x + d x , α 3 = tg - 1 σ vy σ yx , θ e 2 = 1 2 θ b 2 θ c 2 θ b 2 + θ c 2 ;
wherein ω 0 is the central frequency of the transmit signal, c is the velocity of sound, dx and dy are components of d in x direction and y direction respectively, θ b and θ c are transmit beam width and receive beam width respectively; and
[0034] A velocity storage module for storing average values of the relative velocities { V x , V y ,} derived from fitting results of the fit module.
[0035] The present invention has the following advantages:
[0036] (1) When measuring velocities of flow layer, the theoretical sonar array temporal and spatial correlation function provided by the present invention is applicable not only to far field region, i.e. planar wave region, but also to Fraunhofer region, i.e. spherical wave region. However, the conventional acoustic correlation velocity measuring theory is only applicable to the far field region, so that it is difficult to attain good data in a relative large short-distance scope. The theory of the invention makes the short-distance scope less. Moreover, the fluid medium sonar array temporal and spatial correlation function of the invention is succinctly expressed by Kummer function and in good coincidence with experiments. The conventional theory is expressed in series forms of Bessel function and legendary function, which is inconvenient in use, or is expressed in experiential formulas with no sufficient physical foundation.
[0037] (2) The fitting algorithm of the invention uses a sequential quadratic programming method based on the maximum likelihood principle, or on the nonlinear least square principle to fit measured data with the theoretical sonar array temporal and spatial correlation function to attain velocities. Compared with the conventional simplex method, the method of the present invention has faster convergence rate, higher measurement accuracy. Especially, velocity estimation based on nonlinear least square principle, compared with the maximum likelihood principle, has better robustness and small calculation load. In particular to the correlation velocity measuring sonar in actual situation, environmental noises may be uneven in space, the amplitudes and phrases of the receive elements of the sonar array may disaccord from each other. They will affect the least square principle less than the maximum likelihood principle.
[0038] (3) The present invention uses the method to calculate absolute value of and to localize the data fluid medium temporal and spatial correlation function matrix and uses regions with large amplitudes in the matrix to calculate velocities. The absolute value of the correlation function is only related with the average horizontal velocities V x and V y , and regions with low signal noise ratio are eliminated. These two signal processing measures raise the measurement accuracy.
[0039] (4) The invention uses the average value of measured velocities from the N-m th time to the N th time as the initial value of estimated velocity at the N+1 th time, which raises calculation speed and reduces hardware cost.
BRIEF DESCRIPTION OF THE DRAWINGS
[0040] FIG. 1 is a schematic view of a correlation velocity measuring sonar system in operation;
[0041] FIG. 2 is a schematic view of the structure of the correlation velocity-measuring sonar system;
[0042] FIG. 3 is a flow chart of the software for the correlation velocity-measuring sonar system;
[0043] FIG. 4 is a detailed flow chart of the step 609 in FIG. 3 ; and
[0044] FIG. 5 is a diagram of measured velocity comparison between the correlation velocity measuring sonar system (ACCP) and RDI phrased-array acoustic Doppler current profiler (PAADCP) at an area 150 m deep; wherein FIG. 5 a illustrates measured velocity amplitudes 701 and 703 by these two equipments, and FIG. 5 b illustrates measured velocity directions 702 and 704 by these two equipments.
[0045] Numerals:
[0046] Vessel 100 sonar array 200 underwater electronic subsystem 300
[0047] Dry end 400 terminal 500
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0048] The present invention will be described in detail hereinafter in conjunction with the drawings and embodiments.
[0049] With reference to FIG. 1 , a correlation velocity measuring sonar system in accordance with the present invention, used for measuring flow layer velocities, is installed on a vessel ( 100 ). The correlation velocity measuring sonar system generally includes a sonar array ( 200 ) and an electronic subsystem. The electronic subsystem includes an underwater electronic subsystem ( 300 ), a dry end ( 400 ) and a terminal ( 500 ). The sonar array ( 200 ) and underwater electronic subsystem ( 300 ) are installed beneath the water, and the dry end ( 400 ) and terminal ( 500 ) are installed above the water. A transmit transducer array of the sonar array ( 200 ) transmits acoustic pulses into the water. The acoustic pulse 102 in one pulse width spreads in the water and encounters the seabed in a ring ( 103 ) so as to generate a flow echo and a bottom echo. The echoes are received by the receive transducer array of the sonar array ( 200 ), and processed by the electronic subsystem to calculate the velocity of each flow layer.
[0050] The detailed structure of the correlation velocity measuring sonar system composed of the sonar array ( 200 ) and electronic subsystem is illustrated in FIG. 2 . The sonar array ( 200 ) includes receive transducers ( 203 ); transmit transducers ( 202 ), and homeostatic transducers ( 201 ). The receive transducers ( 203 ) and the homeostatic transducers ( 201 ) constitute the receive sonar array. The transmit transducers ( 203 ) and the homeostatic transducers ( 201 ) constitute the transmit sonar array.
[0051] The underwater electronic subsystem ( 300 ) includes multi-channel preamplifiers ( 302 ) connected to the receive transducers ( 203 ) and the homeostatic transducers ( 201 ). Transmit and receive switches ( 301 ) are inter-connected with the preamplifiers ( 302 ) and the homeostatic transducers ( 201 ). The underwater electronic subsystem ( 300 ) also includes a temperature sensor ( 303 ), a water-leaking-detection sensor ( 304 ) and an attitude sensor ( 305 ), all connected to a sonar interface control board ( 407 ) in the dry end ( 400 ).
[0052] The dry end ( 400 ) includes a transmitter ( 401 ) connected to the transmit transducer ( 202 ), multi-channel receivers ( 402 ) connected to the preamplifiers ( 302 ), a multi-channel synchronous AD converter board ( 403 ) connected to the multi-channel receivers ( 402 ), and a DSP board ( 404 ) connected to the multi-channel synchronous AD converter board ( 403 ). The dry end ( 400 ) also includes a computer ( 406 ) connected to the DSP board ( 404 ) and multi-channel synchronous AD converter board ( 403 ) respectively by a data/control bus ( 405 ). The dry end ( 400 ) also includes the sonar interface control board ( 407 ) connected to the multi-channel receivers ( 402 ), the transmitter ( 401 ), the DSP board ( 404 ) and the computer ( 406 ) respectively, and an AC/DC power supply ( 408 ) connected to the sonar interface control board ( 407 ), the multi-channel receivers ( 402 ), the transmitter ( 401 ), the data/control bus ( 405 ), the temperature sensor ( 303 ), the water-leaking-detection sensor ( 304 ) and the attitude sensor ( 305 ) respectively. The dry end ( 400 ) also includes a GPS receiver ( 409 ) and a GYRO ( 410 ) connected to the computer ( 406 ).
[0053] The terminal ( 500 ) includes a terminal computer ( 502 ) connected to the computer ( 406 ) by a network ( 501 ).
[0054] A special velocity measuring program is stored in the computer ( 406 ). The program includes an initialization module, signal coding module, transmit/receive module, demodulation and filter module, matrix calculation module, matrix extraction module, parameter module, fit module and velocity storage module. The program is executed according to steps illustrated in FIG. 3 .
[0055] The step ( 601 ) is the start, in which the terminal computer ( 502 ) sends instructions to the computer ( 406 ) by the network ( 501 ), and then the program in the computer ( 406 ) starts to enable the sonar system in an operating state. In the steps ( 602 ) and ( 603 ), the initialization module initializes software and system hardware. In the step ( 605 ), according to the layer thickness and the range of the flow velocities, signal coding module selects transmit code, whose autocorrelation has a peak value at a non-zero time delay. In the step ( 606 ), transmit/receive module sends the instructions of the computer ( 406 ) through the data/control bus ( 405 ) to enable the DSP board ( 404 ) to send transmit signals to the transmitter ( 401 ), and through the transmit and receiver switches ( 301 ) to drive the homeostatic transducers ( 201 ) and the transmit transducers ( 202 ) to send acoustic pulses into the fluid medium. In the step ( 607 ), transmit/receive module controls the receive transducers ( 203 ) and homeostatic transducers ( 201 ) to receive echoes backscattered by the fluid medium, and to feed the echoes to the multi-channel receivers ( 402 ) through the preamplifiers ( 302 ) and then to the DSP board ( 404 ) through the multi-channel synchronous AD converter board ( 403 ). In the step ( 608 ), the demodulation module controls the DSP board ( 404 ) to demodulate and filter the received echoes.
[0056] In the step ( 609 ), matrix calculation module calculates data temporal and spatial correlation function matrix of the flow layer according to the demodulated and filtered echo signals.
[0057] In the step ( 610 ), the matrix extraction module extracts a data matrix for fitting from the data temporal and spatial correlation function matrix of the flow layer. This data matrix will be fitted with a theoretical function provided by the present invention in the step ( 612 ). In detail, during the step ( 610 ), the matrix extraction module may directly use the data temporal and spatial correlation function matrix derived from the step ( 609 ) as the data matrix for fitting, or use the further processed data temporal and spatial correlation function matrix derived from the step ( 609 ) as the data matrix for fitting. In the latter, matrix extraction module includes an absolute value calculation unit and a localization unit, for which a detailed flow charts, is illustrated in FIG. 4 . With reference to FIG. 4 , the absolute value calculation unit performs an absolute value operation on the data temporal and spatial correlation function to attain an absolute value matrix of the data temporal and spatial correlation function. Then, the localization unit performs a localization operation on the absolute value matrix. Finally, the localized matrix is used as the data matrix for fitting. The localization means selecting the maximum value E Max from the data temporal and spatial correlation function absolute value matrix, and setting a threshold value χ, wherein 0<χ≦1. Then, those elements in the absolute value matrix with numerical value less than χE Max is set to zero, those elements with numerical value equal to or larger than χE Max is retained. The localized temporal and spatial correlation function absolute matrix of the flow layer can be derived by performing the operation on all the elements. The localization operation only chooses the elements larger than or equal to χE Max , i.e. chooses the region with large signal noise ratio and eliminates the region with low signal noise ratio, thus further simplifying calculation and improving measurement accuracy. In practice, the threshold value χ is preferred between 0.7 and 1.
[0058] After the data matrix for fitting is obtained, the fitting operation of the data matrix and theoretical function matrix is performed to attain velocity of each flow layer relative to the vessel from the fitting results. In accordance with the present invention, a theoretical fluid medium sonar array temporal and spatial correlation function is expressed as follow
Rs ( τ , ϑ , d ) = C ( exp { j f ( V z ) } ) { exp ( γβ θ ) - ζ 2 2 [ θ e 2 2 π 1 F 1 ( 2 ; 1 ; β θ ) - cos 2 ( α 3 - α 2 ) B 2 2 θ e 4 8 π 2 F 1 1 ( 3 ; 3 ; β θ ) ] } ( 1 )
[0059] wherein C is a function of ƒ(V z ), ƒ is a certain function, V z is relative velocity of each flow layer in z direction, τ is time delay, d is distance between receive elements of the sonar array, 1 F 1 (·) is Kummer function,
β θ = - β 2 2 θ e / 4 π ,
β 2 = ω 0 c ( ( τ V _ x + d x ) 2 + ( τ V _ y + d y ) 2 ) 1 / 2 , ξ 2 = ω 0 τ c ( σ vx 2 + θ vy 2 ) 1 / 2 ,
α 2 = tg - 1 τ V _ y + d y τ V x + d x , α 3 = tg - 1 σ vy σ yx , θ e 2 = 1 2 θ b 2 θ c 2 θ b 2 + θ c 2 ;
wherein ω 0 is the central frequency of the transmit signal, c is the velocity of sound, d x and d y are components of d in x direction and y direction respectively, and θ b and θ c are transmit beam width and receive beam width respectively.
[0060] According to the equation (1), Rs(τ, , d) is related with V x , V y , V z . If the three-dimension velocities are all estimated together, the calculation is complex and the accuracy is low. After performing absolute value operation on the theoretical fluid medium sonar array temporal and spatial correlation function expressed in equation (1), an equation is expressed as follow:
φ ( τ , ϑ , d ) = R s ( τ , ϑ , d ) = C { exp ( γβ θ ) - ζ 2 2 [ θ e 2 2 π 1 F 1 ( 2 ; 1 ; β θ ) - cos 2 ( α 3 - α 2 ) B 2 2 θ e 4 8 π 2 F 1 1 ( 3 ; 3 ; β θ ) ] } ( 2 )
Where C is a constant. A matrix constructed by absolute values of the theoretical temporal and spatial correlation function expressed in the equation (2), is called theoretical temporal and spatial correlation function absolute value matrix, which is relative only with V x , and V y . This calculation is succinct and the accuracy is high. In practice, V x , V y are often sufficient.
[0061] In the step ( 611 ), the parameter module sets and stores a search range of the unknown ensemble ={ V x , V y , σ vx , σ vy , γ}, wherein the search range of the unknown ensemble is set as large as possible at first measurement to include the true velocity of flow layer in the search range. In the following measurements, the previous measurement result or an average value of multiple previous measurement results is preferably used as the initial value for the search range. Therefore, the calculation speed is high, and the hardware cost is low.
[0062] In the step ( 612 ), the fit module controls the DSP board ( 404 ) to fit the data matrix derived from the matrix extraction module during the step ( 610 ) with the equation (2) so as to attain the velocity of each flow layer relative to the vessel. Here, the fitting algorithm can be a sequential quadratic programming method based on the maximum likelihood principle, or preferably a sequential quadratic programming method based on the nonlinear least square principle.
[0063] In the step ( 613 ), the velocity storage module feeds the fitting results derived from the step ( 613 ) to the computer ( 406 ) through the data/control bus ( 405 ) and the computer stores the fitting results in the memory. After the step ( 613 ), the program can return back to the step ( 605 ) for the next measurement. Absolute velocity of each flow layer can be derived from the average of the velocities of each flow layer relative to the vessel ( 100 ) operated in the step ( 612 ), cooperated with the velocity of the vessel ( 100 ) relative to the bottom.
[0064] Finally, data from the temperature sensor ( 303 ), the water-leaking-detection sensor ( 304 ) and the attitude sensor ( 305 ) are fed to the computer ( 406 ) by the sonar interface control board ( 407 ). The computer ( 406 ) also cooperates data from the GPS ( 409 ) and GYRO ( 410 ) and then sends the final results to the terminal computer ( 502 ) by the network ( 501 ).
[0065] FIG. 5 illustrates diagrams of current velocities in a flow layer 350 m underneath the sea surface obtained respectively by the correlation velocity measuring sonar system with 23.5 kHz central frequency, 4.4 kHz bandwidth of the present invention and an acoustic Doppler current profiler (ADCP). FIG. 5 a illustrates the amplitudes of flow layer velocities ( 701 , 703 ) measured by these two equipments in a time interval, wherein the abscissa represents time and the ordinate represents amplitude of velocity. FIG. 5 b illustrates directions ( 702 , 704 ) of flow layer velocities measured by these two equipments in a time interval, wherein the abscissa represents time, and the ordinate represents direction. The results by these two equipments are quite coincided with each other.
|
The present invention discloses a method and a system for measuring flow layer velocities using correlation velocity measuring sonar. The present invention provides a new theoretical expression for fluid medium sonar array temporal and spatial correlation function, the velocities of each flow layer are derived by fitting experimental data and a theoretical function, or fitting absolute value operated and localized experimental data and a theoretical function. The fluid medium sonar array temporal and spatial correlation function of the present invention is succinctly expressed by Kummer function, and well coincided with the experiments. This function is applicable not only to far field region, i.e. planar wave region, but also Fraunhofer region, i.e. spherical wave region. The present invention has the merits of high measurement accuracy, small calculation load, good robustness and fast convergence.
| 6
|
FIELD OF THE INVENTION
The present invention relates to the treatment of slime deposits produced by microbes in industrial aqueous systems. This method of treating slime is specifically directed toward papermaking and cooling water systems.
BACKGROUND OF THE INVENTION
Microorganisms and the slimes they produce are responsible for the formation of deposits in papermaking and industrial cooling water systems. Bacterial slimes are composed of exopolysaccharides (EPS) which exist as capsules or slime layers outside of the cell walls. When these slimes form on surfaces in paper or cooling systems, they trap organic and inorganic components and debris present in the process waters. As the microorganisms grow within paper system deposits, portions of the deposit may detach from the surface and cause paper breaks and spots in produced paper, which reduces the paper quality and increases machine downtime. Microbial growth and slime formation in cooling systems results in reduced heat exchange caused by biofouling and plugging of heat exchanger tubes, excessive fouling of the cooling water, tower decks and fill, and is a potential cause of under-deposit corrosion.
The term "slime" is a broad one covering a wide range of viscous, mucous, or leathery materials and mixtures found in industrial waters. Slimes are polymeric in nature and can be broadly classified as chemical, biological, or composite slimes depending upon their cause or composition. For example, raw materials and equipment used in the paper industry are not sterile and water used in conjunction with such equipment is continuously being contaminated with a wide variety of micro organisms from such sources as wood pulp, chemicals, air, makeup water, and the like. The growth of certain specific forms of these biological contaminants causes or produces polymeric excretions or products that are or become slime.
Historically, slime formation has been treated by the addition to industrial waters (e.g., white water associated with the pulp and paper industry) of slimicides. The purpose of these slimicides is to destroy or arrest the growth of some of the many organisms present in the water to thereby prevent or retard the formation of slime. Chemicals used as slimicides have included chlorine, phenylmercuric acetate, pentachlorophenol, tributyl tin oxide, and isothiocyanates, all of which are relatively toxic to humans.
Microbially produced exopolysaccharides can build up, retard heat transfer and restrict water flow through cooling water systems. Controlling slime-forming bacteria by applying toxic chemicals is becoming increasingly unaccepted due to environmental problems. In addition, the efficacy of the toxicants is minimized by the slime itself, since the extracellular polysaccharide surrounding microorganisms impedes toxicant penetration.
Toxicants cannot adequately control large populations of attached bacteria and they are effective mainly against floating microorganisms. Although surfactants and dispersants which penetrate and help loosen slime can enhance the activity of toxicants, they are nonspecific and may have deleterious effects on the industrial process or the environment.
Recently, methods directed at controlling microbial slimes include the use of enzymes. These approaches attempt to disrupt the attachment process so that slime formation is prevented, or by hydrolyzing the exopolysaccharide (EPS) produced by the microorganisms after attachment. Using an enzyme to control slime will require knowledge of the composition of the slime, so that an appropriate enzyme-substrate combination is employed.
Differing views of the composition of industrial slime deposits exist, but no data directly supporting those views have been published. Research by H. J. Hatcher (Biochemical Substances as Aids in Process Control, TPPI 62(4):93, 1980) suggests that slimes are composed of levan, a homopolysaccharide composed of repeating units of fructose. This is inconsistent with literature related to the biosynthesis of Tevans, which shows that levans can only be produced by bacteria growing on sucrose (Stanier, R. Y. E. A. Aelber, and J. L. Ingraham; Structure and Function in Procaryotic Cells, Capsules and Slime Layers, The Microbial World. pp. 335-337, Prentice-Hall, Inc., Englewood Cliffs, N.J., 1975). During levan biosynthesis, the fructose unit of sucrose is incorporated into levan, while the glucose unit is used for energy and growth by the microorganism. It is unlikely that bacteria in paper or cooling systems will encounter sucrose in significant amounts, and hence levans should not be a significant component of industrial slimes.
A recent Canadian Patent, No. 1,274,442, suggested that EPS of industrial water systems may be composed of alginate, a polysaccharide composed of mannuronic and guluronic acids. U.S. Pat. No. 4,936,994, claimed that microbial slime in industrial systems can be controlled using cellulase, α-amylase, and protease, which presupposes that the slimes result from polymers of α-and β-linked glucose residues and protein.
These differing views can be contrasted with those more commonly accepted in the technical literature, that slime-producing bacteria form heteropolysaccharides consisting of monosaccharides such as glucose, mannose, galactose, and glucuronic acid. Studies have shown that the composition of EPS is usually independent of the substrate or carbon source used for growth and polysaccharide production (Sutherland, I. W. Bacterial Exopolysaccharides-Their nature and Production, Surface Carbohydrates of the Procaryotic Cell (Sutherland, I. W., ed), pp, 27-96, Academic Press Inc. Ltd., London, 1977). It was therefore felt that slimes found in industrial cooling and papermaking systems were likely to be composed of mixed heteropolysaccharides.
It is an object of the present invention to provide a microbial slime treatment program which will more effectively break down or altogether prevent the production of microbial exopolysaccharide slime than any of the other treatment approaches heretofore employed. This is achieved by using a combination of enzymes that are specific to each of the saccharides present in the slime layer.
DESCRIPTION OF THE INVENTION
The present invention comprises adding to aqueous systems experiencing microbial slime problems a combination of enzymes each specific to the numerous sugars and linkages present in the exopolysaccharide slime biomass. These enzymes are galactosidase, galacturonidase, rhamnosidase, xylosidase, fucosidase, arabinosidase and α-glucosidase. An effective treatment should include all of these enzymes. However, certain exopolysaccharide layers may be treated with fewer than all of these with the proviso that rhamnosidase and fucosidase are always present.
These enzymes may be blended as desired by the user or they may be procured from various commercial sources as pre-blended combinations. Examples include Novozym 234 (Novo Bio Labs), Spark-L (Miles) and SP-249 (Novo/Nordisk).
The amount of enzyme treatment according to the present invention will vary depending upon the severity of the microbially produced slime problem. Nonetheless, for example, if using Novozym 234, from 20 to 200 ppm of the enzyme blend is generally sufficient.
The enzyme treatment of the present invention is to be employed in aqueous systems where microbial slime causes problems. Systems which are particularly susceptible to slime proliferation are papermaking and cooling water systems. The present enzyme treatment is especially effective in these applications.
The types of slime producing bacteria present in these water systems may vary. However, the most predominant microbes found are Pseudomonas, Klebsiella, Aerobacter, Acinetobacter, Enterobacter and Flavobacterium. Although the exopolysaccharide layer produced by each of these bacteria might differ somewhat, it has been found that the saccharides present are glucose, mannose, galactose, rhamnose, fucose and glucuronic acid.
Slime deposits from 16 sites located throughout the U.S. were extracted and analyzed. Results of this analysis are shown in Table I.
TABLE I______________________________________Summary of Carbohydrate Compositions forBiological Field SamplesSOURCE COMPOSITION______________________________________Cooling Tower, LA fucose, mannose, glucose, glucuronic acidPaper Mill, Washington fucose, galactose, glucose, glucuronic acidPaper Mill, PA rhamnose, galactose, mannose, glucosePaper Mill Saveall, PA rhamnose, galactose, mannose, glucosePaper Mill AES, PA rhamnose, fucose, galactose, mannose, glucoseCooling Tower, Georgia rhamnose fucose, galactose, mannose, glucose, glucuronic acidPaper Mill, Georgia rhamnose, fucose, galactose, mannose, glucose, glucuronic acidPaper Mill, Georgia rhamnose, fucose, galactose, mannose, glucosePaper Mill, California rhamnose, fucose, galactose, mannose, glucose, glucuronic acidSulfur Bacteria, Well, FL rhamnose, fucose, galactose, mannose, glucose, glucuronic acidRefinery Cooling Tower, TX rhamnose, fucose, galactose, mannose, glucoseCooling Tower, LA rhamnose, fucose, galactose, mannose, glucoseRefinery Cooling Tower, rhamnose fucose, galactose,LA mannose, glucoseCooling Tower, LA rhamnose, fucose, galactose, mannose, glucose, glucuronic acid______________________________________
EXAMPLE 1
In order to show the efficacy of the enzyme treatment of the present invention, an assay technique was devised based on measuring the viscosities of a slime containing solution before and after various enzyme treatments. It is generally accepted that reductions in the chain length of the polysaccharides (caused by the enzyme breaking the polymeric chain) will result in a measurable drop in solution viscosity.
Exopolysaccharides were obtained from two organisms typically found in cooling and papermaking systems. These organisms produced excessive amounts of slime which was easily isolated in pure form. Several enzymes and enzyme preparations were tested against model polysaccharides.
Assay Procedure
Viscometer: Ubbelohde micro-viscometer (Schott-Gerate).
Sample volume:
3 ml of 2 mg/ml Klebsiella (ATCC 8308) polysaccharide solution or
3 ml of 1.5 mg/ml Pseudomonas (ATCC 31260) polysaccharide solution.
Enzyme volume: 50 microliters per sample.
Assay Temperature: 37° C.
Be measuring the time required for the meniscus of the treated sample to traverse between two reference points, monitored over 24 hours, and comparing that data to a control with no enzyme treatment, a drop in viscosity over time by use of that enzyme treatment is shown.
TABLE II______________________________________Percent Reduction in Viscosity Percent Reduction Percent ReductionEnzyme Used Klebsiella Pseudomonas______________________________________Novozym 234 14.20% 24.10%α-glucosidase 8.52 not runSpark-L.sup.R 7.99 0.81SP-249 0.17 24.53______________________________________ Legend: Novozym 234: (Nova Biolabs) multiple enzymes to attack α-1,3 linkages α-glucosidase: (Sigma Chemical Co.) Spark-L.sup.R : (Miles) pectinase (specific to galacturonic acid, rhamnose, xylose, fucose, arabinose and galactose) SP-249: (Novo Nordisk) galacturonidase, rhamnosidase, xylosidase, fucosidase, arabinosidase, galactosidase.
The above data indicate that these enzymes are breaking bonds within the polysaccharide chains.
EXAMPLE 2
Klebsiella pneumoniae, IPC 500 (Institute of Paper Chemistry), and Pseudomonas aeruginosa, ATTC 10145, were allowed to grow and attach to stainless steel test surfaces in 1500 ml of test medium containing Novozym 234 at concentrations between 2 and 200 ppm. A test unit to which was added 200 ppm of heat-treated (121° C., 15 min) Novozym 234 was included in order to confirm that enzymatic activity was responsible for any bacterial slime control observed in enzyme-treated test units. After 24 and 48 hours, 350 mL of test medium was removed and replaced with 350 ml of fresh test medium. Novozym 234 concentrations between 2 and 200 ppm were replenished at 24 and 48 hours to the appropriate test unit. Heat-treated Novozym 234 was also added to the appropriate test unit. At 72 and 144 hrs, stainless steel test surfaces were removed from each test unit and prepared for scanning electron microscopic (SEM) analysis. Each test surface was examined by SEM and photographed.
After 72 hours the test surface from the unit which had no enzyme treatment had evidence of bacterial attachment as did the test surface treated with 2 ppm of Novozym 234. At 20 and 200 ppm of Novozym 234, no bacterial attachment was observed on the test surfaces. Evidence that enzymatic activity attributed to Novozym 234 was responsible in the disruption of bacterial attachment was confirmed by bacterial attachment in the presence of heat-treated Novozym 234.
Table III contains data related to the total bacterial counts (TBC) found in the bulk water of the test unit throughout the experiment. As shown, these counts remained between 10 5 and 10 7 CFU/mL throughout the experiment. This shows that the enzyme was not preventing attachment as a result of biocidal activity. The enzyme does not function as a biocide.
TABLE III__________________________________________________________________________Total Bacterial Counts (CFU/mL) in Bulk Water of Each Test UnitElapsed Time of Unit 1 Unit 2 2 ppm Unit 3 20 ppm Unit 4 200 ppm Unit 5 200 ppmExperiment (Hrs.) Control Enzyme Enzyme Enzyme Heat-Treated Enzyme__________________________________________________________________________24 58 × 10.sup.7 45 × 10.sup.7 71 × 10.sup.7 29 × 10.sup.7 24 × 10.sup.748 96 × 10.sup.7 82 × 10.sup.7 119 × 10.sup.7 103 × 10.sup.7 23 × 10.sup.772 69 × 10.sup.5 4 × 10.sup.5 <1 × 10.sup.5 80 × 10.sup.7 49 × 10.sup.7144 54 × 10.sup.7 84 × 10.sup.7 6 × 10.sup.5 195 × 10.sup.7 180 × 10.sup.7__________________________________________________________________________
This example shows that enzyme activity against polysaccharides that contain 1,3-α-linkages, controls bacterial attachment and eventual slime formation. Specifically, Novozym 234 contains 1,3-α-glucanase, 1,3-β-glucanase, laminarinase, xylanase, and chitinase enzyme activities. In studies using various para-nitrophenyl (PNP) glucosides, Novozym 234 also contains α-galactosidase which is an enzyme activity which is required for the hydrolysis of slime heteropolysaccharides.
EXAMPLE 3
Using the same test system as in Example 1 the effect of dilution of an enzyme on the rate of polysaccharide hydrolysis was examined.
Assay Procedure
Viscometer: Ubbelohde micro-viscometer (Schott Gerate).
Sample volume: 3 mL of 6.24 mg/mL Klebsiella pneumoniae exopolysaccharide solution.
Enzyme volume: 50 uliters.
Assay Temperature: 35° C.
The enzyme tested here was a pectinase enzyme, Pectinex™, supplied by Novo/Nordisk. The enzyme was diluted to concentrations which were 1/4 and 1/2 the original concentration. FIG. 1 is a graphical representation of the results obtained. As shown, initial hydrolysis is a function of the enzyme concentration with most activity occurring within the first hour of the experiment. This pectinase enzyme which contains enzyme activities such as pectintranseliminase, polygalacturonzase, pectinesterase, and hemicellulase is capable of hydrolyzing an exopolysaccharide involved in the adhesion of a microbe to surfaces. In studies using PNP glycosides, it was further shown that Pectinex™ contains (α-thamnosidasae and α-galactosidase activity.
|
A method for treating the microbial slime that is generated in industrial water systems by adding to the water a combination of enzymes specific to the numerous saccharide units that make up the exopolysaccharide layer. These enzymes comprise galactosidase, galacturonidase, rhamnosidase xylosidase, fucosidase, arabinosidase and α-glucosidase.
| 3
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates in general to oil and gas well production, and in particular to a system for removing accumulated liquid from gas producing wells.
2. Description of the Prior Art
Many gas wells product both gas and liquids such as water, oil and condensate. The gas is often flowed from the casing to a sales line. Part of the liquid, initially entrained as droplets in the gas flow, drops out of the flow because of insufficient velocity of gas. The liquid accumulates in the bottom of the well, and as accumulation increases, exerts an increasingly large back pressure on the formation. This back pressure, which equals the hydrostatic head of the liquid column, may be large enough to reduce the production rate or completely stop production.
It is therefore advantageous to periodically remove accumulated liquid from gas wells. A typical gas well has casing through which the gas flows through the perforations at the gas producing formation to a production or sales line at the surface or well head. Tubing inside the casing is used to remove accumulated liquids. The tubing usually has an open lower end extending close to the producing formation and into the accumulated liquid. Normally, the tubing is closed by the valve at the surface, and the casing is opened to permit gas to flow into the sales line. Accumulated liquid rises in the casing and in the tubing to the same level. To remove liquid the valve at the top of the tubing is opened to reduce the pressure inside the tubing to a value less than the pressure inside the casing and in the sales line. Thus, the pressure of the gas inside the casing forces liquid through the tubing toward the well head. The liquid and gas from the tubing is discharged into a low pressure storage and disposal system.
In the above method, liquid removal is facilitated by use of a loose fitting plunger which separates the liquid and the gas. This helps prevent the gas from migrating through the liquid and prevents the liquid from dropping through the gas.
There are a number of variations of the above described methods. Two such variations may be seen in U.S. Pat. Nos. 3,053,188 and 3,203,351. One disadvantage of such systems is that they require a second pipe system on the surface leading to the lower pressure storage or disposal facility. This represents a considerable additional amount of pipe and equipment that must be installed and maintained. Also, the gas discharged in the lower pressure system may not be usable unless pressurized to the sales line pressure, which may not be economical.
SUMMARY OF THE INVENTION
It is accordingly the general object of this invention to provide an improved system for removing accumulated liquid from gas producing wells.
It is a further object of this invention to provide an improved system for removing accumulated liquids from gas producing wells that does not require a low pressure surface system.
It is a further object of this invention to provide an improved system for removing accumulated liquids from gas producing wells that avoids back pressure on the formation as the liquid accumulates.
As in the prior art, a system is provided in which gas is produced through the casing. A string of tubing is located in the casing, with its lower end adapted to be close to the producing formation and in communication with the accumulated liquid. Unlike the prior art systems, however, the tubing is also connected to the sales line, not to a low pressure system. During gas producing operations, both the tubing and casing communicate with the sales line and have the same pressure.
As in the prior art liquid will accumulate in the tubing, and the gas will be produced from the casing. Periodically, both the tubing and casing are closed to the sales line. Formation pressure will build up in the casing, causing the liquid in the tubing to rise. Then only the tubing is opened to the sales line. Casing gas at the build-up pressure will force the liquid into the sales line. Once discharged, the casing is again opened to the sales line to repeat the cycle.
If sufficient well depth is exists below the perforations, liquid may accumulate therein to avoid back pressure on the perforations. If not, a packer is set above the perforations in the casing. The lower end of the tubing is closed to upwardly flowing fluid and located in a standpipe above the packer. The produced gas from the formation flows through the tail pipe, the annular area between the standpipe and the tubing, then into the annular area between the casing and the tubing. The standpipe and tubing annular area creates a restricted flow passage for the fluid, resulting in higher velocities and improved liquid entrainment. Once discharged from the standpipe, the velocity reduces, and entrained liquid drops out to accumulate on the packer between the casing and the standpipe. This isolates the accumulated liquid from the perforations. A passage communicates the lower end of the tubing with the space between the standpipe and casing, allowing the accumulated liquid to flow into the tubing. Preferably a plunger is located in the tubing to facilitate liquid removal.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1a and 1b are partial schematic representations of a system constructed in accordance with this invention.
FIG. 2 is a schematic in reduced scale of the system of FIG. 1, further simplified and shown in the gas producing mode.
FIG. 3 is a schematic in reduced scale of the system of FIG. 1, further simplified and shown in the shut-in mode.
FIG. 4 is a schematic reduced scale of the system of FIG. 1, further simplified and shown in the shut-in mode at a time subsequent to the mode as shown in FIG. 3.
FIG. 5 is a schematic in reduced scale of the system of FIG. 1, further simplified and shown in the liquid producing mode.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1b, the system includes a conventional casing 11. Casing 11 comprises sections of metal pipe lowered into the well and set by cement pumped up the annular space between the pipe and the borehole wall for a selected distance. Perforations 13 are subsequently made by shaped explosives in the casing, annular cement portion, and formation, to allow fluid from the desired earth formation to be produced.
In the preferred embodiment, a packer 15 is set above the perforations 13. Packer 15 has an annular resilient member that seals against casing 11. Packer 15 has an inner flow passage, and a tail pipe 17 extends downwardly from packer 15 for a shortdistance. A section of pipe or pup joint 19 extends upwardly from packer 15. A collar 21 connects pup joint 19 to a mandrel 23. Mandrel 23 is a member having a longitudinal internal passage 25 with a closed lower end. A lateral passage 27 in mandrel 23 leads from the bottom of passage 25 to the space between mandrel 23 in casing 11, defined herein as part of a collection chamber or area 28. Mandrel 23 also has a longitudinal flow passage 29 separate from passage 25. Mandrel 23 has a reduced diameter threaded upper portion connected to a pup joint 30.
A section of pipe or pup joint 31 is secured to the large diameter portion of mandrel 23 by collar 33. Pup joint 31 extends upwardly, surrounding the upper portion of mandrel 23, pup joint 30, in a continuation of flow path 29. The area surrounding pup joint 31 is also part of the collection chamber 28. The top of pup joint 30 is secured to a stinger receiver 35. A stinger 37 inserts in stinger receiver 35 and extends upwardly, the receiver 35 having an inner bore continuing passage 25. A section of tubing 39 is secured to stringer 37, it having a longitudinal bore continuing passage 25.
Pup joint 31 is secured by a collar 41 to a section of tubing 43 of larger diameter than tubing 39. The annular space between tubing 39 and tubing 41 continues the flow path passage 29. Referring to FIG. 1a, tubing 43 is secured by a collar 45 to a pup joint 47 having opening 49 at its top. Opening 49 serve as the upper open or discharge end of the flow path passage 29. A deflector 51 surrounds openings 49 a selected annular distance from them. Tubing 39 is secured to a receiver nipple 53.
A bumper spring assembly 55 is located on top of receiver nipple 53. The annular space around bumper spring 55 and a set of ports 56 in receiver nipple 53 at the base of the bumper spring 55, continue the passage 25. The lower end of a string of tubing 57 is secured to the receiver nipple 53. A conventional plunger 59, such as shown in U.S. Pat. Nos. 3,053,188, and 3,203,351, is located in tubing 57 and adapted to rest in its lower position on bumper spring 55. Plunger 59 is loosely carried in tubing 57, and is sized so as to allow a low flow rate of gas and liquid past it. It does not form a tight seal with tubing 57, but a sufficient velocity of fluid up tubing 57 will move plunger 59 upward, as is well known in the art.
At the top of the well, a conduit 61 connects the top of casing 11 to the sales line 63. Sales line 63 is the line leading to the processing equipment for the gas, and is maintained at a pressure that may be from 150 psi to 800 psi (pounds per square inch) or more. A valve 65 opens and closes conduit 61. The top of tubing 57 is connected to a lubricator 67. Lubricator 67 receives plunger 59. Lubricator 67 has a bumper string 69 at its top to absorb shock when the plunger 59 strikes the top. A port 71 on the side of the lubricator 67 is adapted to be closed by plunger 59 when in the lubricator. A conduit 73 leads from port 71 to the sales line 63, downstream of valve 65. Conduit 73 serves as a connection means for connecting the tubing 57 to the sales line 63. A valve 75 opens and closes conduit 73. Control circuit 77 pneumatically opens and closes the valves 65 and 75.
The mandrel 23, pup joint 31, collars 33 and 41, tubing 43, collar 45, pup joint 47, and deflector 51 make up an assembly that may be referred to collectively as a standpipe 79. Standpipe 79 is shown schematically in FIGS. 2-5. The lower end of production tubing 57 will be defined herein to include passage 25 in mandrel 23, pup joint 30, stinger receiver 35, stinger 37 and tubing 39. The lower end of tubing 57 will be considered the lower end of longitudinal passage 25. The lower end of tubing 57 is closed to fluid coming up the tail pipe 17, but is open to fluid in the collection area surrounding the standpipe 79 and above packer 15 through lateral passage 27.
In operation, referring to FIG. 2, gas is produced by opening both valves 65 and 75. Gas and entrained liquid droplets, indicated by the dotted areas 81, will flow from perforations 13 into tail pipe 17, as shown by arrows 83. The gas and liquid mixture will flow into the restricted flow path 29. The lesser cross-sectional area of flow passage 29 as compared to casing 11 diameter, increases the velocity of the fluid. The higher velocity prevents a substantial amount of the droplets from falling out of the flow. At the top of the standpipe 79, the flow discharges through openings 49 and enters casing 11 surrounding tubing 57. The larger flow path in casing 11 decreases the velocity of the fluid, casing liquid to drop from the flow and fall by gravity onto the packer 15. The gas continues to flow to the top of casing 11, through conduit 61 and into sales line 63.
As the liquid accumulates in the collection area 28, it will proceed through lateral passage 27 into passage 25 as indicated by the shaded areas 85. The pressure will vary per well, but in general in a gas well, the bottom hole pressure will be only slightly greater than the pressure at the top of the well since the gas and droplets in casing 11 will have little hydrostatic weight. The pressure at the sales line 63 will be substantially the same as the pressure at the top of tubing 57 and at the top of casing 11. There will be no flow through tubing 57 to sales line 63 since no pressure differential on liquid 85 exists to force the liquid up. The equal pressure above liquid 85 in passage 25 of tubing 57 and above liquid 85 in the collection area 28 of casing 11, causes the columns in these respective areas to be at the same vertical level. The perforations 13 will be isolated from the hydrostatic head of the accumulated liquid 85. The standpipe length, typically about 100 feet, will allow a substantial column of liquid to build up. The well may be several thousand feet deep, thus the standpipe length is much less.
Once the accumulated liquid 85 reaches a selected level, both valves 65 and 75 will be shut-in, as indicated in FIG. 3. The time for shutting these valves is determined empirically on a well to well basis, but the shut-in should be before the liquid column 85 reaches the top of the standpipe 79. Once determined for a well, a timer in the control circuit 77 will cause the closure of valves 65 and 75. When shut-in, formation pressure in casing 11 will build up from the flowing pressure in line 63 toward a shut-in pressure. During build-up, fluid will continue to flow from perforations 13, up flow passage 29, and out openings 49 at the top of standpipe 79. As the casing 11 pressure builds up, it will force the level of liquid 85 down in the collection chamber 28, the liquid proceeding through lateral passage 27 into longitudinal passage 25. The level in passage 25 will rise, with some of the liquid possibly flowing past plunger 59.
FIG. 4 illustrates continuing formation pressure build-up. In the collection chamber 28, the fluid level will drop down to the level of lateral passage 27. Gas bubbles, indicated as numeral 87, will migrate up the column of liquid 85 and past plunger 59 to enter the gas above the column. Additional liquid 85 will also flow slowly past plunger 59. The pressure above liquid 85 in tubing 57 will be the same as the pressure in the casing 11 collection chamber 28, less the pressure due to the hydrostatic weight of the liquid column 85. For example, if the pressure at the top of casing 11 is 400 psi, and the pressure at the top of tubing 57 is 320 psi, then a hydrostatic head of liquid 85 exists equivalent to 80 psi. This liquid column might extend to 100 feet or so above plunger 59. These pressure differentials can be used to calculate the amount of liquid in tubing 57.
After a selected time for formation pressure build-up has past, the tubing valve 65 is opened, while the casing valve 75 remains closed, as shown in FIG. 5. The formation pressure need not be fully built up, but should be sufficient to move the liquid 85 to the sales line 63. That is, the casing 11 pressure less the sales line 63 pressure should exceed the hydrostatic pressure due to the height of the column of liquid 85. The time for opening tubing valve 65 may be empirically determined and set by a timer. The time duration for build-up may be from a few minutes to several hours. Also, pressure differential switches between the casing 11 and tubing 57 could indicate the liquid column hydrostatic pressure, and trigger the opening of tubing valve 65 once the differential has reached a selected amount. Also, the pressure in the casing 11 could trigger the opening of tubing valve 65 once the pressure has reached a selected value.
Once the tubing 57 is opened to the sales line 63 pressure, the tubing 57 pressure at the top drops quickly to the sales line 63 pressure. The higher build-up pressure in casing 11 drives the column of liquid 85 upward into the sales line 63. Additional fluid from the formation will be produced through perforations 13, as well. The high velocity flow causes the plunger 59 to move upward at a high rate of speed, it being the interface between the gas entering the tubing 57 and the liquid column 85 above the plunger. Plunger 59 prevents the gas from breaking through the liquid 85 in a large slug.
Once plunger 59 reaches the top of lubricator 67, it closes port 71 (FIG. 1a), closing off tubing 57 flow. The control circuit 77 senses the differential between the higher pressure in tubing 57 below plunger 59, and the lower pressure in sales line 63. This differential causes the control circuit 77 to signal valve 75 to open the casing 11 to the sales line 63. Gas will commence to flow from casing 11 into the sales line 63, fairly quickly dropping to the sales line 63 pressure. The pressure at the lower end of tubing 57 will also drop to the sales line 63 pressure. The plunger 59 will then have the same pressure above and below it, thus will drop by gravity to bumper spring 55. The cycle will be repeated as often as is necessary to remove accumulated liquid.
The standpipe 79 and packer 15 serve as isolation means for isolating the perforations 13 from the accumulated liquid 85. If there is sufficient casing 11 depth below perforations 13, however, this portion of casing 11 could serve as isolation means, and the packer 15 and standpipe 79 could be eliminated. If so, the tubing 57 lower end would be open and would extend into the liquid at the bottom of the casing 11. Plunger 59 would be located close to the bottom of tubing 57.
Valves 65 and 75, lubricator 67, and control circuit 77 serve as valve means for selectively opening and closing the tubing 57 in casing 11 to the sales line 63. The annular area between standpipe 79 and casing 11 serves as collection means for collecting liquid that drops from the fluid flow. The flow path 29 in standpipe 79 serves as restriction means for restricting the cross-sectional area of the flow path for the produced fluid for a selected distance.
It should be apparent that an invention having significant advantages has been provided. The liquid removal system allows accumulated liquid to be produced from gas producing wells without the need for a low pressure system on the surface. The system also isolates the perforations from accumulated liquid, even if there is insufficient hole depth below the perforations. The isolation means avoids forcing the liquids back into the formation during casing gas pressure build-up. The system utilizes the energy of the well created by formation pressure build-up to produce the liquid.
While the invention has been shown in only one of its forms, it should be apparent that it is not so limited but is susceptible to various modifications and changes thereof.
|
Production equipment for oil and gas wells has features that allow accumulated liquid to be removed from the well without the need for a low pressure system. This equipment also isolates the perforations from accumulated liquid back pressure, even if there is insufficient hole depth below the perforations. The well has a tubing string located inside the casing, with the tubing in contact with the accumulated liquid. Both the tubing and the casing are connected to the sales line. Periodically, both the casing and tubing are shut-in, allowing formation pressure to build up in the casing. Then the tubing is opened to the sales line to discharge its accumulated liquid, it being driven by the higher formation pressure that has built up. To isolate the perforations from accumulated liquid, a standpipe is mounted in the casing above the perforations by a packer. The standpipe receives the lower end of the tubing which is closed except for a passage connecting it to the annular area between the standpipe and the casing. Produced fluid flows up the standpipe in a restricted area adjacent the tubing. At the top of the standpipe, liquid droplets drop out and accumulate above the packer between the standpipe and the casing.
| 4
|
FIELD OF THE INVENTION
This invention relates to a wireless clamp tool. More specifically, the invention relates to an apparatus that controls and monitors the operation of the clamp tool.
BACKGROUND OF THE INVENTION
Past embodiments of qualifier technologies have proved challenging when implemented in some production facilities. Many manufacturers would prefer to “cut the cord” and go wireless so that additional cables have to be used in the assembly process. The challenges of creating a wireless tool lie in the current consumption of the microprocessor, tool monitors and tool controllers. In order to operate from a battery and maximize the life of that battery, low power states need to be employed when the tool is at rest and fastenings are not taking place.
Assembly plants are filled with tools, tool monitors, and tool controllers. A typical tool monitor will supervise the tool's fastening process and then report back to both the operator and the system if the fastening was good or bad (OK/NOK). In many cases it would be advantageous to eliminate the signal cables and replace them with radio transceivers.
SUMMARY OF THE INVENTION
This invention is a tool and monitor assembly that verifies clamps have been installed properly with the tool. The radio controlled clamp tool provides accountability and control with a strain gauge sensor operation. The radio tool is designed to perform the operation of a clamp tool, retain the signature and transmit the signal with data to an interface box for error proofing analysis.
The tool is battery operated and uses a moment-insensitive flexure design to normalize the force of the strain gauge to provide an accurate representation of the characteristics of the clamp. These are recorded by an onboard microprocessor analyzed to determine if within predetermined specifications and then transmitted wirelessly to a receiver. The tool is equally effective at sensing a twisting action, push or pulling and or straight on prying action, allowing the tool to access clamps regardless of their orientation and or obstructions. The Tool is designed to work with various clamp types including Popp, Spring Band and Pull Pin Clamp but not excluding similar type clamps.
Other objects and advantages of the present invention will become apparent to those skilled in the art upon a review of the following detailed description of the preferred embodiments and the accompanying drawings.
BRIEF DESCRIPTIONS OF THE DRAWINGS
FIG. 1 shows a typical signal during clamping.
FIG. 2 is an RF enclosure for receiving and processing RF signals from an electrical strain gauge sensor.
FIG. 3 is a block diagram for using a batter powered, wireless tool using an electrical strain gauge sensor.
FIG. 4 is a drawing of the beam.
DETAILED DESCRIPTION OF THE INVENTION
The tool is an apparatus consisting of an effector to release the clamp, A flexure with applied electronic strain gauges to sense the forces being applied to and received from the release action of the clamp, a circuit to amplify and convert the analog electrical signals into a digital representations of the signals, a microprocessor to record and analyze the data produced by the electrical signals, and a radio transceiver to transmit an indication that a clamp has been released to the assembly control box. Transmission of the signals operates in the 900 MHZ or the 2.4 GHZ ranges.
The tools are sized to the clamps that need to be measured, the tools then need to be learned to the receivers that are to receive and process the data. This RF system includes a clamping tool having a transmitter for sending electrical signals to a receiver; and a remote qualifier having a receiver for receiving the electrical signals from the transmitter of the clamping tool.
In the preferred embodiment, the programmed micro processor of the clamping tool is configured to identify and store a portion of the electrical signal as a calibration value. The value of each operation is then compared to the calibration value and then will give a accept or reject signal at the completion of a successful cycle.
This system changes the algorithms to record and read the strain gauge data into an electrical signal representative of the pressure used to bend the strain gauge therefore plotting the data over time to determine the signature of the gauge. The signature is then compared with the stored data and then outputs a accept or reject based on the comparison of the cycle.
FIG. 1 shows a typical signal during clamping.
FIG. 1 shows typical signal levels during clamping, approved clamping and clamp release. Signal level rose above threshold level and remained above calibrated window for the minimum time. The signal level then dropped below threshold level when the clamp released.
EXAMPLE I
FIG. 2 is an RF enclosure for receiving and processing RF signals from an electrical strain gauge sensor. FIG. 2 shows that the radio receiver and micro processor is an interface box that receives data signals from the clamping tool that are recorded and analyzed by an on-board microprocessor to uniquely identify the characteristics of the clamp and determine if the operation was completed as per the specification. The receiver and tool are paired wirelessly and securely. Two-way communication allows for the tool to verify if the data was successfully transmitted from the tool to the receiver. The receiver then generates audible and visual accept and reject outputs. The interface box also monitors signal strength and battery strength of the tool.
Features:
Microprocessor design
Ultra bright LED indicators
900 Mhz or 2.4 GHz wireless transmission
90-240 vac 50/60 power inputs
IEC on/off power cable interface
Configurable dry contact outputs
Key switch protected programming
UUCSA
FCC/CE registered
Patented
The transistor connects the microprocessor to an alarm which indicates incomplete and completed tool cycles. Relays are NO or NC momentary or latching relay outputs. Output 1 provides a signal on a incomplete cycle. Output 2 provides a signal on a completed cycle.
FIG. 3 shows the system of this invention in greater detail. FIG. 3 shows the strain gauge sensor, a battery, algorithm generator, transmitter and RF antenna. FIG. 3 also shows A/D converter and microprocessor in greater detail. Included are RF antenna, 900 MHz or 2.4 GHz receiver, algorithm decoder, microprocessor and alarm. Also included are additional microprocessor and conventional power supply. Microprocessor monitors the low battery function and may provide additional capacity to processor.
FIG. 4 shows the beam strain gauge sensor of FIG. 3 in greater detail.
EXAMPLE II
The clamping tool is designed to perform the operation of a clamp, retain the signature and transmit the signal with data to an interface box for error proofing anaylsis.
The tool is battery operated and utilizes a moment-insensitive flexure design to normalize the force of the strain gauge to provide an accurate representation of the characteristics of clamp. These are recorded by an on-board microprocessor analyzed to determine if the operation is within predetermined specifications and then transmitted wirelessly to a receiver. The tool is equally effective at sensing a twisting action or a straight on prying, push or pull action, allowing the tool to access clamps regardless of their orientation and/or obstructions.
Features:
Microprocessor design
Ruggedized strain gauges
Battery operated (2 AA cells)
Long battery life
900 MHz or 2.4 GHz FCC approved radio outputs
On/Off Switch
Compact design
Interchangeable heads
In addition to these embodiments, persons skilled in the art can see that numerous modifications and changes may be made to the above invention without departing from the intended spirit and scope thereof.
The above detailed description of the present invention is given for explanatory purposes. It will be apparent to those skilled in the art that numerous changes and modifications can be made without departing from the scope of the invention. Accordingly, the whole of the foregoing description is to be construed in an illustrative and not a limitative sense, the scope of the invention being defined solely by the appended claims.
|
This system is a tool and monitor assembly that verifies clamps have been activated properly with the tool. The radio controlled clamp tool provides accountability and control with a strain gauge operation. The radio tool is designed to perform the operation of clamp tool, retain the signature and transmit the signal with data to an interface box for error proofing or tool analysis.
| 1
|
FIELD AND BACKGROUND OF THE INVENTION
The present invention relates to a device for inserting a reinforced introducing point of a sliver into a spinning unit of a rotor spinning machine.
Several devices exist for inserting a new sliver into a spinning unit of a rotor spinning machine by connecting the end of a new sliver to the end of a sliver that has already been inserted into the spinning unit and spun. This connection can be summarized as follows: a feeler for monitoring the sliver that is situated under the spinning unit determines if the sliver being spun has been cut or interrupted and in turn stops the spinning process. A portion of the sliver is withdrawn such that a sufficiently long sliver end hangs from the condenser hole of the spinning unit. When the original textile can is replaced by a new, full can having another sliver end positioned in a holder located on the can, the two sliver ends are grasped by a mechanism and connected by interlacing. The spinning unit is started again for continuing the spinning process and the newly joined sliver is inserted into the spinning unit.
Another known device for inserting the end of an adapted sliver into a spinning machine is a device wherein the end of the sliver is gripped between a pair of rotating rollers and inserted into the condenser hole by the revolving motion of the rollers.
The drawbacks of these known devices include the necessity to install a sliver presence monitoring feeler at each operating station (spinning station) of a rotor spinning machine which requires a modification of existing spinning units. This constitutes a considerable drawback when automating the sliver process operation.
Other drawbacks include the difficulty encountered in ensuring a constant quality connection of the two sliver ends.
Fluctuations in the quality of the connection lead to sliver ruptures when it is drawn into the spinning unit, and thus cause a defect that cannot be repaired by the operating device. The quality of the yarn section produced from the connection of the sliver ends is also affected. First, the yarn fineness changes to such an extent that in the subsequent processing this section is considered as a quality defect in the fabric. Since the end of the original sliver and the length of the connecting section of sliver, together, make a sliver length which cannot be combed out of the rotor in one attempt, the sliver can only be removed by repeatedly cleaning the rotor.
A drawback also exists where the adapted sliver end is gripped in a pair of revolving rollers because there is considerable distance between the gripping point of the revolving rollers of the gripper and that of the feed roller and the table of the spinning unit which requires the adapted sliver end to be stiffer. Again, in case of high-speed rotor machines with small diameter rotors, the adapted sliver end cannot be combed out of the rotor at one time by suction prior to being spun by the spinning machine, thus causing yarn quality fluctuations.
SUMMARY OF THE INVENTION
The above-described drawbacks are eliminated by the present invention because it comprises a rotatably mounted first pneumatic cylinder having a piston rod, coupled with a non-circular static cam for carrying a second pneumatic cylinder on which is rotatably mounted a gripper coupled with its piston rod. The gripper is fitted with two introducing arms wherein at least one of which is rotatably seated.
In a preferred embodiment, the distance between the introducing arms for gripping reinforced introducing point of the sliver is smaller than the width of the recess of the support holder in which the reinforced introducing point of the sliver is seated.
Also, the ends of the introducing arms can be bevelled at an acute angle for better gripping of the sliver.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a partial elevational side view of the present invention;
FIG. 2 is a partial cross-section top plan view of the device of FIG. 1;
FIG. 3 is a partial elevational side view of the device of FIG. 1 gripping a reinforced introducing point of the sliver;
FIG. 4 is a partial cross-sectional top plan view of the device of FIG. 1 inserting a reinforced introducing point of the sliver into a condenser of a spinning unit;
FIG. 5 is a partial cross-sectional side view of a support holder holding the reinforced introducing point of the sliver; and
FIG. 6 is a top plan view of the holder of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 2 illustrates that the present invention comprises a device for inserting a reinforced introducing point 1 of a sliver 2 into a spinning unit 3 of a rotor spinning machine. The present invention comprises a first pneumatic cylinder 4 fixed to a shaft 51 of a pneumatic motor 5. Motor 5 is fixed to a frame 61 of an operating device 6 of the rotor spinning machine 3.
Seated at the end of the piston rod 41 of the first pneumatic cylinder 4 is a second pneumatic cylinder 7 to which is fixed a pin 71 with a roller 72 rotatably seated thereon and being in permanent contact with a non-circular static cam 8 fixed on the frame 61 of the operating device 6. Mounted on the piston rod 41 of the first pneumatic cylinder 4 is a spring 42 pushing the roller 72 into the curved surface of the non-circular static cam 8, also shown in FIG. 1.
A gripper 9 is rotatably mounted to the second pneumatic cylinder 7 by an axis 73. The piston rod 74 of the second pneumatic cylinder 7 is connected by means of a tie rod 75 with the gripper 9 at a pneumatic piston 91. The pneumatic piston 91 moves introducing arms 92 and 93 of gripper 9 for gripping the reinforced introducing point 1 of the sliver 2. The introducing arms 92, 93 are bevelled at an acute angle 2 for at least a part of their length. One of the introducing arms 92 or 93 can be stationary.
FIG. 4 illustrates that the spinning unit 3 of the rotor spinning machine is equipped with a sliver feed device consisting of a condenser 31 carrying at its end a supply table 32. Opposite the supply table 32 is mounted a supply roller 33 connected to a drive device (not shown).
The sliver 2 is deposited in a known non-circular sliver container 10 having a support holder 101 fixed to one of its sides. The support holder 101 has a groove 102 for receiving the reinforced introducing point 1 of the sliver 2. The groove 102 is preferably intersected or interrupted by a recess 103 which is transverse to groove 102 and is deeper and wider than the groove 102 for permitting the introducing arms 92, 93 to enter it. The recess 103 is deeper than the part of the introducing arms 92, 93 which comes into contact with the reinforced introducing point 1 of the sliver 2. In another embodiment, the operating device 6 is accompanied by a device (not shown) for gripping the reinforced introducing point 1 and for locating it between the introducing arms 92, 93 of the gripper 9.
During the transport of the operating device 6, the first pneumatic cylinder 4, like the other mechanisms, is held in a transport position so as to avoid a collision with other mechanisms of the rotor spinning machine. This transport position is maintained until the operating device 6 arrives at the spinning unit 3 after a non-circular sliver container 10 has been exchanged and it has become necessary to insert the reinforced introducing point 1 into the feed device of the spinning unit 3 of the rotor spinning machine for continuing the operation of the spinning unit 3.
At the beginning of the inserting process, the pneumatic motor 5 turns the body of the first pneumatic cylinder 4 so as to place the gripper 9 over the groove 102 of the support holder 101 fixed to the non-circular sliver container 10. At the same time, the pneumatic piston 91 opens the introducing arms 92, 93 of the gripper 9. The first pneumatic cylinder 4 pushes out its piston rod 41, thus bringing the open introducing arms 92, 93 of the gripper 9 into the recess 103 of the support holder 101. Arms 92 and 93 enter on each side of the reinforced introducing point 1. With its reverse motion, the pneumatic piston 91 closes the introducing arms 92, 93 of the gripper 9 and grips the reinforced introducing point 1 leaving its narrow end protruding through the narrowed front part of the introducing arms 92, 93. By means of the spring 42, the first pneumatic cylinder 4 brings its piston rod 41 back into a position in which the gripper 9 is positioned over the groove 102 of the support holder 101 and the roller 72 leans against the operating surface of the non-circular static cam 8.
The pneumatic motor 5 turns shaft 51 so as to place the body of the first pneumatic cylinder 4 into the insertion position in which the gripper 9 is situated opposite the hole of the condenser 31 of the spinning unit 3. The position of the piston rod 41 of the first pneumatic cylinder 4 is ensured during the rotation of the latter by the motion of the presser roller 72 on the operating surface of the non-circular static cam 8 to which the roller 72 is permanently pushed by the spring 42.
The piston rod 74 of the second pneumatic cylinder 7 is turned through 90°, due to its fixed connection with the body of the gripper 9, and thus turns the introducing arms 92, 93 with the reinforced introducing point 1 gripped between and positions arms 92 and 93 with point 1 opposite the hole of he condenser 31 of the spinning unit 3. The first pneumatic cylinder moves its piston rod 41 outwardly causing the introducing arms 92, 93 of the gripper 9 together with the reinforced introducing point 1 gripped between them to be inserted into the condenser 31. Thus, the end of the reinforced introducing point 1 is placed near the supply table 32 and the supply roller 33 which begins to turn. The subsequent motion of the piston rod 41 shifted out of the first pneumatic cylinder 4 brings the reinforced introducing point 1 between the supply table 32 and the revolving supply roller 33 causing the point 1 to be trapped and pulled inside spinning unit 3 while the pneumatic piston 31 opens the introducing arms 92, 93. Once point 1 is inside spinning unit 3, the supply roller 33 stops. At this time, the point is gripped between the supply table 32 and the supply roller 33 for producing suitable sliver 2 quality.
After the introducing arms 92, 93 of the gripper 9 have been opened, the piston rod 41 of the first pneumatic cylinder 4 returns to a position in which the roller 72 contacts the operating surface of the non-circular static cam 8. After the body of the gripper 9 has been turned back through 90°, the pneumatic motor 5 turns the body of the first pneumatic cylinder 4 back to its transport position.
In the further process, the fibres of the reinforced introducing point 1 are sucked off from the rotor of the spinning unit 3, and only then is the rotor spun-in in a well-known manner, and the spinning unit re-starts the yarn production.
|
A device for inserting a reinforced introducing point (1) of a sliver into a spinning unit (3) of a rotor spinning machine uses a rotatably mounted first pneumatic cylinder (4) having a piston rod (41), coupled with a non-circular static cam (8) which carries a second pneumatic cylinder (7) onto which is rotatably mounted a gripper (9). The gripper (9) is coupled with a piston rod (74) of the second cylinder for opening and closing two introducing arms (92, 93) wherein at least one of the arms is rotatably seated.
| 3
|
FIELD OF THE INVENTION
[0001] The present invention relates generally to managing network traffic, and more particularly, to increasing efficiency in determining routing of a data packet through the use of a Cyclical Redundancy Check (CRC) hash function.
BACKGROUND OF THE INVENTION
[0002] In the process of moving data over a network, it is necessary to determine whether the data will be allowed on the network, and if so, where the data will be directed. When the data is sent from a source to a destination, the network may determine if both the sender and the recipient are valid and permitted to use the network, as well as how the data will be processed. Transport Control Protocol/Internet Protocol (TCP/IP) data is typically transferred by means of frames that include at least two components, an address header and a data payload. Information that is typically used to move the data through the network to the destination may be found in the address header in the form of a five-tuple that comprises following fields: a source address, a destination address, a source port, a destination port and a protocol.
[0003] It is not to unusual to have a network addressing scheme that supports as many as 4 billion sources having the ability to send data to any of 4 billion destinations and where each source or destination can have upwards of 64 thousand ports. Thus, trying to support such an addressing scheme may require an enormously large look-up table, as well as a traffic management system with a staggering amount of memory. On the other hand, the presence of a limited amount of traffic on a network at any given time allows the use of a smaller table that includes a lesser amount of information. To accomplish this, a hash function may be used on the pertinent information in the address header to determine an index value into the smaller table.
[0004] A hash function is a mathematical algorithm that is capable of mapping values from a substantially large domain to a smaller one. A “good” hash function includes those, in which the application of the hash function to a large set of values results in a smaller set of index values that are evenly distributed in the smaller domain. A “bad” hash function would be one, in which many of the values in the set from the larger domain are mapped into the same index value of the smaller domain. Any such occurrence is typically referred to as a collision. Because only a single connection can physically reside as an entry at any particular index value, any collision requires that additional information be kept in each table entry to further instruct the network where to look for any additional connections that hashed to the same index value. This chaining of entries that have the same index values requires a processing engine to hash to an index value, read out the entry, compare it to a pre-hashed five-tuple, and if a match is not found to use a pointer in the entry to read another entry. This procedure is repeated until either there is a match or the last entry in a chain is reached, reducing the efficiency of the processing engine because of the repetitive procedure being performed on every data packet.
[0005] Therefore, there is a need in the industry for an apparatus, method and system for managing network traffic through the use of an improved hash function. Thus, it is with respect to these considerations, and others, that the present invention has been made.
SUMMARY OF THE INVENTION
[0006] The present invention is directed to managing network traffic using a CRC index to hash an address header. Determining an address header from a data packet, the invention determines a CRC index based, in part, on particular fields in the address header. A group of predetermined bits is selected from the CRC index through the use of a masking register to form a final index value. The final index value is attached to the data packet as it is retrieved from a buffer forwarded to the network.
[0007] In accordance with one embodiment of the present invention, an apparatus is directed to managing a signal over a network. The apparatus includes a CRC circuit, a scaling circuit, and a reinsertion circuit. The CRC circuit is arranged to determine a CRC index based, in part, on a portion of an input signal. The scaling circuit is arranged to determine at least one bit from the CRC index. The reinsertion circuit is arranged to combine the at least one bit selected from the CRC index to the signal.
[0008] In accordance with another embodiment of the present invention, a device is directed to managing traffic over a network. The device includes a transceiver and an indexing device. The transceiver is arranged to determine an address header associated with a data packet in a flow of data packets and forward the address header to the indexing device. The indexing device is arranged to determine a CRC index based, in part, on the address header, determine a subset of bits from the CRC index, and combine the subset of bits with the data packet.
[0009] In accordance with yet another embodiment of the present invention, a method is directed to managing traffic over a network. The method includes determining an address header associated with a data packet in a flow of data packets, determining a CRC index based, in part, on the address header, selecting at least one bit from the CRC index, and modifying the data packet, in part, by combining the at least one selected bit with the data packet.
[0010] In accordance with a further embodiment of the present invention, a system is directed to managing traffic over a network. The system includes a first network device and a second network device. The first network device is arranged to determine an address header associated with a data packet, determine a CRC index based, in part, on the address header, determine at least one bit from the CRC index, and determine a modified data packet by combining the at least one bit from the CRC index with the data packet. The second network device is arranged to read the modified data packet from the first network device and route the modified data packet based, in part, on the CRC index information.
[0011] A more complete appreciation of the present invention and its improvements can be obtained by reference to the accompanying drawings, which are briefly summarized below, to the following detail description of presently preferred embodiments of the invention, and to the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Non-limiting and non-exhaustive embodiments of the present invention are described with reference to the following drawings. In the drawings, like reference numerals refer to like parts throughout the various figures unless otherwise specified.
[0013] For a better understanding of the present invention, reference will be made to the following Detailed Description of the Preferred Embodiment, which is to be read in association with the accompanying drawings, wherein:
[0014] FIG. 1 illustrates one embodiment of a network system in which the present invention may be practiced;
[0015] FIG. 2 illustrates a block diagram of one embodiment of an apparatus for determining a CRC index; and
[0016] FIG. 3 illustrates a flow diagram generally showing a process for determining a CRC index, in accordance with one embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0017] The present invention is directed to addressing the above-mentioned shortcomings, disadvantages and problems, and will be understood by reading and studying the following specification.
[0018] The present invention now will be described more fully hereinafter with reference to the accompanying drawings, which form a part hereof, and which show, by way of illustration, specific exemplary embodiments by which the invention may be practiced. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Among other things, the present invention may be embodied as methods or devices. Accordingly, the present invention may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. The following detailed description is, therefore, not to be taken in a limiting sense.
[0019] The term “coupled,” and “connected,” include a direct connection between the things that are connected, or an indirect connection through one or more either passive or active intermediary devices or components.
[0020] The terms “comprising,” “including,” “containing,” “having,” and “characterized by,” include an open-ended or inclusive transitional construct and does not exclude additional, unrecited elements, or method steps. For example, a combination that comprises A and B elements, also reads on a combination of A, B, and C elements.
[0021] The meaning of “a,” “an,” and “the” include plural references. The meaning of “in” includes “in” and “on.” Additionally, a reference to the singular includes a reference to the plural unless otherwise stated or is inconsistent with the disclosure herein.
[0022] Briefly stated, the present invention is directed towards a device and method for determining a CRC hash function for use in modifying a data packet. The present invention is further directed towards reducing a likelihood of a collision and improving a speed to perform the CRC hash function. A “good” hash function is one which produces an index that is fairly uniformly distributed throughout a reduced domain. Simple hashing functions based on addition or multiplication of input operands, essentially XOR functions, do not accomplish uniform distribution because changing a single bit in one of the input operands usually results in a single bit change in the produced index and may produce no change in the index at all. A CRC function, as employed in the present invention, as opposed to most commonly used XOR based functions is directed to accomplishing this. A single bit change in a single operand of a CRC function has an effect upon every bit of the produced index due to the CRC function's very serial-based derivation.
[0023] The following describes the CRC hash function as applied to a 32-bit data packet for use in an IPv4 Internet communication. One embodiment of a CRC polynomial for generating a random index value from the 32-bit data packet is:
X 32 +X 26 +X 23 +X 22 +X 16 +X 12 +X 11 +X 10 +X 8 +X 7 +X 5 +X 5 +X 4 +X 2 +X+1,
where the variable X represents a register, and the coefficients of the variable X represent bits that will be selected for the CRC (e.g. bit 32 , bit 26 , and the like).
[0025] Using this CRC polynomial, one may obtain a 32-bit index randomly generated for a 32-bit address header associated with the data packet. The index can be further reduced in length based, in part, on a predetermined bit mask. The index may be combined with the corresponding address header and data payload from the data packet, and reinserted into an IPv4 data stream of packets. A subsequent traffic device in the network, such as a router, a network translation device, and the like, may employ the index to further route the data packet.
[0026] The present invention is not limited to the above described CRC polynomial, and another may be used. Additionally, although a data stream comprising 32-bit data packets is employed for illustration purposes, the invention is not limited to a data width of 32-bits. Furthermore, the invention is not limited to a maximum size input operand of 32-bits. For example, a data packet containing 128-bit addresses for input operands and another CRC polynomial may be employed for a network system using an IPv6 protocol, and the like.
[0027] In software, performing the above described process may take in excess of a thousand cycles for a data packet, regardless of whether the data packet is 64-bytes or 1500-bytes long. Therefore, the use of a CRC hash function in software may be prohibitively time consuming. However, as described below, a similar set of operations may take as few as ten cycles when performed by the present invention. This may provide an increased efficiency through reduced operation time and less need for memory.
[0000] Illustrative Operating Environment
[0028] FIG. 1 illustrates one embodiment of network system 100 , in which the present invention may be practiced. As will be described in more detail below, the present invention is directed to a method and apparatus for managing network traffic in at least a portion of a network. Network system 100 may include many more, or less, components than those shown, however, those shown are sufficient to disclose an illustrative environment for practicing the invention.
[0029] As shown in FIG. 1 , network system 100 includes Local Area Network/Wide Area Networks (LAN/WANs) 102 , 104 , and 108 , and traffic devices 106 and 110 .
[0030] LAN/WANs 102 and 108 are in communication with traffic device 110 . Traffic device 106 is in communication with LAN/WAN 104 and LAN/WAN 102 .
[0031] LAN/WANs 102 , 104 , and 108 are enabled to employ any form of computer readable media for communicating information from one electronic device to another. In addition, LAN/WANs 102 , 104 , and 108 can include the Internet in addition to local area networks, wide area networks, direct connections, such as through a universal serial bus (USB) port, other forms of computer-readable media, and any combination thereof. On an interconnected set of LANs, including those based on differing architectures and protocols, a router acts as a link between LAN's, enabling messages to be sent from one to another. Also, communication links within LANs typically include twisted pair or coaxial cable, while communication links between networks may utilize analog telephone lines, full or fractional dedicated digital lines including T1, T2, T3, and T4, Integrated Services Digital Networks (ISDNs), Digital Subscriber Lines (DSLs), wireless links including satellite links, or other communications links known to those skilled in the art. Furthermore, remote computers and other related electronic devices may be remotely connected to either LANs or WANs via a modem and temporary telephone link. In essence LAN/WANs 102 , 104 , and 108 may include any communication mechanism by which information may travel between network devices.
[0032] Traffic devices 106 and 110 are configured to manage transportation of a data packet between LAN/WANs 102 , 104 , and 108 employing a CRC indexing scheme, according to one embodiment of the present invention. In another embodiment, traffic devices 106 and 100 may reside within LAN/WANs 102 , 104 , and 108 and manage internal network traffic.
[0033] Traffic devices 106 and 110 may be configured to operate as a router, a firewall, a network translation device, and the like.
[0034] FIG. 2 illustrates a block diagram of one embodiment of CRC index system 200 that may be employed within a traffic device, such as traffic devices 106 and 110 of FIG. 1 . CRC indexing system 200 may include many more or fewer components than those shown. The components shown, however, are sufficient to disclose an illustrative embodiment for practicing the invention.
[0035] As shown in FIG. 2 , CRC index system 200 includes splitter 202 , CRC circuit 204 , scaling circuit 206 , and reinsertion circuit 214 . Scaling circuit 206 comprises CRC hash store 208 , hash length store 210 , and AND'ing circuit 212 . Reinsertion circuit 214 comprises buffer 216 and combination device 218 . CRC circuit 204 , scaling circuit 206 , and reinsertion circuit 214 are an illustrative embodiment of CRC index system 200 , and may be combined, rearranged, split into smaller sub-circuits, and the like, to perform essentially the same actions.
[0036] Splitter 202 is coupled to CRC circuit 204 and buffer 216 . CRC circuit 204 is coupled to CRC hash store 208 , which in turn is coupled to one of the inputs of AND'ing circuit 212 . Hash length store 210 is coupled to another input of AND'ing circuit 212 . An output of AND'ing circuit 212 is coupled to combination device 218 along with an output of buffer 216 .
[0037] Splitter 202 is configured to receive a data packet and determine a data payload and an address header from the received data packet. The address header may include any form of network addressing information including, but not limited to an IP header five-tuple, and the like. Splitter 202 may copy the address header to CRC circuit 204 while forwarding the data packet to buffer 216 . Splitter 202 may be implemented as a decoder, shift register, and the like.
[0038] CRC circuit 204 is configured to determine a CRC index based, in part, on the address header. CRC circuit 204 may employ the CRC polynomial described above to determine the CRC index, which may be determined through a polynomial division between the address header and the CRC polynomial. In the example of a 32 bit system, applying this method to a 32-bit address header may yield a single, random 32-bit index.
[0039] CRC circuit 204 may be implemented as a shift register, an XOR-FlipFlop chain, and the like, according to one embodiment of the present invention, but may also comprise virtually any type of determination circuit, configured to determine a CRC.
[0040] CRC hash store 208 includes virtually any device configured to receive and store the CRC index. CRC hash store 208 may be implemented as a register, a memory device, and the like.
[0041] Hash length store 210 includes virtually any device configured to receive and store a predetermined bit mask for the CRC index. At least one bit from the CRC index may be selected to be used in a resultant index. The at least one bit may include one or more bits selected from a consecutive group of bits in a beginning, middle, or end region of the CRC index. The selected bits may also be a non-consecutive group of bits, such as every other bit of the CRC index, and the like. Hash length store 210 , which may be implemented as a register, a memory device, and the like, stores an index that determines which bits of the CRC index will be masked. In one embodiment, the predetermined bit mask stored in hash length store 210 may be a masking index.
[0042] AND'ing circuit 212 includes any device configured to combine an output from CRC hash store 208 and hash length store 210 to provide masked bits from the CRC index to the resultant index. Although described as an AND'ing circuit, the present invention is not limited to an AND'ing operation. For example, an “or” circuit, an XOR circuit, a comparator, and the like, may also be employed.
[0043] Buffer 216 includes virtually any device configured to receive and store the data packet during the CRC index determination and scaling actions. Buffer 216 may be implemented as a register, a memory device, and the like.
[0044] Combination device 218 includes any device configured to combine the data packet received from buffer 216 and the resultant index received from scaling circuit 206 to provide a modified data packet. The resultant index may be combined with the data packet in a variety of ways, including, but not limited to prepending the resultant index to the address header, encrypting the address header with the resultant index, and the like. Combination device 218 may be implemented as a multiplexer, a memory, an encoder, an encryption device, and the like.
[0045] The above described CRC index system 200 may be implemented as part of a traffic device. The traffic device may read the resultant index, remove the resultant index from the data packet and route the data packet to its destination. In another embodiment, the traffic device may transmit the data packet with the resultant index, in which case the routing may be employed by another traffic device. Thus, a traffic device may transmit the modified data packet from CRC index system 200 as is, or remove the resultant index and transmit the original data packet.
[0046] The improved efficiency of the present invention in hardware may be illustrated by comparing a number of clock cycles as employed by a hardware and software implementation. To calculate the CRC index for a 32-Bit word, it may be necessary to process first 6 long-words, each using a single clock cycle in CRC circuit 204 . Concurrently, the same 6 long-words are written to buffer 216 . This may be followed by two additional clock cycles, one for the release of the CRC index to CRC hash store 208 and one for AND'ing the outputs of CRC hash store 208 and hash length store 210 . Finally, two more clock cycles may be used for combining the resultant index the data packet and reinserting the data packet into a data stream. Thus, the present invention may take as few as ten clock cycles when performed in hardware for a 32-bit system. A comparable operation in software may take anywhere from many hundreds of cycles to well in excess of thousand cycles. This may make the process prohibitively time consuming for some network systems.
[0000] General Operation
[0047] FIG. 3 illustrates a flow diagram generally showing one embodiment of a process for determining a CRC index. Indexing process 300 may, for example, operate within CRC index system 200 of FIG. 2 .
[0048] As shown in FIG. 3 , indexing process 300 begins, after a start block, at block 302 , if a data packet to be indexed is received. The received data packet may be an IPv4 data packet, IPv6 data packet, and the like.
[0049] Processing proceeds to block 304 , where a data payload and an address header of the received data packet are determined. The address header, which may be an IP header, a portion of an IP five-tuple, and the like, is copied to a CRC index determination process at block 306 .
[0050] At block 306 , a CRC index is determined based, in part, on the address header. Block 306 may employ the CRC polynomial described above to determine the CRC index, where coefficients of the CRC polynomial represent bit values. A similar polynomial may be formed based on the bits of the address header, and a polynomial division is performed between the CRC polynomial and an address header polynomial. A remainder of the polynomial division provides the CRC index. In the example of a 32-bit system, in compliance with IPv4 protocol, applying this method to a 32-bit address header may yield a single, random 32-bit index.
[0051] At block 308 , at least one bit is determined from the CRC index providing a resultant index. The at least one bit may include one or more bits determined from the CRC index, including and up to all bits. These bits may be a consecutive group of bits in a beginning, middle, or end region, and the like, of the CRC index. The determined bits may also be a non-consecutive group of bits, such as every other bit of the CRC index, and the like. The group of bits determined from the CRC index determines a length of the resultant index.
[0052] At block 310 , the resultant index is combined with the data packet providing a modified data packet. Combination process may be performed by a variety of methods, including prepending, appending, and the like, the resultant index to the address header. The resultant index may also be inserted into a predetermined position inside the address header. In yet another embodiment, the address header may be encrypted with the resultant index.
[0053] The resulting modified data packet may be transmitted over a network for use in routing, and the like, based, in part, on the resultant index information. In another embodiment, routing information from the resultant index may be retrieved prior to transmittal over the network and the resultant index removed from the data packet. In this embodiment, the original data packet may be transmitted over the network. Upon completing block 310 , indexing process 300 returns to a calling process to perform other actions.
[0054] It will be understood that each block of the flowchart illustration, and combinations of blocks in the flowchart illustration, can be implemented by a combination of hardware-based systems and software instructions. The software instructions may be executed by a processor to cause a series of operational steps to be performed by the processor to produce a computer implemented process such that the instructions, which execute on the processor, provide steps for implementing some or all of the actions specified in the flowchart block or blocks.
[0055] Accordingly, blocks of the flowchart illustration support combinations of means for performing the specified actions, combinations of steps for performing the specified actions and program instruction means for performing the specified actions. It will also be understood that each block of the flowchart illustration, and combinations of blocks in the flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified actions or steps, or combinations of special purpose hardware and computer instructions.
[0056] The above specification, examples, and data provide a complete description of the manufacture and use of the composition of the invention. Since many embodiments of the invention can be made without departing from the spirit and scope of the invention, the invention resides in the claims hereinafter appended.
|
Methods, apparatus and systems are directed to managing network traffic using a variable length Cyclical Redundancy Check (CRC) index to hash an address header. The invention copies an address header of a data packet to a CRC generator. A CRC index is determined based, in part, on the address header. A subset of bits is determined from the CRC index based, in part, on a predetermined bit mask. The address header and the data payload are then combined with the subset of bits from the CRC index. The modified data packet is subsequently forwarded over a network. In one embodiment, the invention is implemented on a hardware circuit residing on a traffic device.
| 7
|
[0001] This application claims the benefit of Korean Patent Application No. P2004-89702, filed on Nov. 11, 2004, which is hereby incorporated by reference as if fully set forth herein.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a method for manufacturing a liquid crystal display (LCD) device, and more particularly, to a method for cutting a substrate using a femtosecond laser, which is capable of achieving an enhancement in productivity.
[0004] 2. Discussion of the Related Art
[0005] With the recent rapid development of information communication fields, displays adapted to display desired information are gaining importance. Of such information displays, cathode ray tubes (CRTs) have continuously enjoyed popularity by virtue of their advantages, including the reproducibility of diverse colors and superior screen brightness.
[0006] Due to the recent demand for large-size, portable, and high-resolution displays, flat panel displays are in high demand, in order to replace CRTs which are heavy and bulky.
[0007] Flat panel displays are useful in a wide and diverse range of applications from industrial and consumer uses to applications in aircraft and spacecraft.
[0008] Currently, there are several types of commercially-available flat panel displays, such as LCDs, electroluminescent displays (ELDs), field emission displays (FEDs), plasma display panels (PDPs), and the like.
[0009] Manufacturing flat panel displays generally involves singulation, or separation, of a fragile substrate into unit elements using a cutting process. Normally, a plurality of unit elements such as semiconductor chips are formed on the fragile substrate in a matrix array to produce large-scale integrated circuits.
[0010] The fragile substrates used in flat panel displays are typically manufactured from glass, silicon, or ceramics. There are two representative methods used in the cutting process for separation of the fragile substrate, namely, a dicing method and a scribing method. The dicing method involves cutting grooves on a substrate using a diamond blade having a thickness of 50 to 200 μm by rotating the blade at high speed. The scribing method involves cutting grooves onto a surface of the substrate using a scribing wheel made of a diamond to form a crack in a thickness direction of the substrate. The diamond normally has having a thickness of 0.6 to 2.0 mm.
[0011] The dicing method is suitable for cutting a substrate formed with a thin film or a convex portion at a surface of the substrate because a very thin blade is used. In the dicing method, heat is generated from friction at a region where the blade cuts the substrate. Furthermore, because the cutting process is performed with cooling water being supplied to the cutting region, the dicing method is not considered to be a method suitable for a flat panel display that includes metal portions such as metal electrode layers or metal terminals.
[0012] It is often difficult to completely remove the cooling water after the cutting process. If moisture from the cooling water is not completely removed, the metal portions of the flat panel display may be eroded or rusted. Furthermore, the dicing method typically takes more time than the scribing method, lowering productivity and manufacturing efficiency.
[0013] Cooling water is not required when cutting a substrate using the scribing method, which makes the scribing method a more efficient process than the dicing method.
[0014] FIG. 1 is a sectional view illustrating a general LCD device. This LCD device is manufactured in accordance with the following method. For simplicity, the following description will be given only in conjunction with one pixel region, although the formation of all pixel regions is typical of this description.
[0015] As shown in FIG. 1 , a gate electrode 11 that is made from a conductive material, such as metal, is first formed at a predetermined region on a first transparent substrate 10 . A gate insulating film 12 made of a silicon nitride (SiNx) or silicon oxide (SiO 2 ) is then applied over the entire upper surface of the first substrate 10 including the gate electrode 11 .
[0016] Thereafter, an active layer 13 made of amorphous silicon is placed on the gate insulating film 12 at a region corresponding to the gate electrode 11 . An ohmic contact layer 14 is formed on the active layer 13 at regions corresponding to respective lateral edge portions of the active layer 13 . The ohmic contact layer 14 is made of a doped amorphous silicon.
[0017] Source and drain electrodes 15 and 16 , which are made of a conductive material such as metal, are subsequently applied on the ohmic contact layer 14 . The source and drain electrodes 15 and 16 constitute a thin film transistor T, together with the gate electrode 11 .
[0018] Meanwhile, although not shown, the gate electrode 11 is connected to a gate line, and the source electrode 15 is connected to a data line. The gate line and data line cross each other, and define a pixel region.
[0019] A protective film 17 is then formed over the entire upper surface of the first substrate 10 including the source and drain electrodes 15 and 16 . The protective film 17 is made of a silicon nitride, silicon oxide, or organic insulating material. The protective film 17 has a contact hole 18 through which a predetermined portion of the surface of the drain electrode 16 is exposed.
[0020] Thereafter, a pixel electrode 19 , which made of a transparent conductive material, is applied to the protective film 17 at the pixel region. The pixel electrode 19 is connected to the drain electrode 16 via the contact hole 18 .
[0021] A first orientation film 20 is then formed over the entire upper surface of the first substrate 10 including the pixel electrode 19 . The first orientation film 20 is made of, for example, polyimide, and has a surface on which the molecules of the first orientation film 20 are oriented in a predetermined direction.
[0022] Meanwhile, a second transparent substrate 31 is arranged over the first substrate 10 while being vertically spaced apart from the first substrate 10 by a predetermined distance.
[0023] A black matrix 32 is formed on a lower surface of the second substrate 31 at a region corresponding to the thin film transistor T of the first substrate 10 . Although not shown, the black matrix 32 also covers a region other than the pixel electrode 19 .
[0024] A color filter 33 is then formed on the second substrate 31 beneath the black matrix 32 . Practically, color filters are arranged in the form of repeated filter patterns of red (R), green (G), and blue (B), each of which corresponds to one pixel region.
[0025] A common electrode 34 made of a transparent conductive material is subsequently formed on the second substrate 31 beneath the color filter 33 . A second orientation film 35 is then formed on the second substrate 31 beneath the common electrode 34 . The second orientation film 35 is made of, for example, polyimide, and has a surface on which the molecules of the second orientation film 35 are oriented in a predetermined direction. A liquid crystal layer 40 is sealed between the first orientation film 20 and the second orientation film 35 .
[0026] The above-described LCD device is manufactured using an array substrate fabrication process that involves the formation of thin film transistors and pixel electrodes on a substrate to fabricate an array substrate, a color filter substrate fabrication process involving formation of color filters and a common electrode on another substrate to fabricate a color filter substrate, and a liquid crystal panel fabrication process involving the arrangement of the two fabricated substrates, the injection and sealing of a liquid crystal material, and the attachment of polarizing plates to fabricate a liquid crystal panel.
[0027] FIG. 2 is a flow chart illustrating a general LCD manufacturing method.
[0028] In accordance with this method, a thin film transistor (TFT) array substrate including TFTs and a color filter substrate including color filters are first prepared (S 1 ), as shown in FIG. 2 .
[0029] The TFT array substrate is fabricated by repeatedly performing the processes of depositing a thin film and patterning the deposited thin film. In this case, the number of masks used for patterning the thin films in the fabrication of the TFT array substrate represents the number of processes used in the fabrication of the TFT array substrate. Currently, research is being performed to reduce the number of masks, and thus, to reduce the manufacturing costs.
[0030] The color filter substrate is fabricated by sequentially forming a black matrix for preventing light from being leaked through a region other than from pixel regions, R, G, and B color filters, and a common electrode. The color filters may be formed using a dyeing method, a printing method, a pigment dispersion method, an electro-deposition method, or the like. Currently, the pigment dispersion method is most often used. Thereafter, an orientation film is formed over each substrate to determine an initial alignment direction of liquid crystal molecules (S 2 ).
[0031] The formation of the orientation film is achieved using a process for coating a polymer thin film, and treating the surface of the polymer thin film such that the molecules of the polymer thin film on the treated surface are oriented in a predetermined direction. Generally, polyimide-based organic materials are mainly used for the orientation film. A rubbing method is generally used for the orientation method.
[0032] In accordance with the rubbing method, the orientation film is rubbed in a predetermined direction using a rubbing cloth. This rubbing method is suitable for mass production because it is possible to easily achieve treatment for orientation. Also, the rubbing method has advantages of stable orientation and easy control of pretilt angle.
[0033] An optical orientation method has also been developed and used which achieves orientation using polarized beams.
[0034] Next, a seal pattern is formed at one of the two substrates (S 3 ). The seal pattern is arranged around a region where an image is displayed. The seal pattern has a port for injection of a liquid crystal material, and serves to prevent the injected liquid crystal material from being leaked.
[0035] The seal pattern is formed by applying a thermosetting resin layer in a predetermined pattern. A screen printing method using a screen mask is used when forming the seal pattern. Alternatively, a method using a seal dispenser may also be used.
[0036] The screen printing method has a drawback in that products of poor quality may be produced if the screen mask comes into contact with the orientation film. Furthermore, the screen mask process becomes more difficult and error prone with increased substrate sizes. Therefore, the seal dispenser method is being used more often because it does not have the disadvantages of the screen printing method.
[0037] Subsequently, spacers having a predetermined size are sprayed on one of the TFT array substrate and color filter substrate to maintain an accurate and uniform space between the two substrates (S 4 ).
[0038] A wet spray method is used to spray the spacers, which involves spraying the spacers while mixed with alcohol. Additionally, a dry spray method can be used wherein spacers are sprayed without alcohol. There are two types of dry spraying methods, an electrostatic spray method using static electricity, and an ionic spray method using pressurized gas. Since LCDs are weak against static electricity, the ionic spray method is preferred.
[0039] Thereafter, the two substrates of the LCD, i.e., the TFT array substrate and color filter substrate, are arranged such that the seal pattern is interposed between the substrates. In this state, the seal pattern is cured under pressure to join the substrates (S 5 ). In this orientation, the orientation films of the substrates face each other, and the pixel electrodes and color filters correspond to each other in a one-to-one relationship. Next, the joined substrates are cut, or singulated, into liquid crystal panels (S 6 ).
[0040] Generally, a plurality of liquid crystal panels, each of which will be one LCD device, are formed on one substrate sheet, and are then separated into individual panels. This is done to improve the manufacturing efficiency and reduce the manufacturing costs.
[0041] The liquid crystal panel cutting process includes a scribing process for forming a crack in a surface of each substrate using a scribing wheel made of a diamond material having a hardness higher than that of the substrate, which may be made from glass or similar materials, and a breaking process for positioning a breaking bar at a portion of the substrate where the crack is formed. After the breaking bar is positioned on the substrate, a predetermined pressure is applied to the breaking bar, thereby cutting the substrate in a direction along which the crack extend.
[0042] Subsequently, a liquid crystal material is injected between the two substrates of each liquid crystal panel (S 7 ). A vacuum injection method is often used to inject the liquid crystal, which utilizes a pressure difference between the interior and exterior of the liquid crystal panel. Micro air bubbles may be present in the liquid crystal injected into the interior of the liquid crystal panel, which cause the liquid crystal panel to have poor quality. In order to prevent such a problem, it is necessary to perform a de-bubbling process in which the liquid crystal is maintained in a vacuum state for a prolonged time to remove bubbles.
[0043] After completion of the liquid crystal injection, the injection port is sealed to prevent the liquid crystal from being outwardly leaked through the injection port. The injection port is sealed by coating the injection port with an ultraviolet-setting resin, and the coated resin is irradiated with ultraviolet rays, which sets the coated resin. Next, polarizing plates (S 8 ) are attached to the outer surfaces of the liquid crystal panel and finally, driving circuits are connected to the liquid crystal panel.
[0044] A conventional substrate cutting apparatus and a conventional substrate cutting method using the same will be described with reference to the figures.
[0045] FIG. 3 is a schematic view illustrating a conventional scribing device. The conventional scribing device includes a table 51 , on which a substrate G is laid, and a vacuum chucking unit adapted to fix the substrate G to the table 51 . Additionally, the conventional scribing device includes and a pair of parallel guide rails 52 for pivotally supporting the table 51 in a suspended state while allowing the table 51 to be movable in a Y-axis direction. The scribing device also includes a ball screw 53 for moving the table 51 along the guide rails 52 , a guide bar 54 installed above the table 51 such that the guide bar 54 extends in an X-axis direction, and a scribing head 55 mounted on the guide bar 54 such that the scribing head 55 is slidable in the X-axis direction along the guide bar 54 . The scribing device further includes a motor 56 for sliding the scribing head 55 , a tip holder 57 mounted to a lower end of the scribing head 55 to be vertically movable as well as rotatable, and a scribing wheel 1 rotatably mounted to a lower end of the tip holder 57 .
[0046] In the conventional substrate cutting method using the above-mentioned scribing device, a crack with a predetermined depth is formed in a substrate to be cut, based on the rotation of the scribing wheel 1 . The substrate with the crack is then fed into a breaking device, which applies pressure to the substrate along the crack using a breaking bar to cut the substrate.
[0047] FIGS. 4 and 5 are schematic views respectively illustrating scribing and breaking processes involved in the conventional substrate cutting method. In the scribing process as shown in FIG. 4 , a scribing or cutting wheel 82 makes contact with the surface of a substrate 81 . The scribing wheel 82 is rotated along the substrate 81 while applying a pressure of about 2.40 Kgf/cm 2 to the substrate 81 , which forms a crack 83 having a predetermined depth on the surface of the substrate 81 along the track of the scribing wheel 82 .
[0048] Next, the breaking process to cut the substrate 81 is performed along the crack 83 formed to the predetermined depth in the surface of the substrate 81 . As shown in FIG. 5 , a breaking bar 84 is arranged on the substrate 81 along the line of the crack 83 . The portion of the breaking bar 84 that contacts the substrate 81 is made of a material such as urethane rubber that is sufficiently hard, but does not form scratches on the surface of substrate 81 .
[0049] Pressure is momentarily applied to the substrate 81 with the breaking bar 84 , which causes the crack 83 to be extended and splits the substrate along the line of the crack.
[0050] Thereafter, a grinding process is then performed using a grindstone having a predetermined mesh size, to grind the cut surfaces and corners of the substrate formed during the scribing and breaking processes.
[0051] This conventional substrate cutting method has various problems or disadvantages. One major disadvantage is that the scribing wheel used for cutting the substrate is expensive and has a short lifespan, which requires periodic replacement of the scribing wheel. The scribing wheels are relatively expensive and the replacement cost is a large percentage of the manufacturing cost of the units. For this reason, an increase in manufacturing costs is incurred.
SUMMARY OF THE INVENTION
[0052] A method for cutting a substrate using a femtosecond laser is provided. The method comprises the steps of providing a substrate on a stage, and irradiating a femtosecond laser to a predetermined portion of the substrate arranged on the stage, thereby cutting the substrate along the predetermined substrate portion.
[0053] Additional advantages, objects, and features of the invention will be set forth in the description which follows and will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
[0054] It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0055] The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principle of the invention. In the drawings:
[0056] FIG. 1 is a sectional view illustrating a general LCD;
[0057] FIG. 2 is a flow chart illustrating a general LCD manufacturing method;
[0058] FIG. 3 is a schematic view illustrating a conventional scribing device;
[0059] FIGS. 4 and 5 are schematic views respectively illustrating scribing and breaking processes involved in the conventional substrate cutting method;
[0060] FIG. 6 is a schematic view explaining a method for cutting a substrate using a femtosecond laser in accordance with the present invention; and
[0061] FIG. 7 is a photograph showing the cut state of the substrate after the substrate cutting process is carried out using the femtosecond laser in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0062] Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts.
[0063] Generally, ablation, or cutting by a laser, is used in manufacturing high-accuracy precise elements. High-speed laser pulses are used because these reduce damage to the substrate around the region where the laser pulses are irradiated. Because of this advantage in using lasers with high-speed pulses, laser machines using a YAG laser, or excimer laser, having a pulse speed on the order of nanoseconds, i.e., 10 −9 m/s, are generally used in applications where high accuracy substrate cuts are required. These machines are called a “nanosecond laser machines.”
[0064] However, YAG laser machines, in which an aluminum oxide is artificially crystallized to generate a laser, are problematic because side walls machined by a YAG laser tend to be rough. Carbon dioxide lasers, which are infrared-based, often form craters at the machined region. Therefore, CO 2 lasers cannot be used for a micro machining process that requires accuracy in the order of micrometers or higher.
[0065] The laser machines described above are often referred to as a “thermal laser machining,” because the machining is performed using thermal energy changed from optical energy. It is difficult to achieve precise machining using these machines because the machined structure may be easily collapsed when using thermal laser machines.
[0066] On the other hand, in the case of an excimer laser, sublimate etching is performed with an opto-chemical reaction that causes disconnection of the covalent bonds between carbon atoms. Very precise machining is possible using this process. That is, when an excimer laser is irradiated to the surface of an object to be machined, the irradiated surface of the object is dissipated by forming plasma and shock noise.
[0067] However, the energy of an excimer laser is not completely used for the disconnection of the covalent bonds of carbon atoms. Instead a portion of the excimer laser energy is converted to thermal energy. The effect of the converted thermal energy is considerable because the excimer laser energy has a high density. Therefore, it is difficult to machine mineral materials using the excimer laser such as metal, ceramic, silicon, quartz, and glass that have a low photo absorption rate. Thermal deformation generated by an excimer laser adversely affects the durability of the machined product, even through the thermal deformation is less than that produced with thermal laser machining.
[0068] On the other hand, a femtosecond laser, which has a pulse speed of approximately 10 −15 m/s, has superior characteristics that are capable of solving the above-described problems. It is possible to obtain a very high oscillation density of laser energy by using a laser that oscillates with an ultra-short pulse radiation duration of 1 picosecond (1×10 −12 m/s) or shorter.
[0069] When a laser has photo energy of 1 mJ, and a pulse radiation duration of 100 femtoseconds or shorter, the energy density of the laser reaches a level of about 10 Gigawatts. Under these circumstances, it is possible to accurately machine nearly any material.
[0070] Meanwhile, when an ultra-short pulse laser, such as a femtosecond laser, is radiated to an object to be machined, a multiphoton phenomenon occurs in the lattices of the material of the object, which causes the atoms within the material to be excited. However, the incident laser pulse duration is shorter than the time required for photons to transfer heat to the lattices around the photons during the excitation of the atoms. Therefore, it is possible to accurately machine a substrate without the problems associated with other equipment and methods, such as, thermal degradation, physical and chemical variation in the properties of the material due to the machining process, and partial melting of the machined portion of the object.
[0071] Moreover, particles do not accumulate during the femtosecond laser machining, and little or no byproducts, or craters are formed. Therefore, when using the femtosecond laser, it is unnecessary to use a byproduct removing process, such as an ultrasonic cleaning process, as is required when using conventional cutting methods.
[0072] Additionally, it is possible to machine a material that has a high heat transfer coefficient or a low photo absorption rate. It is also possible to machine two or more different materials, or a composite material having a multi-layer structure, using a single process.
[0073] Hereinafter, a method for cutting a substrate using a femtosecond laser in accordance with the present invention will be described with reference to the annexed drawings.
[0074] FIG. 6 is a schematic view explaining the method and components used in cutting a substrate using a femtosecond laser in accordance with the present invention. A femtosecond laser generating apparatus according to the present invention is illustrated. The femtosecond laser generating apparatus includes a femtosecond laser oscillator 200 for generating a femtosecond laser 201 and a condenser lens 210 for focusing the femtosecond laser 201 emitted from the femtosecond laser oscillator 200 onto a substrate 100 to be cut.
[0075] In accordance with the method of the present invention, the femtosecond laser 201 generated from the femtosecond laser oscillartor 200 having the above-described configuration is irradiated to the substrate 100 , thereby cutting the substrate 100 .
[0076] Since the femtosecond laser 201 has a short pulse width (about 150 fs) and a high peak power per pulse, thermal expansion and generation of shock waves do not occur around a portion of the substrate 100 that is cut during the cutting operation.
[0077] Meanwhile, the femtosecond laser has characteristics different from those of general lasers. The femtosecond laser has a considerably wide spectrum range, while typical lasers are normally monochromatic.
[0078] Also, the femtosecond laser is amplified through the condenser lens 210 and has a peak power on the order of terawatts (10 12 watts), which is much higher than those of general lasers. Recently, such an amplified femtosecond laser has exhibited a peak power increased to petawatts (10 15 watts). The femtosecond laser may be called a “T3 laser” (Table Top Terawatt Laser). It is possible to greatly increase the density of the laser by simply condensing the laser through a condenser lens. Accordingly, because the energy of the laser can be constrained into a small area with a condenser lens, the material of the focus point of the laser is transformed to a plasma state, virtually instantly.
[0079] Normally, a femtosecond laser exhibits a pulse energy on the order of micro-Joules (μJ) per pulse. In some cases, the femtosecond laser uses stronger pulse energy, on the order of milli-Joules per pulse, corresponding to mean power of about 1 Watt.
[0080] Normally, plasma generated by a laser reacts with the laser light to absorb the laser or to heat the material to be machined. As a result, such plasma causes various problems such as increased heating, unstable machining, and degradation in efficiency. However, the femtosecond laser changes such circumstances caused by plasma.
[0081] Generally, the laser energy is received by an acceptor electron at the side of the material being machined. In the case of a metal, the acceptor is a free electron existing in a conduction band or an electron excited into the conduction band by light. The electron (electron system) is vibrated by a vibrating electric field of the laser. In other words, the electron receives energy from the laser. The vibrating electron strikes atoms or ions in the lattices of the material (lattice system), transferring kinetic energy to the atoms or ions. This transfer of energy causes an increase in the material's temperature. As a result, the phase of the material is changed (by either melting or evaporation), which causes the material to be machined.
[0082] For example, the time taken for the atoms of the irradiated material to be ionized, and thus, to generate plasma, is longer than the pulse width of the femtosecond laser. Accordingly, with femtosecond machinging it is expected that the plasma will not react with the laser. Furthermore, the time taken for the heat generated at the irradiated region to be diffused around the irradiated region is longer than the pulse width of the femtosecond layer. The energy of the laser exists locally in the irradiated region, so that the phase change of the material occurs only in the irradiated region.
[0083] Thus, when a substrate is cut using the femtosecond laser in accordance with the present invention, the cutting is achieved without formation of a heat affected zone around the region where the cutting is carried out.
[0084] Hereinafter, the substrate cutting method using the femtosecond laser according to the present invention will be described in more detail in conjunction with the femtosecond laser generating apparatus of FIG. 6 .
[0085] In accordance with this substrate cutting method, a substrate 100 , which is a mother substrate formed with a plurality of liquid crystal panels that are to be cut into unit liquid crystal panels, is first arranged on a movable stage ( 220 ). Thereafter, a femtosecond laser 201 is generated from the femtosecond laser oscillator 200 .
[0086] Meanwhile, when the femtosecond laser 201 is generated from the femtosecond laser oscillator 200 , the cutting position on the substrate is identified using the CCD camera ( 230 ). Also, an image of the substrate 100 is displayed in order to aid in accurate cutting of the substrate 100 .
[0087] Subsequently, the intensity and density of the femtosecond laser 201 generated from the femtosecond laser oscillator 200 are adjusted. The adjusted femtosecond laser 201 is focused by the condenser lens 210 , and irradiated onto a cutting surface of the substrate 100 . Thereafter, the substrate 100 is cut while moving the stage in one direction in accordance with a signal from a controller (not shown). Alternatively, the substrate 100 cut while moving the femtosecond laser oscillator 200 in one direction in a fixed state of the stage. A monitoring device (not shown) may be additionally provided in order to allow the operator to check the cutting condition during the cutting process.
[0088] FIG. 7 is a photograph showing the cut state of the substrate after the substrate cutting process is carried out using the femtosecond laser in accordance with the present invention. It can be seen that the substrate 100 was uniformly and accurately cut in a desired cutting direction under the condition in which the cutting width was about 40 μm. This is because neither thermal expansion nor generation of shock waves occurred around the region where the cutting was carried out. Thus, when the substrate is cut using the femtosecond laser, it is possible to accurately and cleanly cut the substrate without formation of paddings or deposits on the edge and side surfaces of the cut substrate portion.
[0089] It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. Thus, it is intended that the present invention covers the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
[0090] As apparent from the above description, the substrate cutting method using the femtosecond laser according to the present invention has various effects. That is, the femtosecond laser used in accordance with the present invention has a short pulse width and high peak power, so that neither thermal expansion nor generation of shock waves occurs around a region where cutting is carried out. Additionally, the femtosecond laser does not require the periodic replacement of a scribing wheel incurred in conventional cases, which reduces manufacturing costs.
|
A method for cutting a substrate is disclosed which uses a femtosecond laser capable of preventing thermal expansion and generation of shock waves from occurring around a region where a cutting process is carried out when the femtosecond laser is used to cut the substrate, thereby being capable of achieving a reduction in costs. The method includes the steps of arranging the substrate on a stage, and irradiating a femtosecond laser to a predetermined portion of the substrate arranged on the stage, thereby cutting the substrate along the predetermined substrate portion.
| 1
|
BACKGROUND OF THE INVENTION
The present invention relates in general to a sewing machine, and in particular to a zipper foot for use with a sewing machine.
A zipper foot is a device that is used on a sewing machine whenever the machine is to be employed to sew a zipper into a garment or the like. Conventionally, the zipper foot is composed of the actual foot and a supporting member that is integral with the foot and which is releasably securable to the upright presser bar of the sewing machine. Whenever the machine is to be used to sew a zipper in place, the zipper foot is installed on the presser bar; however, because the zipper foot interferes with the use of the machine for applications other than sewing a zipper, for example for merely sewing a conventional seam, it is necessary to remove the zipper foot with its supporting member for the presser bar whenever the machine is to be used for any application other than sewing of a zipper. The zipper foot is then replaced with a presser foot that is connected to the presser bar.
The necessity for frequently exchanging the usually employed presser foot with the zipper foot, and vice versa, is troublesome and time consuming, especially in industrial applications, because the time loss involved of course results in a decrease of the sewing efficiency. This is particularly true because it is absolutely necessary whenever the zipper foot is employed, to so adjust the zipper foot with respect to the needle hole of the throat plate when it is installed on the pressure bar, that the needle will be able to operate properly. This adjustment is the primary reason for the time-consuming installation. Any error in installing the zipper foot may cause breakage of the needle and/or improperly formation of stitches.
SUMMARY OF THE INVENTION
It is therefore a general object of the present invention to overcome the aforementioned disadvantages.
More particularly, it is an object of the invention to provide an improved zipper foot arrangement which is not possessed of these disadvantages.
An additional object of the invention is to provide such an improved zipper foot which can be readily attached to and removed from a supporting member, and which latter in turn can be secured to the presser bar of a sewing machine.
A further object of the invention is to provide an improved zipper foot which can be adjusted relative to the supporting member in respective predetermined positions so that both sides of the zipper, that is the two tapes of the zipper, can be readily sewn in place.
An additional object of the invention is to provide such an improved zipper foot which need not be removed, even when the machine is used for applications other than sewing a zipper in place.
In keeping with these objects, and others which will become apparent hereafter, one feature of the invention resides, in a sewing machine having a presser bar, in a combination which comprises a supporting member that is adapted to be mounted on the presser bar of the machine, a zipper foot, and connecting means which adjustably connects the zipper foot with the supporting member.
The invention makes it possible to shift rapidly and simply from normal sewing to zipper sewing, and back, without requiring the removal of the zipper foot at any time for normal sewing, or requiring installation of the zipper foot for zipper sewing. All that is required is a simple adjustment in the position of the zipper foot.
However, if for any reason it is desired to replace the zipper foot with a conventional presser foot, then the present invention still makes this possible in a simple manner because the zipper foot can be attached to and detached from the supporting member which itself can remain in place on the presser bar. A further advantage of the present invention is that the novel zipper foot is capable of cooperating with the feed dogs of the sewing machine, in order to properly and positively feed the stitched zipper, and thereby to raise the sewing efficiency.
The novel features which are considered as characteristic for the invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together with additional objects and advantages thereof, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view, illustrating a zipper-foot supporting member which is a part of the device according to the present invention;
FIG. 2 is a bottom perspective view of FIG. 1;
FIG. 3 is a perspective view, illustrating a zipper foot according to the present invention, for use with the supporting member in FIGS. 1 and 2;
FIG. 4 is a partly sectioned top view of the top plan view of the device of the present invention, showing the zipper foot of FIG. 3 installed on the supporting member of FIGS. 1 and 2 and illustrating the zipper foot in one adjusted position;
FIG. 5 is similar to FIG. 4, but showing the zipper foot in another adjusted position;
FIG. 6 is a cross sectional view, illustrating a zipper being stitched on a garment by use of the device according to the present invention, with the zipper foot being in the adjusted position shown in FIG. 4; and
FIG. 7 is a view similar to FIG. 6, but showing the zipper being stitched in place with the zipper foot adjusted to the position of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring firstly to FIGS. 1 and 2 it will be seen that reference numeral 1 identifies a supporting member having a portion 11 by means of which it is mounted on a vertically oriented presser bar of a sewing machine. The sewing machine itself is not illustrated because it is not needed for an understanding of the invention. A portion of the presser bar is shown in phantom lines. The supporting member 1 has a lower free end portion 12 having a transverse width X (see FIG. 2) and being formed in a surface which in operation faces downwardly (i.e. towards the material being sewn) with a groove 13 extending across the width, that is transverse to the vertical orientation of the presser bar. The portion 12 has an additional groove 14 (compare FIG. 1) a lower end of which extends to and is open at the surface in which the groove 13 is formed. A spring 4 is mounted on the supporting member 1 as shown and has a hook-shaped lower end portion 41 which is lodged in the groove 14 and which in part extends transversely across the groove 13. A pin 42 is mounted in the supporting member 1 and can be shifted axially of itself by exerting pressure upon its exposed head 43; when this is done, the free end portion of the pin 42 presses against the spring 4 (see FIG. 1) and deflects the spring so that the hook-shaped end portion 41 of the spring is deflected transversely of and out of the groove 13, as a comparison of FIGS. 1 and 2 clearly shows. This retraction of the end portion 41 from the groove 13 will, of course, last only as long as pressure is maintained on the head 43 of the pin 42. A further groove 15 is also formed on the same surface in which the groove 13 is formed, but extends in direction normal to the elongation of the groove 13, i.e. in the direction in which the material being sewn is to be fed.
The zipper foot 2 which together with the supporting member 1 of FIGS. 1 and 2 constitutes an assembly, as illustrated in FIG. 3. It has a base plate 20 that is formed in its opposite lateral edges with recesses or needle holes 21, 22; these are open in outward direction of the lateral edges. An upper surface of the base plate 20 has provided on it a frame 27 having two transversely spaced side walls 23 and 24. A pin 3 is firmly mounted in the side walls 23 and 24 and extends from one to the other thereof across the width of the space located between the side walls, which width is identified with reference character Y. This width is substantially in excess of the dimension X of the supporting member 1.
A pair of upright projections 25 and 26 are fixedly arranged in spaced relation on the upper surface of the base plate 20, inwardly of the side walls 23 and 24 and rearwardly of the pin 3. The transverse thickness of the projections 25 and 26 correspond substantially to the width of the groove 15, and the projections 25 and 26 are intended to be respectively introduced into this groove 15 to thereby position the zipper foot 2 in one or another predetermined lateral position relative to the supporting member 1, that is in a rightwardly displaced position or a leftwardly displaced position. The base plate 20 also has guide edges 18 and 19 on the opposite lateral sides, as shown in FIGS. 4 and 5.
To secure the zipper foot 2 to the supporting member 1 it is merely necessary to so position it that the groove 13 receives the pin 3, for which purpose the pin 43 is depressed to retract the end portion 41 of the spring 4 out of the groove 13. Once the pin 3 is received in the groove 13, pressure on the pin 42 is released and the end portion 41 of the spring 42 moves back across the groove 13 and now retains the pin 3 in this groove.
It is one of the important advantages that the connection between the foot 2 and the supporting member 1 may be maintained at all times, except possibly for brief adjusting periods, whether or not a zipper is to be sewn onto the garment or other article. In other words, when no zipper is to be sewn, then the foot 2 will assume a certain position with reference to the supporting member 1, and when a zipper is subsequently to be sewn, then it is merely necessary to change the position of the foot 2 relative to the supporting member 1 slightly and in a very simple manner, as will be described subsequently.
When a basic seam S or S' is to be stitched, the foot 2 is merely so shifted --after first disconnecting it from the supporting member 1 and inserting one of the upright projections 25 or 26 in the groove 15 of the supporting member 1-- that the guide edges 18 and 19 of the base plate 20 are properly located, these guide edges serving either for the right or for the left hand stitching in a zigzag sewing machine.
FIGS. 4 and 5 show how the foot 2 is arranged when a zipper is to be stitched in place on a garment or the like. It is clear that in FIG. 4 the projection 25 is received in the groove 15, whereas in FIG. 5 the projection 26 is received in the groove 15.
FIG. 4 shows the position of the zipper foot 2 when the tape 9 at the right-hand side of the actual zipper mechanism 8 is to be stitched (compare FIG. 6), whereas FIG. 5 shows the position of the zipper foot 2 when the tape 9 to the left-hand side of the zipper mechanism 8 is to be stitched (compare FIG. 7). The basic needle lines in FIGS. 4 and 5 are inwardly spaced from the corresponding guide edges 18 and 19 by the distance L or L', so as to stitch portions of material (i.e. the tape 9) which are laterally spaced from the actual zipper mechanism 8. Reference numerals 5, 6 and 7 represent feed dogs of the sewing machine. In FIG. 4, the feed dog 5 is located beneath the zipper 8 while the feed dogs 6 and 7 are located under the base plate 20. In the adjusted position of the zipper foot 2, one side of the zipper is being stitched, whereas in FIG. 5 the feed dogs 5 and 6 are located under the base plate 20 and the feed dog 7 is located under the zipper 8 so that in this position of the zpper foot, the other side of the zipper 8 is being stitched.
If for any reason a disengagement of the zipper foot 2 from the member 1 is desired, for example to permit connection of a differnet foot which might be required for a different sewing operation, this can be readily and rapidly carried out in the manner described earlier. The device of the invention may be made of metal or synthetic plastic material, for example by die casting or the like.
The principle of the invention can be applied to a straight stitching sewing machine as well as to a zigzag sewing machine.
This invention has been applied to a zigzag sewing machine stitching with the maximum width of about 7 mm which is presently and generally available. This principle of invention, however, could be applied to a zigzag sewing machine stitching with larger maximum width of about 10 mm. In such an instance, it will be apparent that the base plate 20 of zipper foot 2 is made wider in accordance with the more widely spaced arrangement of feed dogs 5 and 7 of the zigzag machine, and that the upright projections 25, 26 are accordingly arranged in more spaced relation to each other. In this widened space between the projections on the upper side of base plate 20, at least additional projection just like the projections 25, 26 can be provided, so that the projection may be inserted into the groove 15 of supporting member 1. In such a manner, it will also be apparent according to the present invention that the needle positions for sewing a zipper onto the garment or the like can be more variously selected with respect to zigzag sewing machines which could make zigzag stitches of larger maximum width, by providing one or more additional upright projections on the upper side of so widened base plate 20.
It will be understood that each of the elements described above, or two or more together, may also find a useful application in other types of constructions differing from the types described above.
While the invention has been illustrated and described as embodied in a zipper foot for use with zigzag sewing machines, it is not intended to be limited to the details shown, since various modifications and structural changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can, by applying current knowledge, readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention.
|
A supporting member is removably attached to an upright presser bar of a sewing machine, and a zipper foot is attached to the supporting member so as to be removable therefrom. The position of the zipper foot on and with reference to the supporting member can be changed in direction transversely of the upright presser bar of the sewing machine, to thereby make it possible to move the zipper foot to positions in which the sewing machine can be used to sew a zipper, and to a position in which the sewing machine can be used for other work not involving the sewing of a zipper; this eliminates the need for removing the zipper foot at such times when the machine is not used to sew a zipper.
| 3
|
This application is a continuation of copending application Ser. No. 879,254, filed Feb. 21, 1978, now abandoned.
BACKGROUND OF THE INVENTION
The invention relates to bore hole flow meters, and in particular, to a rotary bore hole flow meter which accurately detects and digitally interprets both the direction and the rate of fluid flow within the bore hole.
In the extraction of oil and other petroleum products from the earth, a bore hole is drilled down through multiple strata of earth. The bore hole is conventionally lined with a tubular casing which is selectively perforated to provide communication between oil producing strata and the bore hole. Fluids are conducted from the lower open end of the tubing, back up the bore hole to the surface. In a conventional well, it is desirable to be able to measure the rate of flow of the fluid and the direction of flow thereof by use of a tool which can be temporarily lowered into the bore hole to make such measurement.
In certain other types of petroleum production, a technique known as "water flooding" is employed, wherein water is pumped through a first bore hole to enter surrounding earth strata or formations and force oil contained in the strata into an adjoining producing well. That is, in petroleum production, fluids are forced both into subterranean formations and withdrawn from subterranean formations from various bore hole locations. Consequently, it is desirable to have a means for measuring, downhole, both the direction of flow as well as the rate of flow of fluids within the bore hole. It is preferred to have a simple and accurate flow meter which may be lowered into the bore hole at different depths and which will indicate both the direction and the rate of the flow of the fluids therein.
Prior art flow meter tools for boreholes have included devices for use in well bores with and without packers. Such flowmeters generally include a passageway open at inlet and outlet orifices to the exterior of the tool and a spinner section which measures the rate of fluid flow through the passageway. In a packer-type flowmeter, the horizontal cross section of the well bore, say seven inches in diameter, is packed off and the entire fluid flow is directed through the tool for fairly low rates of flow therein sampling the flow.
In a typical flowmeter spinner section, a spinner is rotated under the influence of the fluid flow at an angular velocity proportional to the velocity of the fluid flow, and the rotation is directed by a sensing system to provide an indication of the velocity of fluid flow. In the typical spinner assembly, particularly for low rates of fluid flow, it is difficult to physically mount the spinner for perfectly free rotation and to detect the true angular velocity of the spinner to provide accurate indications because of friction forces and other retarding forces in the assembly. Such retarding forces include spinner bearing resistance as well as sensor inertial and functional resistances.
Certain problems in prior art flowmeters are the results of the aforesaid resistance aspects of the tool. For example, it is desirable to detect very low fluid velocities in the range of ten to twenty feet per minute. Moreover, the use of packers is not always feasible or practical. Flow meters utilizing spinners or similar propeller structures having low performance efficiency may critically reduce the sensitivity of the tool. Flowmeter sensor units incorporating conventional magnetic pick-up units may also adversely affect sensitivity through start up torque and inertial resistance. Additionally, most prior art sensor units utilize a basic analog signal network which is sensitive to changes in temperature and subject to undiagnosed component error or failure; with low fluid velocities and/or related turbulence in the borehole, signal errors can be critical to proper logging operations and detection of fluid flow direction as well as flow rate.
It is equally important to detect and monitor fluid flow direction with equal sensitivity and accuracy. Many prior art units discriminate between analog signals to distinguish direction; but spinner efficiency, bearing resistance and component eror can render ineffective proper downhole monitoring of direction, as well as rate. In packerless designs, such factors as laminar flow conditions can alter flow reading accuracy, particularly between opposing flow directions. For example, a laminar flow condition will exist from a downward flow from the tool string to the spinner or related propeller element. The same condition will not exist in an upward flow. With the added sensitivity, fluctuations due to temperature and end loading resistance on certain prior art constructions, low or erratic fluid flow can remain undetected or recorded with any degree of accuracy.
It would be an advantage therefore, to overcome the aforesaid problems and disadvantages of prior art flowmeters. The flowmeter apparatus of the present invention is provided in a highly sensitive and reliable configuration which permits the detection and digital sensing of borehole fluid flow. A spinner structure is provided in an impeller configuration having helical vanes disposed therearound. The impeller is magnetically coupled to a digital sensing unit, incorporating a sealed optical chopper having virtually zero functional resistance as compared to magnetic flux sensors. In this manner, a flow meter is provided, having extremely low and accurate threshhold velocity detection capabilities.
SUMMARY OF THE INVENTION
The present invention comprises a rotary flow meter tool for use in bore holes which is both sensitive, highly reliable, and effective in indicating the direction and the rate of fluid flow within the bore hole. In accordance with the broader aspects of the invention, a flow meter includes an impeller, mounted for rotation about a normally vertically disposed axis and having a plurality of generally axially extending helical rotor blades. The impeller is magnetically coupled to rotate the shaft of a sensing unit which produces a discrete output when the propeller is being rotated in one direction, a different output signal if the propeller is being rotated in the opposite direction, and a third digital output signal indicative of the rate of rotation of the propeller regardless of the direction of rotation. This configuration permits the detection of extremely low flow velocities and direction in a highly reliable manner.
In accordance with more specific aspects of the invention, the detecting apparatus includes signal emitter and receiver elements, separated by a butterfly valve, which upon rotation produces a discrete digital signal output. The signal emitter and receiver includes two pairs of light source/light detector arrays. Each of the two arrays or sets of light source/light detector elements is located on the circumference of a circle having as its center the axis of rotation of a detector shaft magnetically coupled to the impeller. The two light source/light detector sets are also positioned along the radii of the circle having a preselected angle therebetween. The butterfly valve is positioned on the detector for rotation thereon and includes a generally circular plate having discrete segments removed from the outer periphery in a preselected pattern. Upon rotation of the plate, a portion of the periphery remaining periodically breaks the light path between each of the two light source/light detector circuits and periodically permits the light to pass between the sets when the plate is positioned such that the removed segment is between the light/detector pairs. The angular position of the light source/light detector pairs from one another in combination with the rotating plate, cause the two light detectors to produce one electrical signal when the plate is being rotated in one direction, a different electrical signal when the plate is being rotated in the other direction, and a third signal which varies with the rate of rotation of the plate regardless of its direction. This construction is assembled in a sealed housing with virtually zero rotational resistance, since only light is being "chopped" by the butterfly valve.
BRIEF DESCRIPTION OF THE DRAWINGS
A more complete understanding of the invention can be had by reference to the following detailed description when taken in conjunction with the accompanying drawing wherein:
FIG. 1 is a side elevational cross sectional view of a well logging system utilizing one embodiment of a rotary flow meter, incorporating the principles of the present invention;
FIG. 2 is an enlarged, side elevational view of the impeller and housing of the rotary flow meter of the present invention;
FIG. 3 is a cut away schematic view of the sensor unit for detecting flow direction and rate;
FIG. 4 is a cross sectional view of the apparatus of FIG. 3, taken along the lines 4--4 thereof;
FIG. 5 is a circuit diagram of one embodiment of the flow direction and rate detecting circuitry of the present invention; and
FIG. 6 is a series of wave form diagrams illustrating output from the circuitry of FIG. 5 under conditions of different flow directions.
DETAILED DESCRIPTION
Referring now to FIG. 1 of the drawing, there is shown one embodiment of a well logging system 10, utilizing a rotary flow meter tool 11 constructed in accordance with the principles of the present invention. The well logging system 10 includes a cable 12 extending from a drum 13 through a capstan 14 and into a depending bore hole 15. The wire line cable 12 is connected at its lower end to a rotary flow meter 11 of the present invention. The bore hole 15 includes a steel casing 16 which is generally of the type commonly associated with petroleum wells. The casing 16 will include perforations at selected locations along its length (not shown) to permit the communication of fluid flow between various strata surrounding the bore hole and the interior of the casing 16. Additionally, the casing 16 may also house a string of production tubing (not shown) having a substantially smaller diameter than the casing 16.
Still referring to FIG. 1, the rotary flow meter 11 of the present invention comprises an elongate cylindrical housing 21 having an intermediately disposed centralizing spring assembly 9. Beneath the spring 9, at the lower end of the housing 21, there is assembled an electronics housing section 22 and a lower, helically configured impeller 23 which rotates upon a shaft 19 as a function of fluid flow within the casing 16. A detector housing section 24 supports an outwardly disposed impeller 23, which is rotatably mounted thereon. The housing section 24 also contains the apparatus for detecting the direction and speed of rotation of the impeller 23. The signals from housing 24 are then communicated to the surface of the borehole for recording on a strip recorder, or the like (not shown).
Referring now to FIG. 2, the impeller 23 includes a generally cylindrical impeller cage 26, comprising a plurality of longitudinally extending curved ribs 27 disposed adjacent the detector housing section 24. The longitudinal ribs 27 may be formed separately and secured to the central body of the cage, as shown, or the structure may be cast of suitably strong material such as steel. The longitudinal ribs 27 are tapered at each end and each has an inward, intermediate portion removed to define a central impeller region 28. A plurality of helically configured impeller blades 29 are mounted within said central region 28 and interposed among the ribs 27. When the impeller 23 is subjected to fluid flowing in the general direction of its axis, said impeller is caused to rotate upon its shaft 19 between jewelled bearings at a speed in proportion to the rate of the flow and in a rotational direction indicative of the flow direction.
The impeller 23 is preferably constructed to respond to the smallest possible fluid flow within the casing 16. Therefore, the impeller 23 is formed with helical vanes, or blades 29, which are longitudinally secured to the shaft 19 in a configuration responsive to bidirectional fluid flow. Consequently the impeller blades 29 are secured upon shaft 19 in opposing sets. For example, the front end taper of a vane 101 is opposite that of a vane 102 and equivalent to a vane 103. Any number of vanes 29 can be utilized, although an array of four is illustrated herein. It should be noted that the utilization of the reversed vane array permits substantially equivalent sensitivity for opposing flow directions. Certain physical flow phenomena do, however, effect perfect sensitivity balancing in bidirectional flow. For example, laminar flow from the upper tool body 22 has a retarding effect on the rotation of the impeller 23 relative to actual fluid velocity. The present invention permits compensation for this phenomena by adjusting the spaced positioning between the lower ends of the vanes 29 relative to the lower end 105 of the ribs 27 of cage 26. Laminar fluid flow developed around the ribs 27, by being more closely disposed to the path of rotation of the vanes 29, will have a similar effect to laminar flow having its genesis from the upper tool body. In this manner, the impeller 23 may be flow balanced for bidirectional sensitivity by shifting its relative positioning within the case 26.
The detector housing section 24 is formed to house a sensor assembly 25 which comprises a housing 31, closed at its lower end by a plug formed of a material permeable to magnetic flux, such as brass. In operation, the sensor assembly 25 is secured within the housing 24 adjacent the impeller 23. As shown in FIG. 3 in the center of the circular plus 32, there is secured a bearing 33, preferably formed of a highly durable, low friction material such as a sapphire, or similar jewel as that disposed on the ends of shaft 19. A second jeweled bearing 34, is spaced from the first bearing 33 a distance along the central axis of the housing 31 and adjustably mounted upon a threaded support member 38 secured within a bulkhead 39. Between the two bearings 33 and 34 is an axially extending shaft 35. A disc 36 formed from a permanent magnet is rigidly fixed to the shaft 35 to rotate adjacent the magnetically permeable plug 32. Located on the opposite, outer side of the plug 32 in the assembled tool 11 is a second permanent magnet 37 which is affixed to the end of the impeller 23 on the shaft 19. Upon rotation of the magnetic disc 37, lines of magnetic flux will be coupled through the plug 32 to rotate the magnetic disc 36 in magnetically coupled engagement with the impeller 23.
Still referring to FIG. 3, the interior of the sensor assembly 25 also includes first and second plates 41 and 42 spaced one from the other. Mounted within the first plate 41 is a pair of signal emitters in the form of light sources 43a and 44a, which may be comprised of light emitting diodes (LEDS). The light sources 43a and 44a are located in the plate 41 along the circumference of a common circle, through the center of which passes the rotating shaft 35. Mounted within the second plate 42 is a pair of signal receiving elements in the form of photo sensitive devices 43b and 44b. The photo detector 43b is in axial alignment with the light source 44a. A generally flat interrupter plate comprising a butterfly valve 46 is mounted on the shaft 35 and rotates between the disc 41 and the disc 42. A pair of tubular conduits 51 and 52 are provided through which electrical leads may be easily run for interconnection with the light sources. Other electrical leads (not shown) are routed through an interconnection space 107 to communicate power and signal transmission with the upper electronic package 22 for communicating with the surface of the borehole 15.
The construction of the sensor unit or "optical chopper" 25 incorporates a sealable, low friction assembly, and the absence of heavy magnets and flux lines permits the utilization of an extremely low resistance sensor operation. Since there is no retarding effect from chopping light beams emitted by LEDS as compared to magnetically engaging flux lines, the sensor has virtually no effect on the impeller 23 relative to retarding the fluid induced rotation thereof.
Referring now to FIG. 4, there is shown an illustrative view of the interrupter plate 46 taken along the lines 4--4 of FIG. 3. As shown in FIG. 4, the interrupter plate 46 of the embodiment shown herein, comprises a generally circular plate having two segments removed from opposite sides thereof. The removed, or open segments define a generally circular inner region 61, the radius of which is less than the radial distance of each of the two light sources 43a and 44a from the axis of rotation of the shaft 35. The remaining portions of the interrupter plate 46 are comprised of diametrically opposed, interrupter segments 62 and 63. The outer periphery of the interrupter segments 62 and 63 extends a greater radial distance than the distance from the axis of rotation of the shaft 35 to each of the light sources 43a and 44a, respectively. Thus, it can be seen that when the interrupter plate 46 is positioned with respect to the light sources 44a and 43a as shown in FIG. 4, light will be blocked between light source 43a and light detector 43b (FIG. 3), while a portion of the light from light source 44a is permitted to pass to light detector 44b. Therefore, as the interrupter plate 46 is rotated by the shaft 35, light is intermittently allowed to pass between light source 43a and light detector 43b, as well as light source 44a and light detector 44b. As shown most clearly in FIG. 4, the light sources 43a and 44a may be placed along circular radii, forming an angle of 135° with respect to one another. The radially extending sides which define interrupter segments 62 and 63 of the interrupter plate 46 are preferably located at an angle of 90° with respect to one another. Similarly, the radially extending edges defined by the portions removed from the interrupter plate 46 are also preferably positioned at 90° with respect to one another.
Referring next to FIG. 5, there is shown a diagram of one embodiment of circuitry used to detect the direction of rotation of the interrupter plate 46, and hence the direction of rotation of the impeller 23, as well as the rate of rotation thereof. FIG. 5 includes the two series connected LEDS 43a and 44a which are connected to an energizing voltage by means of a bias resistor 71. The source voltage is held at a fixed value by means of a zener diode regulator 72. The output of the associated photo transistors 43b and 44b are connected to the source voltage by means of biasing resistors 53 and 54. The output of photo transistor 43b and photo transistor 44b are also connected to the inputs of a phase detector circuit 73, the output of which is coupled through a driving transistor 74 to produce a voltage across the emitter resistor 75. The outputs of the photo transistors 43b and 44b are also connected to two inputs of an edge detector circuit 76 which is connected to a driver transistor 77 to produce an output voltage across a resistor 78.
Referring briefly to FIG. 6, there are shown six separate wave form diagrams A-E. Diagrams A and B show the output voltages of photo transistors 43b and 44b, respectively, during rotation of the impeller in one direction while wave forms C and D show the outputs of the photo transistors 43b and 44b during rotation of the impeller in the opposite direction. Wave form E of FIG. 6 illustrates the output of transistor 77 during rotation of the impeller in either direction, as will be defined in more detail below.
In operation, when the flow measurement meter 22 of the present invention 11 is positioned in a down hole configuration, fluid flow either up the casing 16 or down the casing 16 will cause the impeller 23 to rotate in one direction or the other. As shown in FIG. 2, impingement of fluid flow in a direction parallel to the axis of the impeller 23 moves the impeller blades 29 so as to rotate the impeller 23. As shown in FIG. 3, rotation of the impeller shaft 19 rotates the disc 37 which is magnetically coupled to the disc 36 and thereby rotates the interrupter plate 46 which is attached to the axially extending shaft 35. As is shown most clearly in FIG. 4, rotation of the interrupter plate 46 in the paths between light sources 43a and 44a and the light sensors 43b and 44b, respectively, causes an interruption in the flow of current from those light sensors 43b and 44b. The rate of interruption may be equated to fluid flow velocity, and easily interpreted. As can be seen from FIG. 4, rotation of the interrupter plate 46 about the axis 35 can also be related to flow direction. Rotation of the interrupter plate 46, for example, in a clockwise direction will allow light from LED 43a to pass to its associated photo cell 43b prior to allowing light to pass from LED 43s to photo detector 43b. Conversely, rotation of the interrupter plate 46 in a counter-clockwise direction, as shown in FIG. 4, will allow light to pass freely from LED 44a before light is permitted to pass from LED 43a. It may thus be seen that rotation of interrupter plate 46 in one direction allows photo detector 43b to conduct prior to photo detector 44b. Rotation of the plate 46 in the opposite direction allows photo transistor 44b to conduct prior to photo transistor 43b. That is, upon rotation of the interrupter plate 46, the output signals from photo transistors 43b and 44b will always be out of phase wih one another, with one signal leading the other during rotation in one direction and the same signal lagging the other during rotation in the opposite direction.
As is shown most clearly in FIG. 5, the outputs of the photo transistors 43b and 44b are each connected to the inputs of the phase detector 73. The output of the phase detector 73 is a function of which input signal is leading the other; thereby defining flow direction. By way of example, and with reference to both FIGS. 5 and 6, if wave form A represents the output of photo transistor 43b and wave form B represents the output of photo transistor 44b, the signal from photo transistor 43b is leading the output of photo transistor 44b. This "leading" condition will produce a distinct output from the phase detector 73, which output will be either high or low. If we next view wave form C as being the output of photo transistor 44b, this "lagging" condition will produce an output of the phase detector 73 of an opposite character to that of the "leading" condition (either high or low). Preferably, the circuitry is selected so that rotation of the interrupter plate 46 in a clockwise direction produces a high voltage output level while rotation in a counter clockwise direction produces a line voltage output of a low voltage level. The edge detector 76 detects the level change from photo transistor 43b and 44b and produces a pulse for each level transition. For example, in wave form E of FIG. 6, the circuitry is adjusted such that the leading and trailing edges of each of the wave forms C and D produces a spiked-like pulse. The pulses are accumulated and monitored as a function of the flow rate of the fluid past the impeller and hence, the rate of rotation of the interrupter plate 46.
The sensor unit of the detector housing 24 detects rotation of the impeller 23 with virtually minimum retardation and maximum reliability. The sensor utilizes a digital network as compared to the analog network of most prior art embodiments. For example, prior art flow meters utilizing magnetic signals consistently vary waveforms rather than producing discrete "on-off" pulses. Wave shape and amplitude thus become critical factors in logging operations, although such analog outputs are subject to undiagnosed component malfunction. For this reason, temperature compensating resistors are often used in prior art circuit designs to accommodate down hole conditions. In the present invention, such thermal elements are not needed because signal amplitude variations will not affect the digital output accuracy.
As can be seen from the above description, the invention provides a highly reliable and accurate means for electronically indicating both direction of flow in a down hole environment and the rate of that flow. Having thus described the invention in connection with certain specific embodiments thereof, it is to be further understood that modifications may now suggest themselves to those skilled in the art and it is intended to cover those modifications as fall within the scope of the following claims.
|
An impeller is rotatably mounted in a housing on the lower end of a sub which is lowered by means of a wire line into a bore hole. The fluid flow in either direction within the bore hole engages and rotates helical vanes of the impeller, which in turn rotates a digital sensing device. A magnetic coupling links the impeller to the sensing device which is sealably secured within the housing. Rotation of the sensing device in one direction produces a digital output signal which is distinguishable from the output signal produced when the sensing device is rotated in the opposite direction. The digital signal is produced by the rotation of a butterfly valve between signal emitter elements and signal receiving elements coupled to a distinguishing logic circuit. The direction of flow of fluids along the bore hole is thus easily detected in a reliable, highly sensitive manner. Further, and regardless of the direction of rotation of the sensing device, a third discrete output signal is produced, which is indicative of the rate of flow of fluid within the bore hole independent of the direction of that flow. Because of the low friction operation of the meter, the threshold velocity of detectable fluid flow is extremely low.
| 4
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. patent application Ser. No. 12/670,587, filed Jun. 29, 2010, now abandoned, which is a National Phase Application of PCT International Application No. PCT/EP2008/005680, International Filing Date Jul. 11, 2008, claiming priority from German Patent Application No. DE 10 2007 034 679.6, filed Jul. 25, 2007, all of which are incorporated by reference herein.
BACKGROUND OF THE INVENTION
Heart failure is one of the main causes of death in industrialised countries and is a result of the inability of mature heart muscle cells (cardiomyocytes) to divide and replace damaged heart muscle. Since the therapeutic use of embryonic cardiomyocytes is prohibited in most countries, adult human stem cells could represent an alternative for regenerative medicine. Adult stem cells of differing origin have previously been injected intramyocardially in order to be converted to cardiomyocytes. However, only in animal experiments has such cell-to-cell contact induced mesenchymal stem cells to differentiate into cardiomyocytes. Therefore, in particular the use of human cardiomyocytes from human adult stem cells for the regeneration of injured or damaged myocardium is a goal that for many years has been striven for but not yet been achieved in an optimal manner.
In DE 10 2006 003 996.3 said object has been principally achieved by providing a method for producing autonomously contractile heart muscle cells by differentiation from adult stem cells that have been isolated from exocrine gland tissue and by providing specific material compositions containing said stem cells.
Said cellular compositions which e.g. comprise injectable cellular compositions, may, in some instances, have the drawback that the cells arrive at the desired application site but do not remain there (e.g. possible in the case of an injection) or that the material composition is rather voluminous which delays the desired resorption in the body and requires more space in the body (e.g. in the case that conventional solid supporting materials are used).
SUMMARY OF THE INVENTION
The present invention is based on the finding that these drawbacks can be avoided by providing new material compositions, wherein the stem cells are present on supporting matrices in the form of preferably resorbable thread structures or nets, on which the stem cells can be induced to differentiate, for example into autonomously contractile heart muscle cells.
The inventors have observed that the adult stem cells isolated from exocrine gland tissue are pluripotent and have both the potential for spontaneous differentiation into heart muscle cells and are capable of developing under suitably stimulating conditions, mainly or almost exclusively, into heart muscle cells. Exocrine gland tissue therefore represents a very effective source for stem cells capable of a wide-ranging differentiation from which the desired heart muscle cells can be successfully obtained in large numbers with good yields.
The exocrine gland tissue used according to the invention may stem from a mature organism, a juvenile organism or a non-human foetal organism, preferably a post-natal organism. The term ‘adult’ as used in the present application therefore relates to the development stage of the source tissue and not to that of the donor organism from which the tissue originates. ‘Adult’ stem cells are non-embryonic stem cells.
Preferably, the exocrine gland tissue is isolated from a salivary gland, a tear gland, sebaceous gland, sweat gland, from glands of the genital tract including the prostate gland or from gastro-intestinal tissue, including the pancreas or secretory tissue of the liver. In a particularly preferable embodiment, it is acinar tissue. Especially preferably, the acinar tissue stems from the pancreas, the parotic gland or the mandibular gland.
An advantage of this method resides in that the stem cells can be effectively obtained from living donor organisms, for example from human salivary glands or, by means of a minimally invasive retroperitoneal procedure, from the pancreas without the donor organism being decisively affected. This is particularly advantageous both from ethical standpoints and in view of the possibility of further observation of the donor organism with regard to possible diseases.
According to a first embodiment of this method, the stem cells primarily isolated from the organism are used as a source for further cultivation and differentiation all the way through to heart muscle cells. This version has the advantage of a particularly simple operation. The desired differentiated cells can be obtained directly from a primary culture. Alternatively, according to another embodiment it is provided that, initially, aggregation of the stem cells isolated from the organism to ‘organoid bodies’ takes place.
This version has the advantage that an effective reservoir for relatively large quantities of differentiated cells is created with the organoid bodies. The inventors have found that the stem cells isolated from the exocrine gland tissue form organoid bodies which, when supplied with nutrients, show strong growth to tissue bodies with diameters of up to a few millimeters or more.
This method can essentially be carried out in such a way that heart muscle cells which have formed spontaneously from the primary or secondary (from the organoid bodies) isolated stem cells are identified, where necessary selected, and further multiplied. According to a preferred embodiment, on the differentiation of heart muscle cells, stimulation of the cell culture is provided. Stimulation has the advantage of increased effectiveness and speed in the formation of the desired heart muscle cells. According to a first version, following the differentiation of the stem cells to heart muscle cells, their stimulated multiplication in a cultivation medium is carried out. According to a second version, the stimulation takes place at an earlier stage and concerns the still undifferentiated stem cells the development/differentiation of which into the desired heart muscle cells is instigated.
Said stimulation may comprise one or more of the following stimulation treatments, which can be carried out simultaneously or consecutively. Co-cultivation with differentiated heart muscle cells or with cell lines derived therefrom, treatment (imprinting) with immobilised or dissolved molecular differentiation factors provided in the liquid phase or genetic activation in the stem cell can be provided. In addition, stimulation can comprise the addition of other substances, such as hormones (e.g. insulin) or cell types which influence the differentiation.
If the imprinting takes place with immobilised growth factors, then differentiation factors fixed to a mobile carrier which can be positioned relative to the stem cells are preferably used. Advantageously, targeted differentiation of individual stem cells or particular stem cell groups can be achieved thereby. The carrier is, for example, a synthetic substrate, which has advantages for targeted design with the differentiation factors, or a biological cell on the cell membrane of which the differentiation factors are arranged.
Some examples of non-limiting growth factors and differentiation factors that can be used are 5′-azacytidine, bFGF, Cardiogenol, transferrin and PDGF.
In a specific embodiment, the stimulation treatment is carried out by cultivation of the stem cells under normal conditions (e.g. as described in example 1) in the presence of biological “nanostructured surfaces”. This term herein denotes cells, for example cardiomyocytes or other heart cells, which have been killed by fixation treatment, e.g. with formaldehyde or another suitable fixing agent, and their cell membranes thereby made impermeable, whereas the surface structure of the cells, including the surface proteins and other molecules exposed there, remain intact. By this means, the influence of substances from the interior of these cells is precluded and stimulation takes place specifically through the influence of the surface structure of the fixed cells.
If, according to another preferred embodiment of the method, identification and selection of the differentiated cells from the cell culture are provided, advantages can result for the further use of the heart muscle cells formed. In particular, a cell composition can be provided which consists entirely or largely of heart muscle cells. If the selection takes place with sorting methods which are per se known, such as a preparatory cell sorter method or sorting in a fluid microsystem, advantages can result in terms of compatibility with conventional cell biology procedures.
A further advantage of identification and selection lies therein that cells which are not identified as heart muscle cells and are accordingly not selected from the culture being processed, can be subjected to further cultivation and differentiation. By this means, advantageously, the yield of the method can be increased.
Possibilities for sorting cardiomyocytes and their progenitor cells are, for example, by means of transfection of reporter gene constructs with heart-specific promoters which lead to fluorescing products when they are switched on, or fluorescence-marked antibodies against heart-specific proteins.
According to a preferred embodiment, in order to form the heart muscle cells, stem cells from tissue of secretory glands or glands of the gastro-intestinal tract are obtained from the organism. The stem cells are isolated, in particular, from tissue which consists of acinar tissue or contains acinar tissue. When harvesting from the pancreas takes place, advantages can result in terms of the use of other tissue components of the pancreas for the aforementioned stimulation. If harvesting from the salivary gland is carried out, advantages can arise in terms of the conservative treatment of the donor organism.
Preferred donor organisms are vertebrates and, in particular, mammals. Especially preferred is the human. When human stem cells are used, isolation of the stem cells is performed from non-embryonic states, that is, from differentiated tissue in the juvenile or the adult phase. In the case of non-human donor organisms, use can essentially also be made of differentiated tissue in the foetal condition.
The heart muscle cells produced are preferably used therapeutically. A particular advantage lies therein that human heart muscle cells can be produced from non-embryonic stem cells and used for treatment in humans. A particularly attractive possibility is the autologous treatment of a human with heart muscle cells obtained from stem cells from the human him- or herself. By this means, rejection reactions can be effectively avoided. Typically, the treatment would comprise the regeneration of injured or damaged myocardium. The treatment can either comprise the administration of undifferentiated stem cells and their induced differentiation to heart muscle cells in the body or the administration of already differentiated heart muscle cells, for example, in a transplant.
One subject of the invention are cell compositions which contain adult stem cells from differentiated exocrine gland tissue and/or heart muscle cells derived therefrom. According to a preferred embodiment of the invention, the cell composition may contain other cells or materials which form, for example, a matrix. The cell composition may also comprise a covering or a 3-dimensional matrix in which the heart muscle cells and possibly other cell types are arranged. The covering or 3-dimensional matrix comprises, for example, alginate, collagen, implantable materials, polymers (biopolymers or synthetic polymers), particularly materials that are degradable in the body. The matrix may have a thread-like or net-like structure.
A main aspect of the present invention relates to a material composition wherein the glandular stem cells obtained from exocrine gland tissue are present on a supporting matrix which has the shape of threads or nets. This supporting matrix is preferably physiologically tolerable and degradable in the body. Typically, it is a plastic material capable to be resorbed, e.g. the commercially available Vicryl (from Ethicon) or the above mentioned polymeric materials. The glandular stem cells adhere on the external surface as well as in the microstructures of the threads and nets and can be induced to differentiate there. By use of this supporting matrix the stem cells and the differentiated cells derived therefrom, respectively, can be transferred to desired application sites in the body conveniently and in a targeted manner. Moreover, the application of such a supporting matrix might be able to prevent the arrhythmic disorders often observed in the context of intramyocardial injection of stem cells. By using such a supporting matrix also cell loss (e.g. by migration of stem cells after injection) can be delayed or prevented, since the applied cells adhere tightly to the microstructures of the threads and nets and regenerate the damaged tissue only by means of or upon division.
A specific embodiment of the present invention concerns a bidirectionally transformable stem cell patch (BTS) for myocardial regeneration. A patch of this type comprises adult stem cells from exocrine gland tissue, preferably pancreatic stem cells, and a porous, possibly subdivided, matrix for accommodating the cells, has a large supporting surface for the myocardial wound surface onto which it should be applied after removal of the epicardium, is usually multi-layered, for example, constructed from a plurality of sponge-like membranes, but relatively thin (having a short diffusion path) and readily fixable.
The porous matrix is, for example, a collagen matrix or consists of another physiologically tolerable material (e.g. as described above). The supporting matrix may be present in the shape of a thread structure or a net as defined above. In one embodiment, all the materials of the patch are degradable in the body.
The patch can also contain cells which have fully or partially differentiated out to heart muscle cells or other differentiated cells present in the heart. The patch can also contain substances which promote the differentiation of stem cells to cardiomyocytes and/or pharmaceutically active agents, for example for suppressing a rejection reaction.
The term “bidirectionally transformable” as used herein, indicates that the patch is configured such that the cells contained within said patch, in particular stem cells, can get into contact on both sides with cells from the adjacent tissue or with substances produced by the cells and a transformation/differentiation of the stem cells into the desired cell type can thereby be induced or stimulated.
In a preferred embodiment, the patch is placed between the broad back muscle ( Musculus latissimus dorsi ) and the myocardium freed from epicardium (see FIG. 3 ). The cells of the myocardium or substances produced thereby can then induce differentiation of the stem cells arranged in the patch on the side towards the heart into heart cells, in particular, heart muscle cells. On the other side, the tissue of the back muscle can, on the one hand, provide the cells of the patch with nutrients and, on the other hand, induce transformation of the stem cells on the side towards the back to vessel cells, for example, endothelial cells etc., or permit migration of appropriate cells into the patch, so that formation of new capillary vessels can take place in the patch or the adjoining tissue. If desired, hypercapillarisation of the back muscle covering with intact muscle fascia is induced in the patient by intermittent transcutaneous electrostimulation (e.g. with stimulation electrodes stuck on).
In another preferred embodiment, the stem cells are injected into the (preferably hypercapillarised) muscle tissue ( M. latissimus dorsi ) itself, which wraps round the heart. There they develop and become transformed into heart muscle cells by substances from the adjoining injured myocardial surface (and/or by exogenous differentiation factors that are fed in). The vascular system of the skeletal muscle then becomes the vascular system of the contractile myocardial patch. By means of an implanted muscle pacemaker which electrostimulates the patch, transformation of the muscle fibres of the skeletal muscle into pure, oxygen-dependent type I fibres could be induced. Since, in contrast to the heart muscle fibres, type I fibres cannot survive continuous stimulation, this would in the long term lead to elimination of these skeletal muscle fibres. A myocardial patch with its own vascular supply would be the result.
According to a particularly preferred embodiment of the invention, the adult stem cells used are human stem cells that have been isolated from pancreatic tissue.
Adult stem cells were isolated and cultivated from pancreatic tissue of patients who had undergone a pancreas operation (see example 1 with regard to the conditions). The cells were selected, cultivated with medium (e.g. DMEM) with foetal calf serum and passaged up to more than 25 times. The cultures could also be frozen between individual passages without impairing the cells. In different passages, the cultures showed spontaneously formed reticular cell clusters ( FIG. 1 a ) and some of these cell clusters showed cellular contractions at various sites, indicating a functional contractile system. In an optimized method with which relatively large quantities of contractile heart muscle cells (cardiomyocytes) could be obtained faster, pancreatic stem cells were co-cultivated with small pieces of human heart muscle obtained from a cardiac valve operation. Following a contact time of 48 hours, the myocardium was removed and stem cells were held in culture for a further 2 to 4 days or 2 weeks in order to investigate the influence of the myocardium on differentiation to cardiomyocytes. Thereafter, the various methods, including immunocytochemistry of sarcomeres and heart-specific troponin I, semiquantitative RT-PCR analysis with regard to alpha-actin and troponin T2, and electron micrographic examination, were applied in order to identify cardiomyocytes.
Myocardium for co-cultivation can be obtained by means of biopsies from the cardiac septum, which are already routinely used for the detection of tissue rejection following heart transplantation. The method according to the invention, with which a large number of contractile cardiomyocytes can be produced by easy and convenient means, could be significant for general myocardial regeneration and, in particular, for contractile myocardial patches.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 show the results of various identification methods for cardiomyocytes.
FIG. 1 a Cultures of pancreatic stem cells with reticular cell clusters show autonomous contractions.
FIG. 1 b Immunocytochemical visualisation of sarcomeres (red) in transformed adult pancreatic stem cells (blue nuclei) in contact with human myocardium (M) for 2 days. A falling gradient of M towards the periphery is observable.
FIG. 1 c A gene expression analysis with heart-specific PCR primers for the target genes α-actin and troponin T2 isoform-demonstrates a strong increase in muscle cell-specific molecules in co-cultivated cells (CEpan 3b, human pancreatic stem cells; P14, passage 14; HEp-2, human carcinoma cell line; h-heart-cDNA, human heart-cDNA).
FIG. 2 a,b Human pancreatic adult stem cells with immunocytochemical staining for heart-specific troponin I without contact with human myocardium (a) and following a two-day contact with human myocardium (b). Clear evidence of the presence of heart-specific troponin I in transformed cells is given.
FIG. 2 c,d Various stages of cardiomyocytes, transformed from adult pancreatic stem cells, are shown in the electron micrographs taken four days after 48-hour contact with biopsies of human myocardium. Myofilaments and structures of partial (c) and complete (d) development of the intercalated disks are shown. Vesicles, organised in lines ( FIG. 2 c , arrows), are considered as cross-sections of a premature status of the sarcoplasmic reticulum.
FIG. 3 shows the placement of a bidirectionally transformable stem cell patch (BTS) between the myocardium and the broad back muscle ( Musculus latissimus dorsi ) for myocardial regeneration.
FIG. 4 shows thread-like structures with glandular stem cells grown thereupon.
DETAILED DESCRIPTION OF THE INVENTION
Example 1
Isolation, Cultivation and Co-Cultivation of Adult Pancreatic Human Stem Cells
The source of the human pancreatic tissue was healthy tissue that had been removed for precautionary reasons during a pancreas operation due to cancer or inflammatory disease. The tissue was obtained in physiological saline solution. Pancreas acini were isolated therefrom, as previously described (DE 10328280; Orlic et al., Nature 410: 701-705).
In particular, the pancreatic tissue was treated with a digestant containing HEPES-Eagle's Medium (pH 7.4), 0.1 mM HEPES buffer (pH 7.6), 70% (vol/vol) modified Eagle's Medium, 0.5% (vol/vol) Trasylol (Bayer AG, Leverkusen, Germany), 1% (wt/vol) bovine serum albumin, 2.4 mM CaCl 2 and collagenase (0.63 PZ/mg, Serva, Heidelberg, Germany). Following digestion, the acini were dissociated by suction and ejection using different glass pipettes with narrow openings, and filtered through a nylon sieve. The acini were centrifuged and further cleaned by washing in Dulbecco's modified Eagle's Medium (DMEM, Gibco, Germany), with added 20% foetal calf serum (FCS), equilibrated with Carbogen and brought to pH 7.4. The washing procedure (centrifuging, suction, resuspension) was repeated 5 times. The acini were resuspended in DMEM and cultivated at 37° C. in a humid atmosphere with 5% CO 2 . After 1-2 days of culturing, spindle-shaped cells were observed, surrounding the outer edges of the pancreatic acini. Differentiated acinar cells were removed in each medium exchange. After reaching confluency, pancreatic stem cells were cultivated by means of trypsin treatment, cultivated, counted and resown at a density of 2.4×10 5 cells/cm 2 . This procedure was repeated until sufficient cells were available. As previously shown, no changes occur in the stem cells during the passages (tested by staining). We therefore used passages 14 and 4 for further differentiation.
Stimulation of differentiation into cardiomyocytes was achieved by co-cultivation of the primary cells with 5 pieces of myocardium (4×4×4 mm) in each case for 2 days. The tissue (mitral papillary muscle or auricle) was obtained during an operation for heart valve replacement and transported in physiological saline solution. The heart muscle pieces were placed on the bottom of the culture vessels for 3 hours until the primary cells (1×10 6 ) were applied. After 48 hours, the heart muscle pieces were removed and the stem cells further cultivated as described above. The cells were then subjected to a passage each time after reaching confluency. Immunocytochemical analyses were carried out directly 48 hours after treatment. In order to investigate the long-term effects of differentiation, the cells were harvested 17 days after treatment for PCR analyses.
As the cells became confluent in the culture dishes, reticular clusters could be observed ( FIG. 1 a ). The cell layer was washed with the less nutrient-rich phosphate buffered salt solution (PBS) and partially lifted mechanically from the base of the culture with a scraper. Contractile regions were then documented with a video system. In order to check whether cardiomyocytes grow from biopsies of cardiac tissue, the biopsies were cultivated as described above, but without pancreatic stem cells. After 2 days, no growing cells could be found.
Example 2
Identification of Heart Muscle Cells
1. Immunocytochemistry of Sarcomeres
Both the stimulated and non-stimulated stem cells were sown on chamber slides and cultivated for at least 2 days before being fixed with methanol:acetone (7:3) containing 1 g/ml DAPI (Roche, Switzerland) and washed 3 times in PBS. Following incubation in 10% normal goat serum at room temperature for 15 minutes, the samples were incubated with the primary antibody overnight at 4° C. in a humidity chamber. Primary monoclonal antibody was directed against sarcomere Myosin MF 20 (DSHB, USA). Following rinsing three times with PBS, the slides were incubated for 45 minutes at 37° C. with Cy3-marked anti-mouse IgG, diluted 1:200. The slides were washed 3 times in PBS and covered with Vectashield mounting medium (Vector, USA) and analysed with a fluorescence microscope (Axioskop Zeiss, Germany). In order to rule out identified sarcomeres being released from the biopsy and adhering to the stem cells, controls with myofibroblasts and endothelial cells were co-cultivated with myocardium. In these controls, the tested cells produced negative results in immunochemistry for sarcomeres.
By contrast, an immunocytochemical identification of sarcomeres was successfully carried out using transformed adult human pancreatic stem cells in four preparations following contact with human myocardium (M) from four different patients. A declining gradient of developed sarcomeres from “M” (placement of the myocardium) up to the periphery was found after two days of myocardial contact ( FIG. 1 b ).
2. Immunocytochemistry of Heart-Specific Troponin I
Stem cells were co-cultivated with myocardial biopsies for 48 hours and cultured for 2 to 4 days after removal of the myocardium. The samples were then rinsed twice with PBS and dried for 24 hours in air at room temperature, and thereafter fixed with pure acetone for 10 minutes at −20° C., rinsed again for 2×5 minutes with TBS buffer and pre-incubated with RPMI 1640 with 10% AB serum. Monoclonal antitroponin I-antibodies (Cone 2d5, Biozal 1:25) were included as primary antibodies for 60 minutes. Addition of secondary antibody (antimouse-rabbit antibody; DAKO; 1:25, for 30 minutes) followed by incubation with a complex with alkaline phosphatase or without alkaline phosphatase (DAKO; 1:50, 30 minutes) was repeated several times. Finally, substrate incubation (naphthol/neofuchsin) and contrast staining with haemalaun was carried out before microscopic examination. In addition, isotope testing was carried out with mouse-IgG 1 (DAKO) and, for a further negative control, skeletal muscle was stained. Myocardium was used as a positive control. An isotype control with mouse-IgG 1 (DAKO) was also negative. Additional controls carried out with skeletal muscle were also negative. As expected, a control with human myocardium showed a positive result (data not shown).
The immunocytochemistry of heart-specific troponin I was already strongly positive 2 days after a 48-hour co-culture with a human myocardial biopsy, as FIG. 2 b shows. Stem cells which were not in contact with myocardial biopsies produced mainly negative results in an immunocytochemical test for troponin I and served as a further control ( FIG. 2 a ).
3. Semiquantitative RT-PCR Analysis
Whole-cell RNA was isolated using a Nucleo-Spin® RNA II kit (Macherey-Nagel, Duren, Germany). 0.5 μg total RNA were transcribed in reverse into cDNA using reverse transcriptase Superscript II RNase H − (RT, Invitrogen) and oligo dT primers (Invitrogen) in accordance with the instructions of the manufacturer. The PCR reactions were carried out in a 50 μl reaction volume using Taq DNA polymerase (MBI Fermentas). The reactions were carried out for 38 cycles. A control run of RNA without reverse transcription took place in order to check for contamination with genomic DNA and produced no bands. To normalise the cDNA concentration in different RT samples, we measured the relative expression of GAPDH as a representative control for an internal housekeeping gene. The expected fragment sizes and the optimum PCR annealing temperatures were as follows: GAPDH, 5′:gagtcaacggatttggtcgt, 3′:ggaagatggtgatgggattt (213 bp, 58.8° C.), troponin T2, 5′:gattctggctgagaggagga, 3′:tggagactttctggttatcgttg (197 bp, 62.6° C.), alpha-actin, 5′:gtgtgacgacgaggagacca, 3′:cttctgacccatacccacca (154 bp, 62.6° C.). Purified human heart RNA (Ambion) and a carcinoma cell line (HEp2) served as functional controls for the PCR primer.
A semi-quantitative RT-PCR analysis ( FIG. 1 c ) for α-actin and troponin T2 showed a more markedly raised level of these muscle cell-specific molecules two weeks after contact than in untreated spontaneously differentiated stem cells. The increase in α-actin and troponin T2 after two weeks was reproducible and significant.
4. Electron Microscopic Investigation
Cells which had been cultured on cover glasses were fixed for 1 hr with 2.5% glutaraldehyde in 0.1 M cacodylate buffer. Subsequent fixation with 1% OsO 4 in 0.1 M cacodylate buffer was carried out for 2 hrs; samples were dehydrated with ethanol and embedded in Araldite (Fluka, Buchs, Switzerland). Ultrathin sections were stained with uranyl acetate and lead citrate (Ultrostainer Carlsberg System, LKB, Bromma, Sweden) and examined with a Philips EM 400 electron microscope (Philips, Eindhoven, Netherlands) at 60 kV.
The electron microscope examination ( FIG. 2 c,d ) shows, after 48 hours of contact of adult pancreatic stem cells with human myocardium and a further 4 days of differentiation, cells with a number of contractile fibrils. Various stages of intercalated disks were also observed. Whereas the intercalated disks in FIG. 2 c are only weakly, though clearly, recognisable, in FIG. 2 d , the intercalated disk is well differentiated, as in mature tissue. Since intercalated disks are only found in cardiac muscle, these findings also provide evidence of differentiation of adult human stem cells into cardiomyocytes.
After 14-40 days of growth in culture and after 48 hours in contact with human myocardium, the cells were partially mechanically lifted from the culture vessel and treated with a less nutrient-rich culture medium. The cell complexes showed contractions in various regions. These contractions were autonomous and reproducible in several cultures, thereby demonstrating a functional contractile system. This is a first observation of human autonomously contracting myocardium cells produced from human adult stem cells.
Example 3
Differentiation with 5-azacytidine
The stem cells are sown at a density of 1×10 3 in Petri dishes and cultivated for 24 hours in DMEM (with 10% FKS and 1% penicillin/streptomycin) until they attach adhesively to the base of the culture dishes. The cells are then cultivated for 24 hours in a differentiating medium, containing:
DMEM medium 10 μg/l bFGF 10 μmol/l 5-azacytidine 0.25 mg/l amphotericin.
A comparison with control batches without 5-azacytidine shows that, on stimulation with 5-azacytidine, significantly more stem cells differentiate to cardiomyocytes.
Example 4
Differentiation with Cardiogenol
The cells are sown in Petri dishes at a density of 1×10 3 and directly cultivated for 48 hours with a differentiating medium, containing:
DMEM medium 500 μl Cardiogenol solution.
For the Cardiogenol solution, 5 mg Cardiogenol are dissolved in 4.75 ml DMSO.
Also in this case, more cardiomyocytes develop than in controls without Cardiogenol.
Example 5
Differentiation with Insulin, Transferrin and PDGF
The cells were incubated for 7 days in the following differentiating medium:
DMEM medium 820 μg/ml BSA 5 μg/ml transferrin 5 μg/ml insulin 50 ng/ml PDGF
In this case, also, more cardiomyocytes developed than in the controls without growth factors.
Example 6
Differentiation in the Presence of Co-Cultivated Cardiomyocytes
Version 1:
Cardiomyocytes are sown in a culture bottle such that they completely grow over the base of the bottle. Then stem cells (for example, marked with β-galactosidase) were added to the cells at a density of 1×10 3 and co-cultivated for 14 days. From the marked stem cells, the number of cells differentiated into cardiomyocytes can be determined, for example, with FACS analysis.
Version 2:
Cardiomyocytes are added to freshly sown pancreatic stem cells in a cell culture cage for 14 days. The cardiomyocytes will release various substances which promote the differentiation of the stem cells to cardiomyocytes. Fusion with co-cultivated cells can be ruled out, and the cells do not have to be labelled beforehand.
Example 7
Growth of Glandular Stem Cells on Threads and Nets
Stem cells from exocrine glands of human and goat are sown in different passages onto resorbable threads and nets. These threads and nets for example consist of Vicryl (sterile packed from Ethicon) and are coated with 1% gelatine beforehand. Subsequently, the seeding of the stem cells in DMEM supplemented with 10% FCS is effected. After a few hours already, the stem cells adhere on and in the microstructures of the threads and nets and can then be visualized by the use of different stains, e.g. nucleic stains.
|
The invention relates to material compositions comprising adult stem cells obtained from exocrine gland tissue and a supporting matrix having the shape of a thread structure and/or of a net. The supporting matrix preferably consists of a plastic material which is physiologically acceptable and degradable in the body. The material compositions of the invention are in particular suited for use in regenerative medicine, e.g. for regeneration of injured or damaged myocard tissue.
| 2
|
This is a divisional of application Ser. No. 09/810,616 filed Mar. 19, 2001 now U.S. Pat. 6,590,027; the disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to a paint composition for automotive weather strips and glass runs, as well as processes for producing automotive weather strips and glass runs.
BACKGROUND OF THE INVENTION
Most automotive weather strips and glass runs (which are hereunder sometimes referred to simply as “automotive weather strips”) are coated with curable urethane-based paints on the surface of the substrate to impart it special functions such as wear resistance and slip property (sliding property) or provide it with better appearance.
Conventionally, curable urethane-based paints of a solvent type have been used in the manufacture of automotive weather strips; however, with the recent concern over the global environment and the health of working personnel, a need has arisen for a shift toward aqueous and other paints of a non-solvent type.
However, water which is the medium for paints of the aqueous type have more latent heat of evaporation than solvents, so the aqueous paints require more heat than paints of the solvent type in order to dry up the water after application. In addition, unlike solvent-type paints that allow adjustment of volatilization temperature and rate by combining several kinds of solvents, aqueous-type paints require preliminary drying in order to prevent “flashing” due to nearly instantaneous volatilization of water. As a result, longer drying times are required by the aqueous paints and in order to deal with this low productivity problem, it becomes necessary to build a new drying oven for shifting from the solvent-type paint to the aqueous type.
Most automotive weather strips use substrates that are made of thermosetting elastomers such as EPDM rubber (ethylene propylene rubber) or thermoplastic elastomers such as TPO (thermoplastic polyolefins).
If thermoplastic elastomers are used as the substrate, drying should be carried out at a low temperatures of 150° C. or below to prevent thermal deformation that would otherwise occur during post-application drying; however, if the paint applied is of the aqueous type, the drying operation is not highly productive since water is very difficult to dry.
The EPDM rubber as an exemplary thermosetting elastomer is nonpolar and has low sticking property and it is also hydrophobic; hence, aqueous paints cannot produce a more adhesive coat than solvent-type paints.
With a view to solving this problem, pretreatments such as corona discharge and primer application are conventionally applied to the substrate surface but problems still remain, such as high initial cost and the difficulty involved in performing positive pretreatments on complexly shaped articles.
SUMMARY OF THE INVENTION
Therefore, a first object of the invention is to provide a paint for automotive weather strips that is free from the above-mentioned defects of the prior art and which can achieve strong adhesion to the EPDM rubber without corona discharge, primer application or other pretreatments on the substrate surface while exhibiting high wear resistance.
A second object of the invention is to provide a process for producing automotive weather strips which does not require the as-applied coat to be cured completely in a drying oven but which permits it to be cured completely by the heat inertia of the drying step and which can also shorten the length of the drying oven or lower the drying temperature.
A third object of the invention is to provide a process by which automotive glass runs having high wear resistance in the bottom portion while exhibiting high softness and flexibility in the lip portions can be produced efficiently and with minimum impact on the global environment.
As a result of the extensive studies made in order to attain the above-mentioned objects, the present inventors found that the first object of the invention could be attained by adding at least two specified silane coupling agents or a product of premixing reaction between said at least two silane coupling agents to a curable urethane-based emulsion paint.
Thus, in a first aspect, the present invention relates a paint composition for automotive weather strips comprising a curable urethane-based emulsion paint having added thereto either at least two silane coupling agents selected from the group consisting of a silane coupling agent having an amino group, a silane coupling agent having an epoxy group, a silane coupling agent having a methacryloxy group and a silane coupling agent having an acryloxy group, or a reaction product obtained by previously mixing said at least two silane coupling agents.
The second object of the invention can be attained by a process for producing automotive weather strips which comprises the steps of extruding a semi-finished product of automotive weather strip while it is continuously coated with a urethane-based aqueous paint, then drying and curing the product in a heating furnace, or comprises extruding a semi-finished product of automotive weather strip, heating it, immediately followed by continuous application of a urethane-based aqueous paint, then drying and curing the product in a heating furnace, or comprises unrolling a semi-finished extruded product of automotive weather strip while it is continuously coated with a urethane-based aqueous paint, then drying and curing the extruded product in a heating furnace, wherein a silicone compound having an amino group is applied to the coated surface of the semi-finished product or extruded product after it leaves the heating furnace, or wherein a silicone compound having an amino group is incorporated in the urethane-based aqueous paint.
The third object of the invention can be attained by a process for producing automotive glass runs which comprises the steps of extruding a semi-finished product of automotive glass run as while is continuously coated with a silane-crosslinkable polyethylene, then drying and curing the product in a heating furnace, or comprises the steps of extruding a semi-finished product of automotive glass run, heating it, immediately followed by continuous coating with a silane-crosslinkable polyethylene, then drying and curing the product in a heating furnace, or comprises the steps of unrolling a semi-finished extruded product of automotive glass run while it is continuously coated with a silane-crosslinkable polyethylene, each of which processes further comprises applying an urethane resin-based aqueous paint containing a silicone compound having an amino group or a silicone compound having an amino group or a solution thereof onto the silane-crosslinkable polyethylene coat, then heating the applied product in a heating furnace to dry and cure the applied aqueous paint, silicone compound or solution and to crosslink the silane-crosslinkable polyethylene.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of an abrasion tester according to a method specified by the Japan Society for Promotion of Scientific Research;
FIG. 2 is an illustration of a glass run product;
FIG. 3 is an illustration of another type of glass run product; and
FIG. 4 illustrates how a glass run product is subjected to an abrasion test or a sliding resistance test
DETAILED DESCRIPTION OF THE INVENTION
The following is the description of a mode for carrying out the invention as it relates to a paint composition for automotive weather strips.
The curable urethane-based emulsion paint which is used as the base of the paint composition is a urethane-based emulsion paint which typically uses an isocyanate-, melamine-, epoxy- or carbodiimide-based curing agent.
Examples of the silane coupling agent having an amino group include γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane.
Examples of the silane coupling agent having an epoxy group include γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane and β-(3,4-epoxycyclohexyl)ethyltrimethoxysilane.
Examples of the silane coupling agent having a methacryloxy group include γ-methacryloxypropyltrimethoxysilane, γ-methacryloxypropyltriethoxysilane, γ-methacryloxypropylmethyldiethoxysilane and 3-acryloxypropylmethoxysilane.
At least two of the silane coupling agents listed above or their reaction product is preferably added in an amount of 10 to 40 parts by weight per 100 parts by weight of the involatile content in the base curable urethane-based emulsion paint.
The following is the description of a mode for carrying out the invention as it relates to a process for producing automotive weather strips.
The substrate of automotive weather strips is not limited in any particular way but thermoplastic elastomers are preferably used.
The urethane-based aqueous paint may be a urethane-based emulsion paint which typically uses an isocyanate-, melamine-, epoxy- or carbodiimide-based curing agent.
Preferred examples of the silicone compound having an amino group include aminosilane coupling agent such as γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, as well as amino-modified silicone oils.
If the silicone compound having an amino group is to be applied to the coated surface of the substrate as it emerges from the drying oven, it may be diluted with water. The application method is in no way limited and spraying and brushing may be mentioned as typical examples.
The following is the description of a mode for carrying out the invention as it relates to a process for producing automotive glass runs.
The urethane-based aqueous paint may be a urethane-based emulsion paint which typically uses an isocyanate-, melamine-, epoxy- or carbodiimide-based curing agent.
The silane-crosslinkable polyethylene which is to be applied to the bottom portion of a semi-finished extruded product of automotive glass run is as easily processable as common polyethylenes before crosslinking but, once processed, exhibits better sliding and wear-resistant properties than ultrahigh molecular-weight polyethylenes; hence, the silane-crosslinkable polyethylene is suitable for use as a sliding member in the bottom portions of glass runs that require high wear resistance.
The silane-crosslinkable polyethylene reacts with water and condenses through the removal of alcohol to thereby become crosslinked. If the aqueous paint containing the silicone compound having an amino group is applied to the silane-crosslinkable polyethylene coat, which is then dried and cured in a heating furnace, the water in the aqueous paint and the silicone compound having an amino group which has a catalytic action in the condensation of silane crosslinks by removal of alcohol work together to cause rapid crosslinking and curing of the applied silane-crosslinkable polyethylene coat. The silicone compound having an amino group offers the added advantage of promoting the curing of the as-applied aqueous paint film, thereby increasing its adhesion to the EPDM rubber or silane-crosslinkable polyethylene.
The lip portions of glass runs do not require as high wear resistance as their bottom portions. On the other hand, they should have better sealing and handling properties, higher ability to prevent rattling sound and dust scratching, and more attractive appearance; therefore, the sliding member to be used in the lip portions should not impair the softness and flexibility of the substrate rubber and is suitably based on polyurethane resins.
Preferred examples of the silicone compound having an amino group include aminosilane coupling agents such as γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane and N-β-(aminoethyl) -γ-aminopropyltrimethoxysilane, as well as amino-modified silicone oils. The silicone compound having an amino group is preferably incorporated in amounts ranging from 2 to 15 parts by weight per 100 parts by weight of the involatile content of the aqueous paint.
Coating with the silane-crosslinkable polyethylene may be accomplished by coextrusion with rubber or it may be applied after vulcanization while the rubber is still hot.
The present invention will now be described by way of reference to the Figures, which should in no way be construed as limiting the present invention. FIG. 1 is a schematic representation of an abrasion tester according to a method specified by the Japan Society for the Promotion of Scientific Research, in which D is an abrading glass plate (t=3.5 mm) and E is a coated sample. FIG. 2 is an illustration of a glass run product, in which F is a coated site, G is crosslinked PE, and H is EPDM rubber. FIG. 3 is an illustration of another glass run product, in which F is a coated site and H is EPDM rubber. FIG. 4 illustrates how a glass run product is subjected to an abrasion test or a sliding resistance test.
EXAMPLES
The present invention is illustrated in greater detail below with reference to the following Examples, but the invention should not be construed as being limited thereto.
Examples 1 and 2 and Comparative Example 1
The data in Table 1 demonstrates the advantages of the paint composition according to the invention. Two samples of a curable urethane polymer were mixed with two silane coupling agents to prepare two paint compositions, which were tested for adhesion, wear resistance and dynamic friction coefficient. The results are shown in Table 1 together with those of a comparative paint composition.
TABLE 1
Comp. Ex.
Ex. 1
Ex. 2
Ex. 3
Amount
Curable
100.0
100.0
100.0
(parts by
urethane
wt.)
polymer
Silane A
8.0
8.0
8.0
Silane B
8.0
—
—
Silane C
—
8.0
8.0
Adhesion (N/cm)
7.0
7.0
4.0
Wear resistance
30,000
20,000
10,000
(cycles) 1
Dynamic friction
≦0.1
≦0.1
0.2
coefficient (μK)
Silance coupling agent A: γ-glycidoxypropyltrimethoxysilane (KBM-403 of Shin-Etsu Chemical Co., Ltd.; TSL 8350 of GE Toshiba Silicone; SH-6040 of Toray Dow Silicone)
Silane coupling agent B: 3-acryloxypropyltrimethoxysilane (KBM-5103 of Shin-Etsu Chemical Co., Ltd.)
Silane coupling agent C: γ-aminopropyltrimethoxysilane (KBM-903 of Shin-Etsu Chemical Co., Ltd.; TSL 8330 of GE Toshiba Silicone)
1 Wear resistance: The coated surface was rubbed with a glass plate (see FIG. 1) until the substrate became exposed. The wear resistance of the sample was evaluated in terms of the number of cycles the glass plate was reciprocated before the substrate showed.
Examples 3 and 4 and Comparative Examples 2 and 3
The data in Table 2 demonstrates the advantages of the process for producing an automotive weather strip according to the invention. Extruded, heated and later cooled automotive weather strips were coated with two samples of urethane-based aqueous paint containing γ-aminopropyltrimethoxysilane as a silicone compound having an amino group, thereby preparing weather strip products, which were tested for wear resistance. The results are shown in Table 2 together with those of two comparative products.
TABLE 2
Ex.3
Ex4
Comp. 2
Comp. 3
Treatment with
yes
yes
no
no
silicon compound 1
Drying/curing
200° C. ×
80° C. ×
200° C. ×
80° C. ×
conditions
10 min
10 min
10 min
10 min
Wear
EPDM
20,000
20,000
10,000
5,000
resistance
rubber
(cycles) 2
TPO
5,000
5,000
2,000
100
1 Silicone compound: Gamma-aminopropyltrimethoxysilane (KBM-903 of Shin-Etsu Chemical Co., Ltd.; TSL 8330 of GE Toshiba Silicone) was processed into a 10% solution by means of ion-exchanged water.
2 Wear resistance: The coated surface was rubbed with a glass plate (see FIG. 1) until the substrate became exposed. The wear resistance of the sample was evaluated in terms of the number of cycles the glass plate was reciprocated before the substrate showed.
Examples 5-7 and Comparative Examples 4-6
The data in Table 3 demonstrates the advantages of the process for producing a glass run according to the invention. Glass run products made using γ-aminopropyltrimethoxysilane as a compound having an amino group were tested for wear resistance, resistance to sliding and adhesion to EPDM rubber and crosslinked polyethylene (PE). The results are shown in Table 3 together with those of comparative products.
TABLE 3
Ex. 5
Ex. 6
Ex. 7
Comp. 4
Comp. 5
Comp. 6
Amount
Curable urethane
100.0
—
100.0
100.0
—
100.0
(parts by
polymer
wt.) in
Silane coupling
10.0
10.0
10.0
—
—
—
coating film
agent 1)
(F)
Ion-exchanged water
—
90.0
—
—
—
—
Wear resistance (cycles) 2)
40,000
—
40,000
10,000
—
10,000
Sliding resistance
3.0
3.0
5.0
—
5.0
(N/100 mm) 3)
Adhesion to EPDM rubber_(H) 4)
◯
—
◯
Δ
—
Δ
Adhesion to cross-linked PE (G) 4)
◯
◯
—
X
X
—
Glass run product
FIG. 1
FIG. 1
FIG. 2
FIG. 1
FIG. 1
FIG. 2
1) Silane coupling agent: Gamma-aminopropyltrimethoxysilane (KBM-903 of Shin-Etsu Chemical Co., Ltd.; TSL 8330 of GE Toshiba Silicone).
2) Wear resistance: A glass run product (see FIG. 2 or 3) was set on a test jig (see FIG. 4) and a glass plate (100 × 70 mm; t = 3.5 mm) was allowed to slide back and forth until the substrate became exposed in the coated lip portions and the bottom portion. The wear resistance was evaluated in terms of the number of cycles the glass plate was reciprocated before the substrate showed.
3) Sliding resistance: A glass run product (see FIG. 2 or 3) was set on a test jig (see FIG. 4) and a glass plate (100 × 70 mm, t = 3.5 mm) was allowed to slide for a distance of 70 mm; the resulting resistance was measured.
4) Adhesion: The coated surface was rubbed with a calico cloth under a load of 1 kg until either the coat transferred to the cloth or the substrate became exposed. (The criteria for rating were: ◯, neither transfer to the cloth nor exposure of the substrate; X, the substrate became exposed).
1) Silane coupling agent: Gamma-aminopropyltrimethoxysilane (KBM-903 of Shin-Etsu Chemical Co., Ltd.; TSL 8330 of GE Toshiba Silicone.
2) Wear resistance: A glass run product (see FIG. 2 or 3 ) was set on a test jig (see FIG. 4) and a glass plate (100×70 mm; t=3.5 mm) was allowed to slide back and forth until the substrate became exposed in the coated lip portions and the bottom portion. The wear resistance was evaluated in terms of the number of cycles the glass plate was reciprocated before the substrate showed.
3) Sliding resistance: A glass run product (see FIG. 2 or 3 ) was set on a test jig (see FIG. 4) and a glass plate (100×70 mm, t=3.5 mm) was allowed to slide for a distance of 70 mm; the resulting resistance was measured.
4) Adhesion: The coated surface was rubbed with a calico cloth under a load of 1 kg until either the coat transferred to the cloth or the substrate became exposed. (The criteria for rating were: o, neither transfer to the cloth nor exposure of the substrate; X, the substrate became exposed).
As described on the foregoing pages, the paint composition for automotive weather strips according to the present invention can achieve strong adhesion to the EPDM rubber without corona discharge, primer application or other pretreatments on the substrate surface while exhibiting high wear resistance.
The processes for producing automotive weather strips according to the present invention do not require the as-applied coat to be cured completely in a drying oven but they permit it to be cured completely by the heat inertia of the drying step and they can also shorten the length of the drying oven or lower the drying temperature. The improvement in productivity is particularly noticeable if thermoplastic elastomers such as TPO are used as the substrate of automotive weather strips.
The processes for producing automotive glass runs according to the present invention are such that by using these processes, automotive glass runs having high wear resistance in the bottom portion while exhibiting high softness and flexibility in the lip portions can be produced efficiently and with minimum impact on the global environment.
While the present invention has been described in detail and with reference to specific examples thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
|
A paint composition for automotive weather strips and glass runs which comprises a curable urethane-based emulsion paint having added hereto either at least two silane coupling agents selected from the group consisting of a silane coupling agent having an amino group, a silane coupling agent having an epoxy group, a silane coupling agent having a methacryloxy group and a silane coupling agent having an acryloxy group, or a reaction product obtained by previously mixing said at least two silane coupling agents. Also, discloses are processes for producing automotive weather strips.
| 2
|
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This applications claims priority to Canadian Patent Application No. 2,642,174 filed Feb. 3, 2009. The entire disclosure is incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] 1. Statement of the Technical Field
[0003] The inventive arrangements relate to articles of manufacture (e.g., garments and bags), and more particularly to articles of manufacture that are adjustable in size.
[0004] 2. Description of the Related Art
[0005] There are various conventional multi-stage expandable-contractible systems known in the art for providing expansion and contraction capabilities to bags and garments. The bags include, but are not limited to, luggage bags, duffle bags, sports bags, purses, backpacks, brief cases and hand carried bags. The garments include, but are not limited to, shirts, pants, jackets and sweaters.
[0006] Such a conventional multi-stage expandable-contractible system generally includes an inset element that extends circumferentially around a bag, a sleeve or a pant leg. The inset element includes a single slide fastener configured to provide two or more successive stages of expansion and contraction. In this regard, the slide fastener comprises a zipper element having a three dimensional multi-turn spiral configuration. During use, the expandable inset element is selectively expanded and contracted in a multi-stage fashion by displacing an actuator (or zipper slider) of the zipper element one or more spiral turns at any given time. For example, the expandable inset element is transitioned from a contracted position to a first stage expanded position by displacing the actuator once about a periphery of the bag, sleeve or pant leg. Similarly, the expandable inset element is transitioned from a contracted position to a second stage expanded position by displacing the actuator twice about the periphery of the bag, sleeve or pant leg.
[0007] Despite the advantages of the conventional multi-stage expandable-contractible system discussed above, it suffers from certain drawbacks. For example, the spiral zipper element of the conventional multi-stage expandable-contractible system can not be used in two (2) dimensional applications. Also, the expandable inset element can not be simultaneously placed in a first stage partially expanded position and a second stage partially expanded position. Further, the conventional multi-stage expandable-contractible system can not be assembled in a fully automated process. As such, a bag or garment employing the conventional multi-stage expandable-contractible system is relatively expensive to manufacture.
SUMMARY OF THE INVENTION
[0008] Embodiments of the present invention concern methods for adjusting a volume of an article of manufacture having an expandable-contractible system. The methods generally involve displacing a first actuator in a first direction along first tracks coupled to the article of manufacture. The first actuator can be displaced along the first tracks until it (a) disengages a first one of the first tracks and (b) abuts a first stop mechanism formed at a first end of a second one of the first tracks. The first stop mechanism can be formed by: attaching a grommet to the first end of the second one of the first tracks; or bending the first end of the second one of the first tracks. The first tracks can have a rectilinear shape or a curvilinear shape.
[0009] The methods also involve unfolding a first flexible insert so as to adjust the volume of the article of manufacture by a first amount. The first amount can be defined by the geometrical dimensions of the first flexible insert. The first flexible insert is coupled to at least the first one of the first tracks.
[0010] The methods further involve displacing a second actuator in a second direction along second tracks coupled to the article of manufacture. The second actuator can be displaced in a second direction along the second tracks until it abuts a second stop mechanism formed at first ends of the second tracks. The second tracks can have a rectilinear shape or a curvilinear shape. The second stop mechanism can be formed by joining the first ends of the second tracks together. The second direction can be the same as or different than the first direction. Notably, the second actuator and the second tracks are concealed in the article of manufacture when the expandable-contractible system is not in use.
[0011] A second flexible insert is unfolded so as to further adjust the volume of the article of manufacture by a second amount defined by geometrical dimensions of the second flexible insert. The second flexible insert is coupled to the second tracks. The second amount can be greater than, equal to or less than the first amount.
[0012] The volume of the article of manufacture can be decreased by folding the first flexible insert and displacing the first actuator in a third direction opposed from the first direction alone the first tracks. The volume of the article of manufacture can also be decreased by folding the second flexible insert and displacing the second actuator in a fourth direction opposed from the second direction along the second tracks.
[0013] Embodiments of the present invention also concern expandable-contractible systems implementing the above described methods for adjusting a size of an article of manufacture. Each of the expandable-contractible systems comprises at least two first tracks having non-spiral shapes, at least two second tracks having non-spiral shapes, a first actuator, a first flexible insert, a second actuator and a second flexible insert. The second tracks are disposed in the expandable-contractible system so as to be concealed at least partially by the first tracks when the expandable-contractible system is not in use. The first actuator is configured for being displaced in a first direction along the first tracks. The first actuator is also configured for being disengaged from a first one of the first tracks. The first flexible insert is configured to be transitioned from a folded position to an unfolded position in which the size of the article of manufacture is increased by a first amount defined by geometrical dimensions of the first flexible insert. The second actuator is configured for being displaced in a second direction along the second tracks. The second flexible insert is configured to he transitioned from a folded position to an unfolded position in which the size of the article of manufacture is increased by a second amount defined by geometrical dimensions of the second flexible insert.
[0014] Embodiments of the present invention further concern expandable-contractible systems for adjusting an overall size of an article of manufacture. Each of the expandable-contractible systems comprises first and second closure elements. The first closure element is of first type of closure element. The second closure element is of a second type or closure element. The first type of closure element is different from the second type of closure element. For example, the first type of closure element includes, but is not limited to, a zipper assembly. In contrast, the second type of closure element includes, but is not limited to, a velcro closure element, a loop-and-pile fastener assembly, a snap assembly, a button/hole pair assembly and a latch assembly.
[0015] Embodiments of the present invention further concerns bags having the same or substantially similar types of closure elements. Each of the bags includes at least one compartment structure defining an interior space for carrying articles. The bag also includes an expandable-contractible system configured for adjusting a size of the interior space. The expandable-contractible system comprises at least two first tracks having non-spiral shapes, at least two second tracks having non-spiral shapes, a first actuator, a first flexible insert, a second actuator and a second flexible insert. The second tracks are disposed in the expandable-contractible system so as to be concealed at least partially by the first tracks when the expandable-contractible system is not in use. The first actuator is configured for being displaced in a first direction along the first tracks. The first actuator is also configured for being disengaged from a first one of the first tracks. The first flexible insert is configured to he transitioned from a folded position to an unfolded position in which the size of the interior space is increased by a first amount defined by geometrical dimensions of the first flexible insert. The second actuator is configured for being displaced in a second direction along the second tracks. The second flexible insert is configured to be transitioned from a folded position to an unfolded position in which the size of the interior space is increased by a second amount defined by geometrical dimensions of the second flexible insert.
[0016] Embodiments of the present invention also concerns bag comprising different types of closure elements. Each of the bags includes at least one compartment structure defining an interior space for carrying articles. The bag also includes an expandable-contractible system for adjusting an overall size of the bag. The expandable-contractible system comprises first and second closure elements. The first closure element is of a first type of closure element. The second closure element is of a second type of closure element. The first type of closure element is different from the second type of closure element. For example, the first type of closure element includes, but is not limited to, a zipper assembly. In contrast, the second type of closure element includes, but is not limited to, a velcro closure element, a loop-and-pile fastener assembly, a snap assembly, a button/hole pair assembly and a latch assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Embodiments of the present invention will be described with reference to the following drawing figures, in which like numerals represent like items throughout the figures and in which:
[0018] FIG. 1 is a perspective view of an exemplary article of manufacture comprising a multi-stage expandable-contractible system that is useful for understanding the present invention.
[0019] FIG. 2 is a perspective view of the bag of FIG. 1 having a primary compartment structure in a partially opened position that is useful for understanding the present invention.
[0020] FIG. 3 is a perspective view of the bag of FIG. 1 in a first stage expanded position that is useful for understanding the present invention.
[0021] FIG. 4 is a perspective view of the bag of FIG. 1 in a second stage expanded position that is useful for understanding the present invention.
[0022] FIG. 5 is an exploded view of the multi-stage expandable-contractible system shown in FIG. 1 that is useful for understanding the present invention.
[0023] FIG. 6 is a flow diagram of an exemplary method for adjusting a volume of an article of manufacture that is useful for understanding the present invention.
DETAILED DESCRIPTION
[0024] The present invention is described with reference to the attached figures, wherein like reference numbers are used throughout the figures to designate similar or equivalent elements. The figures are not drawn to scale and they are provided merely to illustrate the instant invention. Several aspects of the invention are described below with reference to example applications for illustration. It should be understood that numerous specific details, relationships, and methods are set forth to provide a full understanding of the invention. One having ordinary skill in the relevant art, however, will readily recognize that the invention can be practiced without one or more of the specific details or with other methods. In other instances, well-known structures or operations are not shown in detail to avoid obscuring the invention. The present invention is not limited by the illustrated ordering of acts or events, as some acts may occur in different orders and/or concurrently with other acts or events. Furthermore, not all illustrated acts or events are required to implement a methodology in accordance with the present invention.
[0025] The present invention generally concerns multi-stage expandable-contractible systems that can he used in a variety of applications. Such applications include, but are not limited to, bag applications and clothing applications. The multi-stage expandable-contractible system generally comprises a plurality of inset elements configured to provide two or more stages of expansion and contraction.
[0026] Notably, the present invention overcomes various drawbacks of conventional multi-stage expandable-contractible systems. For example, the multi-stage expandable-contractible system of the present invention can be used in two (2) dimensional applications. As such, the multi-stage expandable-contractible system can be integrated along a length of a shirt sleeve, a pant leg, and a panel of a bag. Also, the multi-stage expandable-contractible system can be simultaneously placed in a first stage partially expanded position and a second stage partially expanded position. The multi-stage expandable-contractible system can further be implemented during a fully automated process. As such, an article employing the present invention is less expensive to manufacture as compared to articles comprising conventional multi-stage expandable-contractible systems.
[0027] The present invention will now be described in more detail in relation to FIGS. 1-5 . Although the present invention will be described in relation to a bag, the present invention is not limited in this regard. For example, the present invention can also be used with other articles of manufacture, such clothing (e.g., shirts, pants, gloves and boots).
[0028] In FIG. 1 , there is provided a perspective view ofan exemplary bag 100 in a closed position. A perspective view of the bag 100 in a partially opened position is provided in FIG. 2 . Notably, the bag 100 comprises a multi-stage expandable-contractible system 102 . The multi-stage expansion/contraction system 102 is generally configured to facilitate the expansion and contraction of the bag 100 . The multi-stage expandable-contractible system 102 will be described in detail below in relation to FIGS. 3-5 .
[0029] As shown in FIGS. 1-2 , the bag 100 includes wheeled luggage comprising wheels 150 and an extendable handle 104 that allow for convenient maneuverability thereof. Embodiments of the present invention are not limited in this regard. For example, the bag 100 can alternatively include a backpack, a purse, a garment bag, a sports bag, a travel bag, a duffle bag, a backpack or a carry-on bag.
[0030] As also shown in FIGS. 1-2 , the bag 100 includes a primary compartment structure 106 and a plurality of secondary compartment structures 108 , 110 for carrying articles. Such articles include, but are not limited to, cloths, shoes, towels, toys, fluid/liquid products, books, school supplies, toiletries, makeup and other items. The primary and secondary compartment structures 106 , 108 , 110 can be formed from any suitable material. Such materials include, but are not limited to, non-woven materials, woven materials, mesh materials, water-resistant materials, leather, canvas, collapsible fabric materials, fabric materials impregnated with plastic, and fabric materials impregnated with a rubberized material. Notably, each of the compartment structures 106 , 108 , 110 can be formed from the same material or different material(s). The material(s) forming the compartment structures 106 , 108 , 110 can have a design or pattern printed thereon so as to provide an ornamental or decorative appearance to the bag 100 .
[0031] Notably, the primary compartment structure 106 is joined to the secondary compartment structure 108 by the multi-stage expandable-contractible system 102 . Consequently, the primary compartment structure 106 is movable with respect to the secondary compartment structure 108 such that the bag 100 is adjustable between a contracted position (shown in FIG. 1 ) and a plurality of expanded positions (shown in FIGS. 3-4 ). The multi-stage expandable-contractible system 102 will be described in detail below.
[0032] Although two (2) secondary compartment structures are shown in FIGS. embodiments of the present invention are not limited in this regard. The bag 100 can include more or less secondary compartment structures than those shown in FIGS. 1-2 . For example, the bag 100 can include at least one secondary compartment structure 108 , 110 disposed on a front panel 112 of the primary compartment structure 106 (as shown in FIGS. 1-2 ) and at least one secondary compartment structure disposed on a sidewall 114 of the primary compartment structure 106 (not shown in FIGS. 1-2 ). Secondary compartment structures can also be provided inside the bag 100 (not shown in FIGS. 1-2 ). In this scenario, the secondary compartment structures can be coupled to inner surfaces 202 , 204 , 206 , 208 , 210 , 212 of the panels 112 , 116 and/or sidewalls 114 of the bag 100 .
[0033] The primary compartment structure 106 may be considered the primary article-carrying compartment structure because it provides the largest unrestricted volume for carrying articles. If only the primary compartment structure 106 is desired to be used, then one would only need to open the primary compartment structure 106 via a closure element 118 . This configuration is ideal for carrying articles which require the volume of the primary compartment structure 106 . Such articles can include, but are not limited to, electronic equipment, clothing, books, sports equipment, retractable umbrellas, and thermoses.
[0034] As shown in FIGS. 1-2 , the primary compartment structure 106 has a front panel 112 defining a first bag opening 228 which is selectively closable via the closure element 118 . The closure element 118 can include, but is not limited to, a zipper assembly (shown in FIGS. 1-2 ), a velcro closure element, loop-and-pile fasteners, snaps, button/hole pairs and latches. The closure element 118 extends around at least a portion of a periphery of the bag 100 . If the closure element 118 includes a zipper assembly, then it includes a first track 214 , a second track 216 and at least one actuator 154 , 156 . In this scenario, the tracks 214 , 216 include sets of teeth and the actuator 154 , 156 includes a zipper slider. A portion of the first track 214 is coupled to the front panel 112 of the primary compartment structure 106 . A portion of the second track 216 is coupled to the multi-stage expandable-contractible system 102 . The actuator 154 , 156 is coupled to the tracks 214 , 216 so as to facilitate the separation and joinment thereof. For example, the tracks 214 , 216 are separated and joined by moving the actuator(s) 154 , 156 around at least a portion of the periphery of the bag 100 . Notably, the actuator(s) 154 , 156 is(are) unable to be detached or disengaged from the tracks 214 , 216 . The tracks 214 , 216 and actuator(s) 154 , 156 can be formed from plastic or metal.
[0035] The primary compartment structure 110 also includes the back panel 116 and at least one sidewall 114 which extends between the front panel 112 and the back panel 116 . At least one of the panels 112 , 116 and sidewalk 114 is formed of a rigid or semi-rigid material suitable to maintain its shape and structural integrity during use of the bag 100 . Alternatively, at least one of the panels 112 , 116 and sidewalls 114 includes a rigid or semi-rigid insert. A ribbing or tubing 120 can be utilized to provide additional stability and rigidity to the bag 100 . The ribbing or tubing 120 can be disposed around peripheral edges 122 , 124 of at least one of the panels 112 , 116 and/or sidewalls 114 . The ribbing or tubing 120 can include, but is not limited to, a plastic tubing and a rubber tubing.
[0036] Notably, the panels 112 , 116 and sidewalls 114 of the primary compartment structure 110 define a first interior space 226 sized and shaped to carry various articles. In this regard, it should be understood that the panels 112 , 116 and sidewalls 114 are joined together via a plurality of joinder lines 128 , 130 , 132 , 134 . Each of the joinder lines 128 , 130 , 132 , 134 can be formed from a sewn stitching, adhesive bonding and/or heat bonding. If the joinder lines 128 , 130 , 132 , 134 include sewn stitching, then the seams formed From coupling the components 112 , 114 , 116 together can be water-tight and/or air-tight.
[0037] The secondary compartment structures 108 , 110 are considered the secondary article-carrying compartment structures because they provide smaller volumes for carrying articles as compared to the main compartment structure 106 . If a secondary compartment structure 108 , 110 is desired to be used, then one would need to open it via a respective closure element 144 , 162 of the secondary compartment structure 108 , 110 . This configuration is useful for carrying articles which are not to be commingled with articles disposed in the main compartment structure 106 , or vice versa. Such articles include, but are not limited to, pens, pencils, calculators, mobile telephone, cellular phones, personal digital assistants, handheld personal computers, sports cloths, sport shoes, towels, wet cloths, and fluid/liquid products.
[0038] Accordingly, the secondary compartment structure 108 includes sidewalk 140 , 142 defining a second bag opening (not shown in FIGS. 1-2 ). At least a portion of the sidewall 142 is attached to the hag 100 via a U-shaped closure element 144 . The U-shaped closure element 144 provides a means for selectively opening and closing the second bag opening (not shown in FIGS. 1-2 ). The closure element 144 can include, but is not limited to, a zipper assembly (as shown in FIGS. 1-2 ), a velcro assembly, loop-and-pile Fasteners, snaps, button/hole pairs and latches. The sidewall 140 is joined to the main compartment structure 106 via at least the joinder line 132 . The sidewall 142 is joined to the sidewall 140 via at least one joinder line 160 . The joinder lines 132 , 160 can he formed from sewn stitching, adhesive bonding and/or heat bonding.
[0039] The secondary compartment structure 110 is coupled to secondary compartment structure 108 so as to define a third bag opening (not shown in FIGS. 1-2 ). The third bag opening (not shown in FIGS. 1-2 ) is selectively opened and closed using a closure element 162 . The closure element 162 can include, but is not limited to, a zipper assembly (as shown in FIGS. 1-2 ), a velcro assembly, loop-and-pile Fasteners, snaps, button/hole pairs and/or latches.
[0040] As noted above, the bag 100 includes an extendable handle 104 . The extendable handle 104 can formed from any suitable material. Such materials include, but are not limited to, plastics and metals. The bag 100 can additionally or alternatively include one or more non-extendable handles 170 , 172 and a mechanical fastener 174 . The non-extendable handles 170 , 172 can be formed from any suitable material. Such materials include, but are not limited to, leather, plastic, wood, metal, non-woven fabric, woven fabric, canvas, mesh materials, collapsible fabric materials, a flat rope or a combination thereof. The non-extendable handles 170 , 172 are attached to the bag 100 via sewn stitching, adhesive bonding and/or mechanical connectors (e.g., a clip or hook/loop fastener). The mechanical fastener 174 provides a means for attaching objects (e.g., carry-on bags, purses, and backpacks) to the bag 100 . In this regard, the mechanical fastener 174 can include, but is not limited to, a buckle and/or a loop, The mechanical fastener 174 is attached to the bag 100 via sewn stitching, an adhesive bond and/or a mechanical connector (e.g., a clip or snap assembly).
[0041] An exemplary embodiment of the multi-stage expandable-contractible system 102 will now be described in detail in relation to FIGS. 3-5 . A perspective view of the multi-stage expandable-contractible system 102 in a first stage expanded position is provided in FIG. 3 . A perspective view of the multi-stage expandable-contractible system 102 in a second stage expanded position is provided in FIG. 4 . An exploded view of the multi-stage expandable-contractible system 102 is provided in FIG. 5 .
[0042] As noted above, the multi-stage expandable-contractible system 102 is generally configured to facilitate the expansion of the bag 100 so as to provide a compartment structure of a bag with an increased volume for carrying articles. Notably, the multi-stage expandable-contractible system 102 overcomes various drawbacks of conventional multi-stage expandable-contractible systems. For example, the multi-stage expandable-contractible system 102 can be used in two (2) dimensional applications. As such, the multi-stage expandable-contractible system 102 can be integrated along a length of at least one panel 112 , 116 or sidewall 114 of the bag 100 . Also, the multi-stage expandable-contractible system 102 can be simultaneously placed in a first stage partially expanded position (not shown in FIGS. 1-5 ) and a second stage partially expanded position (not shown in FIGS. 1-5 ). The multi-stage expandable-contractible system 102 can further be implemented during a fully automated process. As such, the bag 100 including the multi-stage expandable-contractible system 102 is less expensive to manufacture as compared to a bag comprising conventional multi-stage expandable-contractible systems.
[0043] As shown in FIGS. 3-5 , the multi-stage expandable-contractible system 102 comprises a plurality of elongated closure elements 302 , 304 and a plurality of elongated flexible inserts 306 , 406 . Notably, when the multi-stage expandable-contractible system 102 is in its contracted position shown in FIGS. 1-2 , the closure element 304 is concealed in the bag 100 . Consequently, the bag 100 has a more appealing overall appearance when the multi-stage expandable-contractible system 102 is in its contracted position as compared to the appearance of a bag including a conventional multi-stage expandable-contractible system. When the multi-stage expandable-contractible system 102 is in a first stage expanded position shown in FIG. 3 , the closure element 304 is visible to an observer as shown in FIG. 4 .
[0044] Although the closure elements 302 , 304 are shown in FIGS. 3-5 to have rectilinear shapes, embodiments of the present invention are not limited in this regard. For example, the closure elements 302 , 304 can alternatively have curvilinear shapes or other desirable shapes. Also, the closure elements 302 , 304 need not be parallel to one another when the multi-stage expandable-contractible system 102 is in its contracted position and/or expanded position. Alternatively, the closure elements 302 , 304 can be perpendicular to each other, diagonal to each other or offset with respect to each other when the multi-stage expandable-contractible system 102 is in its contracted position and/or expanded position. Further, the closure elements 302 , 304 can be of the same type or different types of closure elements. For example, both of the closure elements 302 , 304 can include a zipper assembly as shown in FIG. 4 . Alternatively, at least one of the closure elements 302 , 304 can include a velcro closure assembly (not shown). Embodiments of the present invention are not limited in this regard.
[0045] Each of the flexible inserts 306 , 406 can be formed of any suitable material. Such materials include, but are not limited to, leathers, plastics, non-woven fabrics, woven fabrics, canvases, mesh materials, collapsible fabric materials, flat ropes and combinations thereof. Although the closure elements 302 , 304 and flexible inserts 306 , 406 are shown in FIGS. 3-4 to extend around the entire periphery of the bag 100 , embodiments of the present invention are not limited in this regard. For example, the closure elements 302 , 304 and flexible inserts 306 , 406 can alternatively extend around a portion of the periphery of the bag 100 . In this scenario, the closure elements 302 , 304 and flexible inserts 306 , 406 can extend along a length of one or more panels 112 , 116 or sidewalls 114 of the bag 100 .
[0046] A first closure element 302 of the plurality of elongated closure elements 302 , 304 is generally configured to facilitate the transition of the multi-stage expandable-contractible system 102 from the contracted position shown in FIGS. 1-2 to the first stage fully expanded position shown in FIG. 3 or a first stage intermediary position (not shown), and vise versa.
[0047] As such, the first closure element 302 can include, but is not limited to, a zipper assembly (shown in FIGS. 1-5 ), a velcro assembly, loop-and-pile fasteners, snaps, button/hole pairs and latches.
[0048] If the first closure element 302 includes a zipper assembly (as shown in FIGS. 1-5 ), then it includes a first track 308 , a second track 310 , at least one actuator 312 , at least one actuator pull tab 330 , and a plurality of stop mechanisms 360 , 560 , 504 . Each of the tracks 308 , 310 includes a plurality of teeth members 314 a, 314 b coupled to a flexible member 316 a, 316 b via any suitable means. The teeth members 314 a, 314 b can be formed of plastic or metal. The flexible members 316 a, 316 b can be formed from any suitable material. Such materials include, but are not limited to, leathers, tapes, plastics, non-woven fabrics, woven fabrics, canvases, mesh materials, collapsible fabric materials, flat ropes and combinations thereof.
[0049] Each of the flexible members 316 a, 316 b is coupled to the hag 100 via sewn stitching, adhesive bonding and/or heat bonding. For example, a first flexible member 316 a is joined to a first portion 318 of the sidewalls 114 of the primary compartment structure 106 . Similarly, a second flexible member 316 b is joined to a second portion 320 of the sidewalls 114 of the primary compartment structure 106 . Notably, the flexible members 316 a, 316 b are attached to the bag 100 such that the tracks 308 , 310 oppose each other in a manner that allows for the interlocking of the respective teeth members 314 a, 314 b. The teeth members 314 a, 314 b are interlocked by the displacement of the actuator 312 along the lengths of the tracks 308 , 310 . The actuator 312 is displaced along the lengths of the tracks 308 , 310 by the pulling of the actuator pull tab 330 over the teeth members 314 a, 314 b.
[0050] As noted above, the first closure element 302 includes three (3) stop mechanisms 360 , 560 , 504 . Each of the stop mechanisms 360 , 560 is configured to prevent the actuator 312 from traveling past an end 362 , 562 of a respective track 308 , 310 . The stop mechanisms 360 , 560 can be formed by bending and attaching the ends 362 , 562 of the tracks 308 , 310 to the bag 100 so that the actuator 312 is prevented from sliding past the ends 362 , 562 of the tracks 308 , 310 . Alternatively, the stop mechanisms 360 , 560 can include, but are not limited to, grommets (not shown in FIGS. 1-5 ). The stop mechanism 504 is configured to prevent the actuator 312 from traveling past an end 510 of the second track 310 . The stop mechanism 504 can include, but is not limited to, a grommet 508 as shown in FIG. 5 .
[0051] Notably, the end 350 of the first track 308 is absent of a stop mechanism. Instead, the end 350 includes an engagement member 352 sized and shaped for insertion in an aperture (not shown) of the actuator 312 . As such, the actuator 312 can travel past the end 350 so as to be disengaged from the first track 308 . The actuator 312 can be aligned and re-engaged with the first track 308 by inserting the engagement member 352 in the aperture (not shown) thereof. Consequently, the multi-stage expandable-contractible system 102 can be transitioned from its contracted position shown in FIG. 1 to its first stage fully expanded position shown in FIG. 3 or a first stage intermediary position, and vice versa. In the first stage fully expanded position, the flexible insert 306 is unfolded so as to extend between the front panel 112 and sidewalls 114 of the primary compartment structure 106 of the bag 100 . Accordingly, the bag 100 has a width W 1 as shown in FIG. 3 . The width W 1 is greater than the width W 0 of the bag 100 (shown in FIG. 1 ) when the multi-stage expandable-contractible system 102 is in its fully contracted position (shown in FIG. 1 ). In the contracted position, the flexible insert 306 is folded and housed in the primary compartment structure 106 of the hag 100 .
[0052] A second closure element 304 of the plurality of elongated closure elements 302 , 304 is generally configured to facilitate the transition of the multi-stage expandable-contractible system 102 from a contracted position (shown in FIGS. 1-2 ) to a second stage fully expanded position (shown in FIG. 4 ) or a first stage intermediary position (not shown), and vise versa. In the contracted position, the flexible insert 406 is folded and housed in the primary compartment structure 106 of the hag 100 . In the first stage fully expanded position, the flexible insert 406 is unfolded so as to extend between the flexible insert 306 of the multi-stage expandable-contractible system 102 and the sidewalls 114 of the primary compartment structure 106 of the bag 100 . Accordingly, the bag 100 has a width W 2 as shown in FIG. 4 . The width W 2 is greater than the width W 0 of the bag 100 (shown in FIG. 1 ) when the multi-stage expandable-contractible system 102 is in its fully contracted position (shown in FIG. 1 ). Similarly, the width W 2 is greater than the width W 1 of the hag 100 (shown in FIG. 3 ) when the multi-stage expandable-contractible system 102 is in its first stage expanded position (shown in FIG. 3 ).
[0053] The second closure element 304 can include, but is not limited to, a zipper assembly (shown in FIGS. 1-5 ), a velcro assembly, loop-and-pile fasteners, snaps, button/hole pairs and latches. If the second closure element 304 includes a zipper assembly (as shown in FIGS. 1-5 ), then it includes a First track 420 , a second track 422 , at least one actuator 424 , at least one actuator pull tab 426 , and a plurality of stop mechanisms 428 , 430 , 432 . Each of the tracks 420 , 422 includes a plurality of teeth members 434 a, 434 b coupled to a flexible member 436 a, 436 b via any suitable means. The teeth members 434 a, 434 b can be formed of plastic or metal. The flexible members 436 a, 436 b can be formed from any suitable material. Such materials include, but are not limited to, leathers, tapes, plastics, non-woven fabrics, woven fabrics, canvases, mesh materials, collapsible fabric materials, flat ropes and combinations thereof.
[0054] Each of the flexible members 436 a, 436 b is coupled to the bag 100 via sewn stitching, adhesive bonding, and/or heat bonding. For example, a first flexible member 436 a is joined to the flexible insert 306 of the multi-stage expandable-contractible system 102 . Similarly, the second flexible member 436 b is joined to portion 320 of the side panel 114 of the primary compartment structure 106 (not shown in FIGS. 1-2 ). Notably, the flexible members 436 a, 436 b are attached to the bag 100 such that the tracks 420 , 422 oppose each other in a manner that allows for the interlocking of the respective teeth members 434 a , 434 b. The teeth members 434 a, 434 b are interlocked by the displacement of the actuator 424 along the lengths of the tracks 420 , 422 . The actuator 424 is displaced along the lengths of the tracks 420 , 422 by the pulling of the actuator pull tab 426 over the teeth members 434 a , 434 b.
[0055] As noted above, the second closure element 304 includes a plurality of stop mechanisms 428 , 430 , 432 . Although the stop mechanism 428 , 430 are shown in FIG. 4 to be offset relative to the stop mechanisms 360 , 560 of the first closure element 302 , embodiments of the present invention are not limited in this regard. For example, the stop mechanisms 428 , 430 can be longitudinally aligned with the stop mechanisms 360 , 560 of the first closure element 302 .
[0056] Notably, the stop mechanisms 428 , 430 , 432 of the second closure element 304 are configured to prevent the actuator 424 from being fully disengaged from the tracks 420 , 422 . In this regard, it should be appreciated that the stop mechanism 428 is configured to prevent the actuator 424 from traveling past an end 450 of the first track 420 . The stop mechanism 430 is configured to prevent the actuator 424 from traveling past an end 452 of the second track 422 . The stop mechanism 432 is configured to prevent the actuator 424 from traveling past ends 454 of the first track 420 and end 456 of the second track 422 .
[0057] As shown in FIG. 4 , the stop mechanism 428 is formed by bending and attaching the end 450 of the first track 420 to the bag 100 so that the actuator 424 is prevented from sliding past the end 450 of the first track 420 . Similarly, the stop mechanism 430 is formed by bending and attaching the end 452 of the second track 422 to the bag 100 so that the actuator 424 is prevented from sliding past the end 452 of the second track 452 . The stop mechanism 432 is formed by joining the respective ends 454 , 456 of the tracks 420 , 422 together and/or joining the ends 454 , 456 of the tracks 420 , 422 to a v-shaped end 530 of the flexible insert 406 . Embodiments of the present invention are not limited in this regard. For example, the stop mechanisms 428 , 430 , 432 can alternatively include, but are not limited to, grommets (not shown in FIGS. 1-5 ).
[0058] As shown in FIG. 4 , the first track 420 of the second closure element 304 is shown to reside a distance D from the first track 308 of the first closure element 302 . The second track 422 of the second closure element 304 are shown to be adjacent to the second track 310 of the first closure element 302 . Embodiments of the present invention are not limited in this regard. For example, the first track 420 can reside a distance D′ from the first track 308 of the first closure element 302 . The distance D′ can be greater than or less than the distance D shown in FIG. 4 . Also, the second track 422 of the second closure element 304 can reside a distance D″ (not shown) from the second track 310 of the first closure element 302 . The distance D″ (not shown) can be selected in accordance with a particular application. For example, the distance D″ (not shown) can be equal to, greater than or less than the distance D (shown in FIG. 4 ) or D′ (not shown).
[0059] As also shown in FIG. 4 , the first and second closure elements 302 , 304 are opened and closed by displacing the actuators 312 , 424 in the same directions along the respective tracks 308 , 310 , 420 , 422 . Embodiments of the present invention are not limited in this regard. For example, the first and second closure elements 302 , 304 can alternatively be opened and closed by displacing the actuators 312 , 424 in different directions along the respective tracks 308 , 310 , 420 , 422 . The different directions can include, but are not limited to, opposing directions, orthogonal directions, and other directions that are at angles with respect to each other.
[0060] Referring now to FIG. 6 , there is provided a flow diagram of a method 600 for adjusting a volume of an article of manufacture (e.g., bag 100 ) that is useful for understanding the present invention. As shown in FIG. 6 , the method 600 begins with step 602 and continues with step 604 . In step 604 , a first actuator (e.g., actuator 312 of FIG. 3 ) is displaced in a first direction along first tracks (e.g., tracks 308 , 310 of FIG. 3 ). The first actuator is coupled to the article of manufacture. The first actuator can be displaced along the first tracks until it disengages one of the first tracks (e.g., track 308 of FIG. 3 ) and abuts a first stop mechanism (e.g., stop mechanism 504 of FIG. 5 ) formed at an end (e.g., end 510 of FIG. 5 ) of a second one of the first tracks (e.g., track 310 of FIG. 3 ). The first stop mechanism can be formed by attaching a grommet to the end of a second one of the first tracks.
[0061] After completing step 604 , step 606 is performed where a first flexible insert (e.g., flexible insert 306 of FIG. 3 ) is unfolded. As a consequence of this unfolding, the volume of the article of manufacture is increased by a first amount. The first amount can be defined by the geometrical dimensions of the first flexible insert.
[0062] In a next step 608 , a second actuator (e.g., actuator 424 of FIG. 4 ) is displaced in a second direction along second tracks (e.g., tracks 420 , 422 of FIG. 4 ). The second tracks are coupled to the article of manufacture. The second direction can be the same as or different than the first direction. The second actuator can be displaced along the second tracks until it abuts at least one second stop mechanism (e.g., stop mechanism 432 of FIG. 4 ) formed at ends (e.g., ends 454 of FIG. 4 ) of the second tracks. The second stop mechanism can be formed by joining the ends of the second tracks together.
[0063] Upon completing step 608 , the method 600 continues with step 610 . In step 610 , a second flexible insert (e.g., flexible insert 406 of FIG. 4 ) is unfolded. As a consequence of this unfolding, the volume of the article of manufacture is further increased by a second amount. The second amount can be the same as, greater than or less than the first amount. The second amount can be define by the geometrical dimensions of the second flexible insert.
[0064] The volume of the article of manufacture can be decreased by performing at least one of the steps 612 and 614 . In step 612 , the volume of the article of manufacture is decreased by: folding the second flexible insert; and/or displacing the second actuator in a third direction along the second tracks. The third direction is opposed from the second direction. The second actuator can be displaced along the second tracks until it abuts stop mechanisms (e.g., stop mechanisms 428 , 430 of FIG. 4 ) formed at second ends (e.g., ends 450 , 452 of FIG. 4 ) of the second tracks. The stop mechanisms can be formed at least partially by bending the second ends of the second tracks or attaching grommets to the second ends of the second tracks.
[0065] In step 614 , the volume of the article of manufacture is decreased by: folding the first flexible insert; and/or displacing the first actuator in a fourth direction along the first tracks. The fourth direction is opposed from the first direction. The first actuator can be displaced along the first tracks until it abuts stop mechanisms e.g., stop mechanism 360 of FIG. 3 and stop mechanism 560 of FIG. 5 ) formed at second ends (e.g., end 362 of FIG. 3 and end 562 of FIG. 5 ) of the first tracks. The stop mechanisms can be formed at least partially by bending the second ends of the first tracks or attaching grommets to the second ends of the first tracks. Subsequent to completing step 614 , step 616 is performed where the method 600 ends, returns to step 602 or continues with the performance of other actions.
[0066] The word “exemplary” is used herein to mean serving as an example, instance or illustration. Any aspect or design described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other aspects or designs. Rather, use of the word exemplary is intended to present concepts in a concrete fashion. As used in this application, the term “or” is intended to mean an inclusive “or” rather than an exclusive “or”. That is, unless specified otherwise, or clear from context, “X employs A or B” is intended to mean any of the natural inclusive permutations. That is if, X employs A; X employs B; or X employs both A and B, then “X employs A or B” is satisfied under any of the foregoing instances.
[0067] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. Furthermore, to the extent that the terms “including”, “includes”, “having”, “has”, “with”, or variants thereof are used in either the detailed description and/or the claims, such terms are intended to be inclusive in a manner similar to the term “comprising.”
[0068] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
[0069] All of the apparatus, methods and algorithms disclosed and claimed herein can be made and executed without undue experimentation in light of the present disclosure. While the invention has been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations may be applied to the apparatus, methods and sequence of steps of the method without departing from the concept. spirit and scope of the invention. More specifically, it will be apparent that certain components may be added to, combined with, or substituted for the components described herein while the same or similar results would be achieved. All such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and concept of the invention as defined.
|
Systems ( 102 ) and methods ( 600 ) for adjusting a volume of an article of manufacture (AOM). The methods involve displacing a first actuator (FA) in a first direction along tracks ( 308, 310 ) until FA ( 312 ) disengages a first track ( 308 ) and abuts a first stop mechanism ( 504 ) formed at an end ( 510 ) ofa second track ( 310 ). A first flexible insert (FFI) is unfolded so as to adjust the volume of AOM by a first amount defined by geometrical dimensions of FFI ( 306 ). A second actuator (SA) is displaced in a second direction along tracks until SA ( 424 ) abuts a second stop mechanism ( 432 ) formed at ends ( 454 ) of the tracks ( 420, 422 ). A second flexible insert (SFI) is unfolded so as to further adjust the volume of AOM by a second amount defined by geometrical dimensions of SFI ( 406 ).
| 0
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to an improved umbilical hose coupling that is useful with textile-reinforced hoses in the oil and gas industry, especially high pressure hoses for use in offshore systems. It is also useful with other hoses.
[0003] 2. Description of Related Art
[0004] FIG. 1 shows a perspective cut-away view of one prior art embodiment of a hose coupling 1 with a reinforced hose 2 having a layer of a textile 5 sandwiched between an inner liner 8 and an outer cover 7 . The hose coupling has a sleeve 3 and an insert 4 , each having a set of teeth in the area represented by 6 for engaging the hose when swaged or crimped. As shown in FIG. 1 , the coupling is not yet swaged or crimped onto the hose. For the purposes herein, the end where the sleeve and insert engage each other is the coupling end while the end terminating at the hose is the hose end. For the purposes herein, the words crimped and swaged are used interchangeably to mean the sleeve is pressed or compressed onto the hose and insert.
[0005] U.S. Pat. No. 5,255,944 to Blin et al. and British Patent No. 992,378 to New disclose hose fittings having annular teeth for engaging a hose when the fittings are crimped onto the hose. In particular, both of these references disclose sleeves having either rectangular or trapezoidal teeth as the final teeth contacting the hose at the hose end of the coupling. These teeth have sharply defined edges; as the sleeve is crimped onto the hose, these sharp-edged projections embed into the hose covering. This ensures a good connection between the fitting and the hose.
[0006] FIG. 2 illustrates a cross-section for a prior art coupling 10 having a sleeve 3 swaged or crimped onto a hose 2 , and engaging both the hose and the insert 4 . The sleeve and insert are shown with sharp-edged or rectangular teeth. It has been found in some instances that when such hoses are put in use and pressurized, the hose fails at the hose end of the coupling in the general area designated by 11 . It is thought the hose fails because the hose in the area 11 experiences highly localized stress created by the last sharp-edged rectangular tooth or teeth on the hose end of the sleeve. It is believed the sharp edge of the last tooth is so effective in rigidly penetrating into the covering that a stress concentration occurs at that area when the hose balloons out under pressure. Large, penetrating, sharp-edged projections or teeth on the sleeve at the hose end of the coupling, therefore, are thought to contribute to the failure of such hoses. What is needed, therefore, is an improved hose coupling that better distributes the load over a number of the teeth.
BRIEF SUMMARY OF THE INVENTION
[0007] This invention relates to a hose coupling useful with a textile-reinforced hose, comprising a sleeve and an insert for the sleeve, the insert having a hose end for insertion into the hose and the sleeve having a hose end for covering the exterior of the hose and the insert, and the insert and sleeve each having a coupling end for engaging each other, and the sleeve having an interior surface for gripping the hose, the interior surface having:
[0008] i) distributed on the hose end, a plurality of grooves with at least one rounded annular tooth, and
[0009] ii) distributed on the coupling end, a plurality of grooves with rectangular annular teeth.
[0010] In another embodiment, the insert also has an exterior surface for gripping the hose, the exterior surface having:
[0011] i) distributed on the hose end, a plurality of grooves with at least one rounded annular tooth, and
[0012] ii) distributed on the coupling end, a plurality of grooves with rectangular annular teeth.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a perspective cut-away view of one prior art embodiment of an uncrimped hose coupling including a sleeve, an insert, and a hose.
[0014] FIG. 2 is a cross-section view of a prior art sleeve crimped onto a hose and insert.
[0015] FIG. 3A is one prior art hose coupling and FIG. 3B is one embodiment of the present invention of an improved hose coupling.
[0016] FIGS. 4A to 4F are various embodiments of possible combinations of various shapes, spacings, relative heights, and sizes of teeth and grooves on the surface of the sleeve and/or insert of the present invention.
[0017] FIGS. 5A to 5I are various embodiments of the present invention of possible rounded tooth shapes used on the sleeve and/or insert.
[0018] FIGS. 6 to 9 are some embodiments of the present invention of the hose couplings showing possible mechanical variations that can be used.
DETAILED DESCRIPTION OF THE INVENTION
[0019] This invention relates to an improved hose coupling that is useful with high pressure textile-reinforced hoses in the oil and gas industry, the sleeve of the coupling having at least one rounded annular tooth at the hose end of the coupling and rectangular annular teeth at the coupling end of the coupling. It is thought that rounded teeth help reduce localized stresses in the hose at the hose end of the coupling, while the rectangular teeth securely hold the hose at the coupling end of the coupling. Hoses that fail at the hose end of the coupling under the influence of a pressure impulse or loading, usually fail in the region of contact between the hose and the first rectangular tooth on the hose end of the sleeve. The incidence of failure can be reduced if the hose can gripped by the coupling sleeve in a graduated manner, such that the load is better spread over a number of the teeth.
[0020] As used herein, the teeth and grooves on the sleeve and insert are understood to be annular, that is they form projections in the case of teeth or indentations in the case of grooves that are continuous around or into the interior of the sleeve or the exterior of the insert. In a preferred embodiment, the annular surface of the sleeve and insert is round; however, non-round sleeves or inserts are thought to be useful. By “continuous around or into” it is meant the teeth or grooves either create (1) substantially continuous circumferential interior and/or exterior bands, which in the case of a round sleeve or insert are generally ring-shaped grooves and teeth; or (2) substantially continuous helical interior and/or exterior bands, which in the case of a round sleeve or insert are generally spiral-shaped grooves and teeth similar to the threads on a screw or bolt. If desired, the sleeve and the insert can have different types of continuous projections or indentions. Also, the individual sleeve and insert can have on its exterior or interior surface a combination of these two types of continuous projections or indentations if desired.
[0021] In some preferred embodiments the grooves and teeth are positioned orthogonal to the axis of the sleeve and insert. In other words, these grooves and teeth are non-helical, meaning at least two of the indentations or grooves, and likewise the teeth or projections, are not connected by being continuous around the periphery like the threads of a screw; that is, at least two of the teeth and/or two of the grooves are spaced apart and separated from one another. In some embodiments, the grooves and teeth can be helically arranged on the annular surface of either the sleeve or insert. In some embodiments, combinations of orthogonal and helical teeth and grooves can used.
[0022] FIG. 3A is an illustration of a typical prior art uncrimped hose coupling and FIG. 3B is an illustration of one embodiment of an uncrimped hose coupling of the present invention having both rounded and rectangular teeth and non-helical or orthogonal grooves. Prior art coupling 20 has a series of identical rectangular teeth 21 shown on both the sleeve and the insert. The illustration in FIG. 3B of one preferred embodiment shows a plurality of substantially uniformly-spaced, rounded annular teeth 22 on the interior surface of the sleeve at the hose end. The interior surface of the sleeve also grips the hose with a plurality of substantially uniformly-spaced, rectangular annular teeth 23 . The plurality of rounded and the plurality of rectangular teeth both form a plurality of non-helical annular grooves 24 between the teeth. In this illustration, the insert of the coupling also has plurality of substantially uniformly-spaced, non-helical annular grooves formed by rectangular annular teeth. As shown in this embodiment, the sleeve and the insert both have a plurality of rounded annular teeth. In addition, the exit shoulders 22 A on the sleeve and the insert are also rounded. In one preferred embodiment, any exit shoulder on the sleeve and/or insert on any of the possible embodiments is also rounded.
[0023] The arrangement of teeth on the sleeve and the insert as shown in FIG. 3B is only one embodiment and many combinations of teeth are possible. FIGS. 4A to 4F illustrate other possible tooth and groove embodiments in accordance with the present invention. As shown in FIG. 4A , a plurality of uniformly-spaced, same-height rounded teeth are shown at the hose end as represented by 25 and a plurality of uniformly-spaced, same-height rectangular teeth are shown at coupling end as represented by 26 . In FIG. 4B , the first two rounded teeth on the hose end 25 have different heights, while the next two have identical heights, and then two rectangular teeth on the coupling end 26 have the same height. While the figures illustrate a preferred embodiment wherein there is a plurality of rounded teeth on the hose end of the sleeve or the sleeve and insert, however, it is thought only one rounded tooth used as the last tooth of the sleeve or sleeve and insert is required. FIG. 4C illustrates the grooves between teeth of the present invention can be rounded or rectangular. FIG. 4D illustrates the set of rounded teeth of the present invention can be spaced apart from the rectangular teeth on the sleeve or sleeve and insert. FIG. 4E illustrates a combination of features can be used, including variable spacing of the teeth and/or grooves and different heights of both the rounded and rectangular teeth. As used herein, rectangular teeth are understood to be teeth having a sharp edge for projecting into the cover of a hose to grip the hose securely.
[0024] FIG. 4F illustrates one preferred embodiment for the combination of teeth on the sleeve or insert. This embodiment has a set of rectangular teeth at the coupling end, followed by a set of rounded teeth having rounded corners, with the radii of the rounded corners increasing as the teeth are positioned closer to the hose end, eventually becoming circular in cross-section. Further, the centerline height of each rounded tooth decreases as the position of the tooth gets closer to the hose end. Finally, this embodiment also illustrates an especially useful spacing or grooves between the teeth; this spacing is shown as being wider at the hose end, and gets progressively narrower toward the coupling end of the sleeve. Therefore, in some embodiments, the grooves and teeth are uniformly spaced, but if desired in some embodiments, the grooves and teeth have wider spacing at the hose end than at the coupling end.
[0025] The rounded teeth and grooves of the present invention can be in many different forms and combinations as represented in FIGS. 5A through 51 . As in FIGS. 5A to 5C , the rounded teeth can have flat grooves and be semi-circular in shape, be shaped from a portion of an arc of a circle, or have the shape of a projected semi-circular with straight sides. As shown in FIGS. 5D to 5F , the same shapes can be combined with rounded grooves. In addition, as shown in FIGS. 5G to 5I teeth having a flat top with rounded edges can also be used as rounded teeth. The flat top can be parallel to the annular axis of the sleeve as shown in FIG. 5G or can be at an angle to the axis as shown in FIG. 5H , as long as the sharp edges are rounded. By rounded edges for these flat top teeth, it is meant the teeth are provided with a circular radius 27 as shown in FIG. 5I that can be machined or otherwise created or formed on the teeth to avoid sharp edges. In some embodiments this radius is from one-tenth to one-third the width of the tooth. In one embodiment there is a plurality of rounded teeth, each tooth having a set of rounded edges, wherein the radius of the set of rounded edges on each tooth is progressively larger from the coupling end to the hose end.
[0026] FIG. 6 illustrates a coupling sleeve 3 of the present invention uncrimped on an insert 4 , and included in this illustration is the coupling device 5 , such as a hex-shaped threaded nut, used to attach the hose to another object. The type of coupling device is not critical and while all illustrations do not show such a coupling device, it should be understood that the purpose of the hose coupling, comprising the sleeve and insert, is to attach the hose to something and therefore some type of coupling device can be and will normally be attached to the coupling end of the hose coupling. In some instances, the coupling device could be another hose coupling.
[0027] The embodiment of FIG. 6 illustrates a set of annular teeth and grooves 30 on the interior of the sleeve and a set of annular teeth and grooves 33 on the exterior of the insert. The last tooth 31 on the hose end of the sleeve is shown slightly rounded, as is the adjacent shoulder of the sleeve, while the last tooth 32 on the coupling end of the sleeve is shown as rectangular.
[0028] As shown in the hose coupling FIGS. 6 to 9 of the present invention, a plurality of rectangular teeth is shown at the coupling end, followed by a number of teeth having either round shape or other rounded teeth having a pseudo-rectangular shape with rounded corners at the hose end. While not to imply any particular method of generating either the sleeve or the insert, due to the ease at which parts can be machined, if desired, after at least two rectangular teeth are present at the coupling end of the sleeve, the remaining teeth on the sleeve can be machined to have rounded corners with the radius of those corners being progressively larger as the teeth are machined toward the hose end. If desired the entire tooth can have a semi-circular shape, or the tooth can have a portion of an arc of a circle, especially the final teeth at the hose end.
[0029] FIG. 7 illustrates an embodiment wherein the sleeve has a set of teeth 35 having different heights. Also, if desired, the insert can have a set of teeth 36 having different heights. In this embodiment, the teeth vary from slightly rounded to rectangular as in FIG. 6 , however, the height of the teeth increase as the roundness of the teeth decrease. As shown in this illustration, the wall thickness of the sleeve, as defined as the thickness of the wall in the groove, does not substantially vary from the coupling end to the hose end of either the sleeve or the insert.
[0030] FIG. 8 illustrates an embodiment wherein the sleeve has a set of teeth 45 wherein the inside radius from the centerline of the coupling to the annular tooth surface increases from the coupling end to the hose end. Dotted line 47 illustrates the angle formed by the increasing radii of the teeth. Also in this embodiment, the centerline height of individual teeth on the sleeve can be the same, and the wall thickness as defined by the thickness in the groove increases from a thick wall thickness at groove 42 to a thin wall thickness at groove 43 . If desired, the coupling can include on the insert a similar set of teeth 46 that have an outside radius from the centerline of the coupling to the annular tooth surface that decreases from the coupling end to the hose end. Dotted line 44 illustrates the angle formed by the decreasing radii of the teeth. As with the sleeve, the centerline height of individual teeth on the insert can be the same, and the wall thickness as defined by the thickness in the groove increases from a thick wall thickness at groove 40 to a thin wall thickness at groove 41 .
[0031] FIG. 9 illustrates an embodiment combining a substantially constant wall thickness, as defined by the thickness of the groove, with the variation in radius as described for FIG. 6 . The set of teeth 50 for the sleeve is shown again with dotted line 52 illustrating the angle formed by the increasing radii of the annular teeth on the sleeve. If desired the insert can have a set of teeth 51 that have an outside radius from the centerline of the coupling to the annular tooth surface that decreases from the coupling end to the hose end. Dotted line 53 illustrates the angle formed by the decreasing radii of the teeth. As with the sleeve, the centerline height of individual teeth on the insert decreases from the coupling end to the hose end and the wall thickness as defined by the thickness of the wall of the sleeve or insert in the groove remains substantially constant from the hose end to the coupling end.
[0032] As shown in the above illustrations, in some embodiments of the present invention the wall thickness of the hose end of the sleeve is smaller than at the coupling end, the wall thickness being defined as the thickness of the wall in the groove. In some embodiments of the invention, there is a plurality of rounded annular teeth and the centerline height of all the rounded annular teeth is the same. In some other embodiments of the invention, the centerline height of all the rectangular annular teeth is the same. In some other embodiments of the invention, the centerline height of the each of the annular teeth varies linearly from the coupling end to the hose end. In some other embodiments of the invention, the height of the teeth vary gradually and continuously in something other than a linear variation, such as a logarithmic or parabolic variation. In some preferred embodiments of the invention, the centerline height of each tooth decreases from the coupling end to the hose end. In particular, the centerline heights of the rounded annular teeth at the hose end are smaller than the centerline heights of the rectangular annular teeth at the coupling end. These embodiments can apply equally to the sleeve or the insert.
[0033] While the above are useful, other embodiments and combinations of features can be used to form suitable hose couplings. The hose coupling is especially useful with textile reinforced hoses, but the hose coupling can also be used with other hoses such as those having other types of layered reinforcement, such as metal reinforcement; or hoses having limited or no reinforcing layers. In some embodiments such hoses include a thermoplastic covering, a section of textile reinforcement, and a liner. In others, the hose can simply be thermoplastic or elastomeric.
[0034] Suitable materials useful as covers for the hoses include thermoplastic and/or elastomeric materials or various combinations thereof. Suitable materials useful as liners for the hoses include thermoplastic, elastomeric, and/or fluoropolymer or various combinations thereof. While these materials are especially typical of hoses, essentially any material useful for a hose can be used.
[0035] The textile reinforcement can include fiber or yarn that is braided, or the fiber or yarn can be spirally or helically oriented in the hose. The textile reinforcement can also be wound fiber tapes. The preferred textile reinforcement includes aramid fiber, and most preferred aramid is poly(paraphenylene terephthalamide). Other types of fibers and yarns, such as polyamides, polyesters, glass fiber, carbon fiber, ceramic fiber, and other high strength aramids, polyazoles, extended chain polyetheylenes, and liquid crystal polyesters, or mixtures of any of these materials could also be used if desired.
|
This invention relates to an improved umbilical hose end coupling that is useful with textile-reinforced hoses in the oil and gas industry, especially high pressure hoses for use in offshore systems. This hose coupling comprises a sleeve and an insert for the sleeve, the insert having a hose end for insertion into the hose and the sleeve having a hose end for covering the exterior of the hose and the insert, and the insert and sleeve each having a coupling end for engaging each other, and the sleeve having an interior surface for gripping the hose, the interior surface having
i) distributed on the hose end, a plurality of grooves with at least one rounded annular tooth, and ii) distributed on the coupling end, a plurality of grooves with rectangular annular teeth.
| 5
|
BACKGROUND OF INVENTION
Field of Invention
The present invention relates to the field of aerospace turbomachines and, more particularly, that of pressurizing the internal chambers of such turbomachines.
Description of Related Art
Modern turbomachines generally take the form of an assembly of modules comprising either moving parts or stationary parts. Starting from the upstream end, they first of all comprise one or more compressor modules, arranged in series, which compress air sucked into an air intake. The air is then passed into a combustion chamber where it is mixed with fuel and burned. The combustion gases pass through one or more turbine modules which drive the one or more compressors. The gases are finally ejected either through a nozzle to provide a propulsive force or through a free turbine to provide power on a transmission shaft.
The rotating parts, such as the one or more rotating shafts, the one or more compressors and the one or more turbines, are carried by structural parts by means of bearings which are enclosed in chambers allowing the bearings to be lubricated and cooled. Turbomachines generally comprise two lubrication chambers, one located in the forward region which encloses the compressor-side bearings and one located in the rear region which encloses the turbine-side bearings. These chambers consist of a collection of moving and stationary walls, between which are arranged labyrinth-type devices in order to ensure the necessary sealing therebetween.
The stationary part of the forward chamber is made up of elements of a structural part termed the intermediate frame, while the rear chamber is made up of elements of a second structural part termed the exhaust frame. Examples of such chambers are represented in FIGS. 1 and 2 . These structural parts support the bearings which in turn support the moving parts of the turbomachine.
In order to ensure that the oil is maintained inside the lubrication chambers, these are generally kept at a higher pressure than the surrounding spaces. To this end, pressurized air is injected into these chambers through orifices designed for this purpose. At the outlet of the chamber, an air/oil mixture is collected, the constituents of which are then separated by an oil separator-type device so that the oil can be sent to the ad hoc reservoir and the pressurization air can be vented to the outside.
In the prior art, the air for pressurizing the chambers is bled from downstream of a compressor stage, generally downstream of the low-pressure (LP) compressor. In existing engines, this pressure is sufficiently high to achieve the desired overpressure, without the air bled therefrom being at too high a temperature. In modern engines, where compression ratios in the compressors are ever higher, the temperature of the air leaving the LP compressor is relatively high. It follows that the temperature of the air entering the second chamber is too high, due to the heat energy imparted to it during its passage through the engine, this path taking it alongside the hot parts of the engine. It would then not be able to carry out its task of cooling the oil of the chamber, the temperature of which could then exceed 200° C. in certain working phases, which is not within acceptable limits.
One possible solution might be to bleed air further upstream than the exit from the LP compressor, but the pressure of the air bled would then not be high enough, especially at low engine speeds and when running on the ground, to adequately supply the chambers. There would then be the risk of inadequate air flow rate, or even of the air for cooling the chambers reversing its flow direction.
Another solution might be to fit an additional heat exchanger of the air/oil or air/fuel type and/or a return line for returning the fuel to the tank in order to increase the oil flow rate, and thus its cooling potential, at low engine speeds. However, such solutions are complicated to implement and give rise to additional weight.
BRIEF SUMMARY OF INVENTION
The aim of the present invention is to solve these drawbacks by proposing a system for pressurizing the air for cooling the chambers for lubricating the bearings of modern turbomachines, said system not having some of the drawbacks of the prior art and, in particular, ensuring effective circulation of the air for conditioning the chambers under all operating conditions of the turbomachine.
To this end, the invention relates to a system for pressurizing at least one chamber for lubricating the bearings of a turbomachine, comprising a circuit for supplying said chamber with pressurized air, and a circuit for recovering the oil mist formed in the chamber and for returning this mist to the oil reservoir of the turbomachine. It is characterized in that the supply circuit supplies said chamber with air bled from upstream of the low-pressure compressor. Choosing suction by air bled from upstream of the LP compressor, i.e. directly from the air intake of the engine, makes it possible to work with the coldest possible air and thus to avoid the air having an already raised temperature before it is circulated in the chambers to be lubricated and cooled.
Preferably, the supply circuit is supplied both with air bled from upstream of the compressor and with air bled from downstream of a compressor stage, the latter air being returned to the pressure of the air bled from upstream of the compressor by being passed through a labyrinth.
This ensures an adequate flow rate for cooling the chambers. The air bled from downstream of a compressor is returned to the pressure of the air from the air intake by passing it through labyrinths which cause its pressure to drop.
In a preferred embodiment, the recovery circuit comprises, downstream of said chamber, means for suction of said mist. This device makes it possible to cause the cooling air to flow even at low speeds or on the ground, where the pressure in the air intake would be insufficient to ensure this flow.
Advantageously, said suction means is arranged downstream of an oil separator for separating the air and oil forming said mist, such that the suction acts on oil-free air.
This configuration has the advantage of simplicity, as the air removed by suction can then be vented directly to the outside.
Preferably, said suction means is fitted to the oil reservoir. All the functions of oil separation and venting of the pressurization air are then gathered in a single location.
In one particular embodiment, the suction means comprises a jet pump.
Such a device is simple to implement thanks to the free availability of pressurized air which can be bled from the flow of the turbomachine.
Advantageously, the jet pump is supplied with air bled from a stage of a compressor.
In one particular embodiment, the circuit for supplying air to the jet pump comprises a valve for regulating the supply pressure of said jet pump.
This device makes it possible to regulate the level of suction of the jet pump and therefore the pressure drop to which the recovery circuit for the oil-free air is subjected.
Advantageously, said regulating valve is actuated in dependence on the difference in pressure between the interior and the exterior of the oil reservoir. This makes it possible to ensure the integrity of the oil reservoir and to avoid it collapsing under too great a pressure difference.
Preferably, the pressurization system comprises a control module which switches off the suction when the turbomachine exceeds a predefined rotational speed.
As the need for suction appears only at low engine speeds, a module of this type makes it possible to avoid unnecessary bleeding of air when the turbomachine is required to deliver power.
The invention also relates to a turbomachine comprising at least one chamber for lubricating at least one of its bearings, characterized in that it comprises a pressurizing system as described hereinabove for supplying said chamber with pressurized air.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The invention will be better understood, and other aims, details, features and advantages of the invention will appear more clearly, in the course of the detailed explanatory description which follows, of an embodiment of the invention which is given as a purely illustrative and non-limiting example, with reference to the attached schematic drawings, in which:
FIG. 1 is a view in section of a turbomachine, at the level of its forward chamber;
FIG. 2 is a view in section of a turbomachine, at the level of its rear chamber;
FIG. 3 is a schematic view of a system for lubricating and pressurizing the chambers of a turbomachine, according to one embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows the forward portion of a turbomachine comprising a LP compressor 1 and the first stage of a high-pressure (HP) compressor 2 . The LP compressor 1 is carried by a low-pressure shaft 3 which rotates on a forward LP bearing 4 fitted with a rolling-contact thrust bearing and on a rear LP bearing 5 (visible in FIG. 2 ) fitted with a roller bearing. The HP compressor is, for its part, carried by a high-pressure shaft 6 which rotates on a forward HP bearing 7 fitted with a rolling-contact thrust bearing and on a rear HP bearing (not shown). The forward LP and HP bearings are held in place by flanges 8 a and 8 b of the intermediate frame 9 . The flanges 8 a and 8 b form with the LP shaft 3 a cavity 10 , creating the chamber for cooling and lubricating the various bearings of the forward portion of the engine. Sealing between the stationary flanges 8 a and 8 b and the LP rotor 3 is ensured by labyrinths 11 a and 11 b which close off the forward chamber 10 .
The figure shows the direction of flow of the air for pressurizing the forward chamber 10 , with primary bleeding of air through the front cone of the turbomachine, such that the air bled therefrom is at a relatively low temperature as it has not been compressed. This air comes from the air intake duct of the engine and enters the front cone through an orifice (not shown) which may be located either at the tip of the cone or on the surface thereof. It then passes from the front cone to the forward chamber 10 by means of openings made in the high-pressure and low-pressure rotors.
Complementary air is bled from downstream of the LP compressor 1 , at the exit from the final stage of this compressor, and at the entrance to the HP compressor 2 in order to ensure adequate flow rate. This air, which enters the forward chamber 10 through the labyrinths 11 a and 11 b , is returned to a pressure close to that of the air from the cone by means of the efficiency of these labyrinths being regulated. As the air coming from the cone enters the chamber 10 downstream of the labyrinths 11 a and 11 b , it is possible to ensure that the pressures of these two air inlets are similar, such that the risk of flow reversal is avoided.
When circulating in the chamber 10 , the pressurization air becomes laden with oil, and the mist thus formed is recovered in the lower part of the chamber in order to be passed into an oil separator 12 where the air and oil are separated.
Similarly, on the downstream side of the engine as shown in FIG. 2 , a rear pressurization chamber 20 , which encloses the bearings carrying the rotating shafts 3 and 6 , is bounded on one hand by a flange 18 and by stationary partitions carried by the exhaust frame 19 and, on the other hand, by moving partitions connected to the rotating parts. Labyrinths 21 a , 21 b and 21 c provide sealing between the stationary parts and the rotating parts. The pressurization air, coming from the front cone via the interior of the high-pressure and low-pressure rotating shafts, enters the chamber 20 through orifices made for this purpose in the one or more rotating shafts of the engine, where it becomes laden with oil to form a lubricating mist, and exits therefrom through an oil separator 22 which separates the oil from the air and returns the recovered oil to the general oil reservoir for the turbomachine.
With reference now to FIG. 3 , there follows a description of the diagram of a device for lubricating and pressurizing the forward chamber 10 and rear chamber 20 in one embodiment according to the invention. The oil circuit comprises, in the conventional way, a reservoir 30 containing oil which is held, by means of known heat exchanger systems, at a temperature which is low enough to make cooling of the various bearings of the engine possible. The circuit comprises an oil circulation pump 31 and conduits 32 , 32 a and 32 b for conveying the oil into the forward chamber 10 and rear chamber 20 , respectively, where the oil is injected onto the parts to be cooled by means of nozzles (not shown). Recovery conduits, 33 a and 33 b respectively, recover the oil mist as it leaves the forward chamber 10 and rear chamber 20 . The mist recovered from the two chambers empties into the reservoir 30 which comprises an oil separator 12 (in the configuration of FIG. 3 , the two oil separators 12 and 22 of FIGS. 1 and 2 are as one).
The oil separator removes the oil from the mist; the oil falls back into the reservoir while the air is expelled from this same reservoir. The expulsion of the air is facilitated by a pressure drop generated by means of a jet pump 35 which works on the principle of a Venturi tube: pressurized air is bled from the exit of a compressor stage by a conduit 36 and is sent through a nozzle 37 to generate a pressure drop at the exit from the oil separator 12 . A regulating valve 38 is positioned on the conduit 36 supplying air to the jet pump 35 so as to regulate the pressure drop in the Venturi tube and thus control the pressure difference between the interior and exterior of the oil reservoir, in order to ensure its integrity.
The air used for the operation of the Venturi tube, which flows through the conduit 36 , is bled from the exit of a compressor stage so as to have a pressure which is above that of the air from the intake duct. The temperature of this air, which is therefore above that of the pressurization air, has no effect on the cooling of the various bearings as it does not flow through the chambers 10 and 20 .
There follows a description of the operation of the circuit for pressurizing the forward and rear chambers by means of a device according to the invention, as represented in FIG. 3 .
The air for pressurizing the chambers is bled at a relatively low pressure in order for the temperature of said air not to be too high, because if it were, it would not be able to effectively cool the various bearings of the rear chamber 20 . This air becomes laden with oil in the two chambers and the mist thus formed is recovered at the exit by recovery conduits 33 a and 33 b which convey it into the oil reservoir 30 .
The oil separator 12 separates the oil, which falls back into the reservoir 30 , from the pressurization air which is removed by suction by the jet pump 35 and expelled outside the engine. Circulation of the pressurization air is thus ensured, both by the pressure generated in the intake duct and by a pressure drop at the exit, generated by the suction of the jet pump 35 . It is thus no longer necessary to choose air which has been pressurized by one or more compressor stages—which would cause the temperature of the air entering the chambers to rise above acceptable levels—in order to ensure, under all operating conditions, circulation in the chambers of the air for pressurizing and cooling. The turbomachine designer is therefore free to choose the pressure of the air supplied to the Venturi tube. As the pressurization air is bled at a pressure that is still relatively low, the temperature of this air is not too high, which solves the technical problem addressed by the invention.
In the embodiment represented, the jet pump 35 is attached to the oil reservoir, which offers the advantage of providing suction for the pressurization air downstream of the oil separator, so that the suction acts on oil-free air.
The presence of the regulating valve 38 is intended to regulate the pressure drop generated in the jet pump 35 and, consequently, to control the pressure difference between the interior and the exterior of the oil reservoir. The presence of the valve makes it possible to ensure that the pressure drop generated inside the reservoir by the jet pump will not exceed the structural limits of the reservoir, which will then not collapse under the surrounding pressure.
Finally, a control device can be assigned to this valve, which control device switches the jet pump on or off according to the operating conditions of the turbomachine. As the need to generate suction at the exit of the pressurization circuit arises only when on the ground or at low engine speeds in flight, a suitable control module makes it possible to close the regulating valve 38 once a predetermined engine speed is reached. By closing the air supply conduit 36 , air is no longer bled from the compressor, as so-doing becomes irrelevant at high engine speeds precisely at the time when the pilot requires more power from the engine.
The system has been described with a jet pump 35 situated at the exit from the oil separator 12 , but it is obvious that this jet pump could be replaced by any device which generates suction of the air at the exit from the forward chamber 10 and rear chamber 20 , and which would therefore permit the choice of a less marked overpressure at the entrance to the pressurization circuit.
|
A system for pressurizing at least one chamber for lubricating bearings of a turbine engine, including a circuit for supplying the chamber with pressurized air, and a circuit for recovering oil mist formed in the chamber and for returning the mist to an oil tank of the turbine engine. The supply circuit supplies the chamber with air taken upstream from the low-pressure compressor.
| 5
|
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. provisional application No. 61/583,432, filed Jan. 5, 2012, which is incorporated herein by reference as if fully set forth.
FIELD OF INVENTION
[0002] The subject matter described herein relates to advanced dynamic interaction between consumer and packaged food.
BACKGROUND
[0003] The profitability of food retailers, such as groceries or supermarkets, and Consumer Packaged Goods (CPG) producers can be adversely affected by high commodity prices, transportation costs, high labor costs, in store waste and the high cost of advertising and product development. Retailers need to optimize use of their layout and display space in ways that integrate consumer understanding of shopping patterns, decision patterns, impact of number of SKUs on the decision to visit a store, and an aisle of location within that store. CPG producers, which control product definition need to optimize brand and marketing experiences that include consumer understanding of the frequency and type of consumer communications. They are doing this within the confines of Government regulations on labeling. Such consumer understanding is costly to obtain and is often incomplete. Typically, the data collection through which consumer habit analysis is extrapolated is done at the point of sale. Influencing consumers though couponing is typically done on a post-purchase basis, either at the point of sale and/or at home before new purchasing activities are started. Neither of these are highly targeted and aligned to individual consumer preferences, and thereby suffer from low redemption rates and low impact, while at the same time increasing costs due to over-distribution. Coupons are typically distributed to a broad audience to find a limited interest audience.
[0004] Such data collection is widespread and fails to provide specific insights as to a consumer's behavior, namely the reasons a consumer chooses a particular product for purchase. Today, retailers do not have a system with the ability to gain consumer insights nor influence purchase at either the point of purchase decision or the point of use decision. The only known method of gaining a consumer's insight at the point of purchase decision is by hiring one or more persons skilled and trained at conducting focus group testing to follow the consumer in their retail store. This is costly in both time and personnel resources, and may be uncomfortable to individual consumers.
[0005] As one of their principal expenditures consumers are increasingly sensitive and conscious of cost inflation in their monthly food bills. Yet, time pressures in modern lifestyles limit the time consumers can allocate to searching and cutting out coupons or other saving mechanisms typically offered by retailers and CPGs. Therefore, consumers need a means to optimize their shopping time and food costs, while increasing the relevance of their purchases to minimize redundant purchases while insuring that all ingredients necessary for menu planning are in the household pantry.
[0006] Retailers currently use elaborate in-store presentations on aisles, end caps, shopping carts and shelves to seize the consumer's attention and influence product selections before, during, and after a consumer's product consideration. These non-targeted, non-customizable attempts to influence consumers are often disregarded by the consumer, whose objective is to get out of the store as fast as possible, completing the task of shopping while talking on their cell phone or interacting with media on other personal handheld devices, such as smartphones. Prior attempts to deal with consumer disregard of retailer presentations have involved methods that proved to be expensive, inefficient, ineffective and annoying.
[0007] Food industry suppliers need low-cost, highly effective methods for responding to and influencing a consumer's product selection and decision-making at home and in stores. Such methods should aim to enhance, simplify and expedite a consumer's experience on a cost-neutral (and time-neutral) basis to consumers and a cost-neutral to positive impact to retailer profit margins. Retailers are interested in maximizing profitability by moving consumers to higher margin products or in-store brands. Implementations vary whether the retailer uses an Every Day Low Pricing (EDLP) strategy or a Promotional (HiLo) strategy. This has typically been done through broad store brand promotions. Due to their lack of specific consumer targeting, these may achieve market share objectives at the expense of profitability. Moreover, such broad promotions may also adversely impact relationships with certain CPG manufacturers (whether they are supplying the store brand or not). Another method is changing store configuration between center of store and side of the store, which is costly due to its labor intensity, and disruptive to the store, and the shopper.
[0008] To address these issues, attempts have been made to tie marketing messages to the item being purchased by the consumer, while that item is in the hand of the consumer or the shopping cart. These initial attempts, because they were developed before smart phones supporting GPS, high-speed communication and fast processing chip were readily available, have suffered from major limitations.
[0009] In U.S. Pat. No. 7,225,979, Silverbrook et al. teaches interaction between objects and consumers based on coded data printed on the document being examined. The inventors teach limited interactivity where the co-location of a sensing device (an electronic pen) against the package triggers the extraction of non-interactive information from the web. The invention does not consider or anticipate the case where the sensing device has memory allocated to store and dynamically process interactions that can vary based on considerations such as historical purchase information, stored or retrieved preferences, alternative purchase possibilities and other relationships between the product being considered for purchase and the consumer owner or user of the device.
[0010] Knowles in U.S. Pat. No. 5,905,251, and Wilz and Knowles in U.S. Pat. No. 6,464,139 teach another limited example of an interactive packaging application. There, a hand held scanner is used to extract an encoded applet visually encoded in the form of a bar code. QR codes were not yet popularized when the invention was developed in the former and a URL in the later. These narrow inventions do not consider the utilization of information, if any, that may be stored in the scanner, other than a transient basis to alter the consumer experience, nor do they allow or direct themselves in any way to customization of the consumer shopping experience.
SUMMARY
[0011] In an aspect, the invention relates to a computer-implemented method. The method includes providing a first set of instructions configured to cause a portable device to: i) scan all or a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into at least one index, iv) access one or more extraction attributes; identifying one or more digital objects based on the at least one index and the one or more extraction attributes; and presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects.
[0012] In an aspect, the invention relates to a computer-implemented method. The method includes providing a first set of instructions configured to cause a portable device to: i) scan all or a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into at least one index, iv) access one or more extraction attributes, and v) send the at least one index and the one or more extraction attributes to a server; receiving, at the server, from the portable device, a first request comprising the at least one index and the one or more extraction attributes; identifying one or more digital objects by the server, based on the at least one index and the one or more extraction attributes; sending to the portable device a second set of instructions by the server in response to the first request, configured to cause the portable device to: i) present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) send information identifying the particular digital object to a server upon a consumer selecting the control; and iii) send to the server, from the portable device, a second request identifying the particular digital object.
[0013] In an aspect, the invention relates to a computer-implemented method. The method includes providing a first set of instructions configured to cause a first portable device to: i) scan a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into an index, and iv) access one or more of a first set of extraction attributes; transmitting the index and the first set of extraction attributes to a second portable device; accessing one or more of a second set of extraction attributes; sending the index and the first or second set of extraction attributes to a server by the second portable device; receiving, at the server, from the second portable device, a first request comprising the index and said attributes; identifying one or more digital objects by the server based on the index and said attributes; sending a second set of instructions to the second portable device by the server, in response to the first request, configured to cause the second portable device to: i) present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects, ii) send information identifying the particular digital object to a server upon a consumer selecting the control, and iii) send to the server, from the second portable device, a second request identifying the particular digital object.
[0014] In an aspect, the invention relates to a non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, perform actions including: scanning a portion of packaging; locating a visual indicator in the visible portion of packaging; mapping said visual indicator into at least one index; accessing one or more context attributes; presenting an interactive interface comprising information about one or more digital objects; presenting to a consumer a control for selecting a particular digital object of the one or more digital objects; and sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0015] In an aspect, the invention relates to a non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including: providing a first set of instructions configured to cause a portable device to: i) scan all or a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into at least one index, iv) access one or more extraction attributes; identifying one or more digital attributes based on the at least one index and the one or more extraction attributes; presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; and storing use of the particular digital object into non-volatile memory upon a consumer selecting the control.
[0016] In an aspect, the invention relates to a non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including: providing a first set of instructions configured to cause a portable device to: i) scan all or a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into at least one index, iv) access one or more extraction attributes; identifying one or more digital objects based on the at least one index and the one or more extraction attributes; presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; and sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0017] In an aspect, the invention relates to an interactive packaging processing system comprising: one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory, and a user interface; the one or more portable devices capable of extracting one or more extraction attributes; at least one of the one or more portable devices capable of selecting one or more digital objects based on information from scanning the packages and the one or more attributes and presenting the one or more digital objects to the portable device user interface.
[0018] In an aspect, the invention relates to an interactive packaging processing system comprising: one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory and user interface and said portable devices capable of extracting one or more extraction attributes; one or more servers comprising one or more digital objects stores, a central processing unit and memory, said one or more digital objects stores storing one or more digital objects; at least one portable device capable of scanning a package, extracting a first of set of one or more of said attributes and transmitting information about scanned package; at least a second portable device capable of extracting a second set of one or more of said attributes; said at least one portable device capable of exchanging said first set of attributes to a second device; said portable devices capable of transmitting first set of attributes, second set of attributes and information about scanned package to one or more servers, said one or more servers capable of selecting one or more digital objects based on scanned package information and attributes, and said servers capable of transmitting one or more digital objects to one or more portable devices.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The following detailed description of the preferred embodiments of the present invention will be better understood when read in conjunction with the appended drawings. For the purpose of illustrating the invention, there are shown in the drawings particular embodiments. It is understood, however, that the invention is not limited to the precise arrangements and instrumentalities shown. In the drawings:
[0020] FIG. 1 illustrates components of a basic system which includes scanning of a food item(s) performed by a consumer holding an extracting device or using a device holding said device.
[0021] FIG. 2 illustrates how an extracting device ( 201 ) may be architected to enable context aware interaction with packaging.
[0022] FIG. 3 illustrates a system that supports context aware interaction with packaging.
[0023] FIG. 4 illustrates the structure of some of the key databases used in the supplier servers described in FIG. 3 above.
[0024] FIG. 5 illustrates the logic and flow of digital objects used to provide context aware interaction to consumers.
[0025] FIG. 6 illustrates how the context of a consumer interaction can be computed.
[0026] FIG. 7 illustrates nominal examples of the evolution of contexts for both store ( 701 ) and home ( 702 ) scanning scenarios.
[0027] FIG. 8 illustrates the scanning of a specific food item used to display multiple media objects on multiple phones, and methods of facilitating a group purchase of said items.
[0028] FIG. 9 illustrates another embodiment including enabling customized and dynamic pricing as well as real-time price bidding.
[0029] FIG. 10 illustrates another embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0030] Certain terminology is used in the following description for convenience only and is not limiting. The words “right,” “left,” “top,” and “bottom” designate directions in the drawings to which reference is made. The terms “memory” and “memory device” are used interchangeably. The terms “Stock Keeping Unit”, “SKU” and “item” are used interchangeably. The terms “state” and “context” are used interchangeably. The words “a” and “one,” as used in the claims and in the corresponding portions of the specification, are defined as including one or more of the referenced item unless specifically stated otherwise. This terminology includes the words above specifically mentioned, derivatives thereof, and words of similar import. The phrase “at least one” followed by a list of two or more items, such as “A, B, or C,” means any individual one of A, B or C as well as any combination thereof.
[0031] Described herein are methods and apparatus for the creation and use of dynamic individualized interactions between consumers and packaging while at home or shopping, enabling among others dynamic and/or context sensitive pricing, real time bidding for the consumer business, and consumer/context tailored information, or referrals.
[0032] Embodiments include computer implemented methods. In an embodiment, the method includes providing a first set of instructions configured to cause a portable device to scan all or a portion of packaging, locate a visual indicator in the visible portion of packaging, map said visual indicator into at least one index, and access one or more extraction attributes. The one or more attraction attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters. The method may also include identifying one or more digital objects based on the at least one index and the one or more extraction attributes and presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects. The step of identifying may also include transmitting the at least one index and the one or more attraction attributes to a second portable device. The second portable device may access the at least one index and the one or more extraction attributes and the second portable device may identify one or more digital objects based on the at least one index and the one or more extraction attributes. Alternatively, the step of identifying may include transmitting the at least one index and the one or more extraction attributes to a second portable device, accessing a second set of one or more extraction attributes by the second portable device, and identifying one or more digital objects based on the at least one index, the one or more extraction attributes, and the second set of one or more extraction attributes by the second portable device. The extraction attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters. The method may include sending at least one of the one or more digital objects to a third portable device.
[0033] The method may include storing use of the particular digital object into non-volatile memory upon a user selecting the control. The method may include sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0034] The one or more digital objects may include but are not limited to a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information. The financial instrument may include a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
[0035] Selecting the particular digital object may be based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, preferences or restrictions.
[0036] The method may further include creating a second index to the particular digital object, generating one or more unique transaction identifiers based on that second index, and transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0037] In an embodiment, a computer-implemented method includes providing a first set of instructions configured to cause a portable device to scan all or a portion of packaging, locate a visual indicator in the visible portion of packaging, map said visual indicator into at least one index, access one or more extraction attributes, and send the at least one index and the one or more extraction attributes to a server. The extraction attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters.
[0038] The method may also include receiving, at the server, from the portable device, a first request comprising the at least one index and the one or more extraction attributes, identifying one or more digital objects by the server, based on the at least one index and the one or more extraction attributes, and sending to the portable device a second set of instructions by the server in response to the first request, configured to cause the portable device to present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects, send information identifying the particular digital object to a server upon a consumer selecting the control, and receive at the server, from the portable device, a second request identifying the particular digital object.
[0039] The step of identifying may include querying a second server based on at least one of a context attribute, and identifying the one or more digital objects based on the context attribute from the second server, the at least one index and the one or more extraction attributes.
[0040] The method may include sending at least one of the one or more digital objects to a second portable device. The one or more digital objects may include at least one of a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information. The financial instrument may include a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
[0041] Selecting the particular digital objects may be based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, preferences or restrictions.
[0042] The method may include creating a second index to the particular digital object, generating one or more unique transaction identifiers based on that second index, and transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0043] In an embodiment, the computer-implemented method may include providing a first set of instructions configured to cause a first portable device to scan a portion of packaging, map said visual indicator into an index, and access one or more of a first set of extraction attributes. The extraction attributes may include location, speed, time, velocity, orientation, sound, lighting, distance to packaging, portable device parameters, application parameters, and identification parameters.
[0044] The method may also include transmitting the index and the first set of extraction attributes to a second portable device, accessing one or more of a second set of extraction attributes by the second portable device, sending the index and the first or second set of extraction attributes to a server by the second portable device, receiving, at the server, from the second portable device, a first request comprising the index and said attributes, identifying one or more digital objects by the server based on the index and said attributes, sending a second set of instructions to the second portable device by the server, in response to the first request, configured to cause the second portable device to present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects, send information identifying the particular digital object to a server upon a consumer selecting the control, and receive at the server, from the second portable device, a second request identifying the particular digital object.
[0045] The second set of extraction attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters.
[0046] The method may include sending at least one of the one or more digital objects to a second portable device. The one or more digital objects may include a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information. The financial instrument may include a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
[0000] Selecting the particular digital objects may be based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, preferences or restrictions.
[0047] The method may also include creating a second index to the particular digital object, generating one or more unique transaction identifiers based on that second index, and transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0048] Embodiments include a non-transitory machine-readable storage medium. The non-transitory machine-readable storage medium may include recorded and stored instructions thereon that, when executed, perform actions including scanning a portion of packaging, locating a visual indicator in the visible portion of packaging. mapping said visual indicator into at least one index, accessing one or more context attributes, presenting an interactive interface comprising information about one or more digital objects, presenting to a consumer a control for selecting a particular digital object of the one or more digital objects, and sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0049] The one or more context attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters.
[0050] The non-transitory machine-readable storage medium may also include sending the index and one or more extraction attributes to a server, and receiving a set of instructions, prior to presenting an interactive interface comprising information about one or more digital objects.
[0000] Embodiments include a non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including providing a first set of instructions configured to cause a portable device to scan all or a portion of packaging, locate a visual indicator in the visible portion of packaging, map said visual indicator into at least one index, access one or more extraction attributes, identifying one or more digital attributes based on the at least one index and the one or more extraction attributes, presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects, and storing use of the particular digital object into non-volatile memory upon a consumer selecting the control.
[0051] The extraction attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters.
[0052] Embodiments include a non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including providing a first set of instructions configured to cause a portable device to scan all or a portion of packaging, locate a visual indicator in the visible portion of packaging, map said visual indicator into at least one index, access one or more extraction attributes, identifying one or more digital objects based on the at least one index and the one or more extraction attributes, presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects, and sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0053] Embodiments include an interactive packaging processing system. The interactive packaging processing system may include one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory, and a user interface, the one or more portable devices capable of extracting one or more attributes at least one of the one or more portable devices capable of selecting one or more digital objects based on information from scanning the packages and the one or more attributes and presenting the one or more digital objects to the portable device user interface.
[0054] The one or more attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters.
[0055] Embodiments include an interactive packaging processing system. The interactive packaging processing system may include one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory and user interface and said portable devices capable of extracting one or more attributes, one or more servers comprising one or more digital objects stores, a central processing unit and memory, said one or more digital objects stores storing one or more digital objects, at least one portable device capable of scanning a package, extracting a first of set of one or more of said attributes and transmitting information about scanned package, at least a second portable device capable of extracting a second set of one or more of said attributes, said at least one portable device capable of exchanging said first set of attributes to a second device, said portable devices capable of transmitting first set of attributes, second set of attributes and information about scanned package to one or more servers, said one or more servers capable of selecting one or more digital objects based on scanned package information and attributes, and said servers capable of transmitting one or more digital objects to one or more portable devices.
[0056] The attributes may include location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, and identification parameters;
[0057] Referring to FIG. 1 , components of a basic system which includes scanning of a food item(s) performed by a consumer holding an extracting device or using a device holding said device is illustrated. The extracting device may include but is not limited to a cell phone, an infrared scanner, a tablet, RFID reader, a RFID enabled or Near-Field Communication (NFC) enabled device or a similar portable device with access to internet sourced information. The extracting device can of course be multi-functional. The device holding device can be, but not limited to, a cart or a basket.
[0058] Referring to FIG. 1 , a food item ( 101 ) contains an identifiable mark ( 102 ), which can be a logo, UPC code, or another similar type of mark. The consumer ( 103 ) holds an extracting device ( 104 ) and uses it to interact with food item(s). This extracting device has at least one device ID ( 105 ) that is unique to him. This device ID can be derived from a hardware component inside the extracting device such as IMEI (International Mobile Equipment Identity), Media Access Control (MAC) Address, Integrated Circuit Card Identifier (ICCID) of a Subscriber Identification Module (SIM). The device ID can also be derived from consumer information ( 106 ) such as email address, account login information, name. An extraction sensor bank ( 107 ) holds one or more extracting sensors ( 108 ), ( 109 ) each adapted to a specific type of meta-element ( 102 ). The extracting device is controlled by a CPU ( 110 ), typically a micro controller such Texas Instrument MSP430 or Apple A5 with volatile and nonvolatile memory. A clock or clock subsystem ( 111 ) maintains time and date. A bank ( 112 ) of sensors/sensor subsystems ( 113 ) is used to capture different attributes. In an embodiment, one of the sensors is an assisted-GPS to capture location information. In another embodiment, one of the sensors extracts the SSID or the certification information associated with a Wi-Fi Wireless LAN system. In another embodiment, temperature is being measured. In yet another embodiment, a single pixel sensor, such as by not limited to Charge-Coupled Device (CCD) or Complementary Metal-Oxide-Semiconductor (CMOS) sensor is used to measure light. A consumer interface ( 114 ) is used to interface with the consumer. In an embodiment, the consumer interface may include but is not limited to at least one of a visual, audio or textual interface.
[0059] Referring to FIG. 2 , methods in which an extracting device ( 201 ) may be architected to enable context aware interaction with packaging are illustrated. This device is controlled by a micro-controller ( 202 ). This microcontroller includes a memory device, herein referred to as Extractor Configuration Memory or ECM ( 203 ), typically non-volatile (EEPROM or FLASH memory) to store configuration operation about the extractor hardware and software it hosts. This ECM may include but is not limited to: Device ID ( 204 ), typically set at manufacturing and unique to each extractor, NFC ID ( 205 ) if used also as an electronic wallet, Operating system Version Number ( 207 ), Application Signed Certification ID ( 208 ) used to register application with the operating system provider, Consumer ID ( 209 ) used to identify primary consumer of extracting device, Kitchen ID ( 210 ) an identifier of the primary kitchen group the consumer uses. The microcontroller can also include (or have access to) a memory bank that stores recent transactions dubbed the Extractor Actions Memory or EAM ( 215 ). This may be a dedicated memory area or may be shared with other applications. An event with EventID 1 ( 212 ) and another one with EventID 2 ( 213 ) are stored. Each event has among other attributes the time and date recorded, event type (capturing information such as whether the information/exchange associated with the event was pulled, pushed, one-on-one, broadcast, private, public consumer-initiated, etc.) and relevance code used to categorize and organize which past actions are relevant to consider as part of a specific transaction or set of transactions. The extractor has also a bank ( 214 ) of sensors used to capture different attributes. A GPS Receiver ( 215 ) is used to capture location and speed. An indoor locator ( 216 ) is used to detect whether the extractor is indoor or outdoor. This can be accomplished by looking at RF channel response or light spectrum. A proximity sensor ( 217 ) (capacitive, inductive or otherwise) is used to check whether the consumer or an object is near the extractor. A temperature sensor ( 218 ) measures temperature (many micro-controllers have a built in temperature sensor. A light sensor ( 219 ) measures lighting intensity. A pressure sensor ( 220 ) measures pressure. A gyroscope ( 221 ) measures the three-dimensional position of the extractor. A contact switch ( 222 ) measures whether the extractor is in contact with a solid or liquid surface. A microphone ( 223 ) captures sounds. A still camera ( 224 ) captures images. A video camera ( 225 ) captures videos. The sensors ( 215 ) to ( 224 ) can store information collected.
[0060] Referring to FIG. 3 , a system that supports context aware interaction with packaging is illustrated. A consumer ( 301 ) who may have a loyalty card ( 302 ) uses his or her extracting device ( 303 ) while shopping. The cell phone ( 303 ) is brought up close to a food package ( 304 ), a merchandising display ( 305 ), a shopping basket ( 306 ), or a shopping cart ( 307 ). The merchandising display may be located by the cashier or point of sales (POS) terminal. It should be noted nothing precludes the interaction between consumer and packaging might take place at the consumer home and is not restricted to be solely at a grocery store, supermarket, or other food retailer. Each of the ( 304 - 307 ) possible items holds one or more uniquely identifiable logo or code ( 308 ). In order for the cell phone ( 303 ) to add context awareness to the interaction with the food package, merchandising display, basket, or cart, certain items must be present in cell phone, namely a microcontroller ( 309 ), memory ( 310 ) and software ( 311 ). The memory also holds information about the consumer such as consumer ID ( 312 ). The memory also holds an object store ( 313 ) with one or more digital objects ( 314 ). Food suppliers maintained a series of servers ( 315 ) used in conjunction with the consumer cell phone to provide a context aware interaction. In this embodiment, suppliers maintain their own servers ( 315 ). Each server includes a digital object Store ( 316 ) that includes one or more digital objects ( 317 ). Program memory ( 318 ) maintains the computing; customization, processing or presentation (e.g. display of images or text, play of video or audio, control of vibration), rules of the digital objects organized by ID ( 319 ). These IDs can be the same as, or related to one another, through database manipulation, taxonomy, or algorithmically to the consumer ID ( 312 ), or unique ID of specific packages, store, or location. These rules are executed by a central processing unit ( 320 ). While this figure shows multiple servers distinct from one another holding digital objects, it should be noted that these servers can be located, or can be deployed, using so-called cloud based systems, merged across multiple suppliers, or a combination of the above. Suppliers can be, but not limited to, consumer packaged group manufacturers, restaurants, supermarkets, grocery stores, etc.
[0061] Referring to FIG. 4 , the structure of some of the key databases used in the supplier servers described in FIG. 3 above are illustrated. An integrated database structure is shown as ( 401 ). The digital object database ( 402 ) is organized by SKU (stock keeping unit) ( 403 ). For each SKU, a UPC, GS1, serial number, version number or similar code ( 404 ) is stored. A default digital object ( 405 ) is associated with these SKU item(s). These default digital object IDs may be a brand label or store level advertising message. This default object can be unique to each SKU, or generic to a brand (that is a collection of SKUs), or generic to a store. If appropriate, a default financial object ( 406 ), a default media ( 407 ), or default application object ( 408 ) can also provided. Optionally, in addition to the above, a collection of digital objects ( 409 - 410 ) is provided. These objects can be organized using a multitude of potential architectures ranging, among others, from a flat file format, to a SQL based structure, and/or non-SQL based relational structures. The context use database ( 411 ) is another key element used to provide a context aware interaction. This database contains a series of contexts ( 412 , 413 , and 414 ). In this specific embodiment, context information is organized on a per context basis ( 415 ). This context information can be organized in other manner, most notably on a per SKU basis. For each context considered, requirements ( 416 ) associated with the proper presentation, customization, execution or display of one or more digital objects are encoded. These requirements can be (among others):
a. Restriction on the location such as, but not limited to, home vs. store, store 1 rather than store 2, store location 1 vs. store location 2, location within the store itself b. Quality of the communication bandwidth available: this can be a quantitative measure, say bit/sec, ICMP performance—or a qualitative measure imparted by the air interface support—say WiFi vs. 3G vs. LTE) c. Time of day, day of week (certain dry counties in the United States do not allow the purchase of alcohol on Sunday before noon, so marketing wine at that time does not make sense) d. Age of consumer (the information presented to a three year old should be different from that presented to a 25 year old even if they are both using the same extracting device) e. Compliance with HIPAA (The Health Insurance Portability and Accountability Act of 1996, Pub. L. 104-191, 110 Stat. 1936, enacted Aug. 21, 1996) f. Compliance with Children's Online Privacy Protection Act of 1998 (COPPA, 15 U.S.C. §§6501-6506 (Pub. L. 105-277, 112 Stat. 2581-728, enacted Oct. 21, 1998) g. Other specific interaction between consumer held device and packaging (such as distance between device and packaging or angle of device) h. The presence of specific tokens or information inside the scanning device or devices associated or paired with said device.
[0070] In this embodiment, these contexts are applicable to one or more SKUs ( 417 ). These SKUs can be organized in the form of a list of individual SKUs or a range of applicable of SKUs. They can be provided explicitly in a declarative or formulaic manner, organized by class of products (see 424 ). Consumer input ( 418 ), whether directly from the consumer interface (press here button appearing on screen of device, associated device, or paired device), or already stored into memory (possibly based on previous interaction history, group membership, social group membership) are used to shape or alter the consumer interactions, and provide context-awareness to them. In order to provide appropriate business intelligence feedback, and an improved performance of the overall system, feedback from the consumer all can be captured, and stored in memory ( 419 ). Examples of such captured data includes the amount of time a device is scanning a specific piece of package, or whether additional information was requested by the consumer. Another optional element of the database is the so-called associated SKU database ( 420 ). This associated SKU database is used to provide alternate SKU items to the consumer when scanning an original SKU. For each original SKU item for which a substitute or compliment is to be provided ( 421 ), one or more SKUs ( 422 ) are listed. Some of these SKUs belong to the same class of food as the original SKU, others don't. An example of class is for instance canned fruits, or nuts. The “in class” and “other food class” ( 423 ) are shown in the SKU taxonomy database ( 424 ). Here, a series of classes ( 425 ) is used to categorize different food items ( 426 ) in a manner logical and familiar to consumers. This taxonomy database is optional. Different suppliers will have different taxonomy databases for the SKUs they sell to the marketplace. It should be noted that different digital objects will be stored using different formats, an example, by no means restricting, is provided in ( 402 ). Financial objects can be stored as encrypted files. Media objects can be stored using media file formats such as JPEG, HTML5, and mp3 among others. Application objects can be stored using byte code, applet structures, or JavaScript among others.
[0071] Referring to FIG. 5 , the logic and flow of digital objects used to provide context aware interaction to consumers is illustrated. The extracting device ( 501 ) includes a microcontroller ( 502 ) and the consumer ID ( 503 ) is stored along with optional associated consumer ID ( 504 ) might actually be stored. This extracting device is referred to as phone 1 (but can be any of the devices listed in FIG. 1 ). This invention allows for group interaction, as well as social networking of specific interactions between consumers, such as family members or friends. Because extracting devices such as cell phones, RFID readers have a finite amount of memory, it may be necessary for online as well as data repositories be deployed in order to cover as many SKUs as possible. These are represented by the servers ( 509 ). In each one of these servers, the logical rules of specific media objects are stored into memory ( 510 ). These rules are organized according to IDs ( 511 - 512 ). Each server (which can be a set of dedicated servers in a server farm, on the web using cloud-based services such as SAAS) holds one or more digital object stores ( 513 ), each storing one or more digital objects ( 514 ). Each server is controlled by at least one central processing unit ( 515 ). The management of these digital objects is controlled by the so-called pre-fetch/push digital object manager ( 516 ). Algorithms controlling this pre-fetch/push digital object manager are implemented by a central processing unit ( 517 ). The pre-fetch/push digital object manager holds for each consumer a specific database ( 519 ) of SKUs ( 520 ) already purchased by the consumer or his family. In this embodiment, ( 520 ) such SKUs are stored in the (or a) database. Another part ( 521 ) of the database stores information about SKUs recently scanned or searched by the user, family, or social network ( 522 ). These searches could take place on the web or database, using a computer or a mobile device. In this embodiment, v such SKUs ( 522 ) are stored in the database. Based on heuristics developed by suppliers and third parties, SKUs in the associated SKU database of FIG. 4 with scanned SKUs may be added to this database. Yet another part ( 523 ) of the database includes digital objects ( 524 ) that need to be pushed (or downloaded) to devices. In this embodiment, x such SKUs ( 524 ) are stored in the database. Yet, another part ( 525 ) of database keeps track digital objects ( 526 ) that need to be pushed (or downloaded) to devices (there can be more than one). In this embodiment, y such SKUs ( 526 ) are stored in the database. This number of SKUs stored in each part of the database, that is n, v, x and y will vary with time. The pre-fetch/push digital object manager may be collocated or remote from one or more of the servers. Servers, pre-fetch/push digital object manager and consumer phone or through one or more wireless or wired network ( 528 ). On a regular, scheduled or ad-hoc basis, a command ( 527 ) is executed to tag part or whole of the digital objects in the purchased item part ( 519 ) of the database and scanned/searched (and associated) part ( 521 ) of the database into the digital objects to push to devices part ( 523 ) of the database. On a regular, ad-hoc, and/or based on wireless network performance (bandwidth, latency, etc.), a command ( 529 ) is issued from the pre-fetch/push digital object manager to the servers, which, in turn, transfers ( 530 ) the referenced objects to the consumer phone. This can also be done using synchronization services as i-could, intellisync, active-sync. Push notification technologies that may be used for this purpose include but are not limited technologies such as Apple's Apple Push Notification Service (APNS) (which is supported on iOs) and Cloud to Device Messaging (C2DM) (which is supported in the Android operating system). A phone 2 ( 531 ) is associated with phone 1 ( 501 ) because the consumer ID ( 532 ) of phone 2 is one of those associated with that ( 504 ) of phone 1 . Phone 2 is connected to one or more other servers through one or more wireless or wired networks ( 533 ). Digital objects are transferred ( 534 ) from the servers to form 2 . These objects do not have to be the same as those transferred to phone 1 .
[0072] Referring to FIG. 6 , methods in which the context of a consumer interaction can be computed are illustrated. One or more of sensor data extracted from one or more portable devices ( 601 ), preferences stated by the consumer ( 603 ), references gathered from analysis of consumer interactions ( 603 ), restrictions (diet, brands, other) indicated by the consumer ( 604 ), consumer history such as, but not restricted, purchases or queries ( 605 ), and the history of consumers associated (family, social network, neighbors) with the consumer ( 607 ) that can be used to compute the context. The computation ( 601 ) is performed by the consumer cell phone, a portable device in the vicinity of said cell phone, or on a server where consumer information is kept. The sensor data from multiple phones can be used to enable services where the location of one family member impacts the context (and this interaction) of another family member. This computation also redistributed between consumer phone and one or more servers. Upon scanning of a specific item ( 608 ), its SKU is identified ( 609 ). The SKU digital object database is queried ( 610 ), the SKU context use database is also queried ( 611 ). These two databases are preferably but not necessarily stored on the consumer phone. They can be located at the store or remotely at the supplier. Finally the digital object is selected and then presented on one or more cell phones.
[0073] Referring to FIG. 7 , nominal examples of the evolution of contexts for both store ( 701 ) and home ( 702 ) scanning scenarios are illustrated. For each context ( 703 ) architected and supported by one or more extracting devices, a description of the context ( 704 ) is provided. Column ( 705 ) encodes which media objects to present for an associated specific context. In the context of this software description, one can think of context as a state of a state machine. When entering the store, the default context is Default context S 1 ( 706 ). This context is used to control the displaying of media objects use before any specific interaction is performed by the consumer with any packaging, and also when after some scanning activities are performed, consumer inactivity is establish by the timer ( 707 ) expiring. In this embodiment, context 1 ( 708 ) reflects the case where a consumer scans a package that happens to contain a food with a specific allergen affecting the consumer, or his/her family. A warning about the presence of the allergen is provided to the consumer and, optionally, recommendations for a proposed substitution SKU is provided. This interaction moves the consumer to context 2 ( 709 ). In this context, upon scanning, a different media object is presented, in this case a coupon that fosters the purchase of a, substitution product. This move from context 1 to context 2 and the associated media objects that would be presented to the consumer a typical example of “in hand marketing” enabled by this invention. At home ( 702 ), there is an equivalent default context called default context H ( 710 ). The scanning device might be displaying information about say food inventory status, such as in this embodiment a reminder that certain foods might be about to go bad (banana is really really black). This embodiment highlights the case where the consumer is working to collect items for a recipe. There are multiple ways to start. The consumer might be checking a recipe on the web from his computer or using a mobile browser. The scanning device can be made aware of this search (through signaling or deposit of information into approach memory location), and information about ingredients transferred dynamically to recipe management software. This action brings the extracting device to context 3 ( 711 ). Another starting point might be for the consumer to scan a specific item ( 712 ) and based on his item, select a recipe that includes the ingredient. This is context 4 . From that point on and until the consumer indicates so or all items of the recipe are scanned for, the scanning device interactions moves back and forth between context 5 ( 713 ) when the ingredient scanned is in the recipe and context 6 ( 714 ) when it is not. If no action is detected after timer ( 715 ) expires; the scanning device is moved back to default context H ( 701 ). It should be noted that the same consumer might experience a different interaction—supported by the presentation of different media objects—for the same item at home compared to the store. This is a typical example of the context aware interactive packaging enabled by this invention.
[0074] Referring to FIG. 8 , scanning of a specific food item used to display multiple media objects on multiple phones, and methods of facilitating a group purchase of said items. A group of consumers ( 801 ) each carrying a scanning device, say a cell phone ( 802 ). They belong to a food service database hosted on a server which allows, among other services; consumers to help one another find specific food items. In this figure, seven consumers are listed. These consumers register what type of food they seek to find. This registration is done as part of registration, preferences, or analysis of their and other purchases. Food 1 ( 804 ) is a choice for consumers A, C, D and E. Food 2 ( 805 ) is also the choice of consumer E. At this embodiment illustrates, a specific consumer may register more than one food item. Food 3 ( 806 ) is the choice of consumers B and C. Consumer E registers that it is interested to receive information about food and from 3rd parties inside and outside his/her social network. Consumers A, B, C, D and G belong to the same, or one of the same inter-connected, social network(s) (say Facebook, twitter, Google+). The server manages the database the different cell phones of the consumers who are connected to one or more wireless networks ( 809 ). Consumer G while shopping at a market ( 810 ) scans a mark ( 811 ) that identifies the market to be supported for a specific food service ( 811 )—this step can be skipped. Consumer G also a food that is a registered food 1 ( 812 ) at said market. This market is within a geographical area ( 813 ). Upon scanning of item ( 812 ), a message is sent from consumer G phone to the server, which transmits a digital media object to members of consumer G social group and to third parties agreeing to receive such requests who happen to be within the geographical area ( 813 ) convert by the market ( 810 ). Those consumers will receive in digital object indicating that hard to find food 1 has been spotted and is available for purchase market ( 810 ). In this embodiment, only consumers D and E will receive media objects on their cell phone. Optionally, consumer D may receive and additional digital object permission in consumer G to purchase item ( 812 ) on her behalf.
[0075] Referring to FIG. 9 , another embodiment including enabling customized and dynamic pricing as well as real-time price bidding is illustrated. A consumer ( 901 ) owns a mobile device ( 902 ) with an ID ( 903 ) stored. Consumer operates phone within a store ( 904 ) operated by Retailer C ( 905 ). Profile and history information ( 906 ) are stored in a server ( 907 ). At the store, the consumer scans a series of products ( 908 ). Pricing information on these products is in the form of the label affixed ( 909 ) to the product or affixed to the shelf next to the product ( 910 ). Upon scanning of said items, one or more financial objects are displayed on the phone. These financial items may be coupons or offer from one or more suppliers to substitute food scanned with another (say for instance moving from garlic to minced garlic). The consumer scans an item ( 911 ), which has a regular price, affixed to it ( 912 ). In this embodiment, item ( 911 ) is a store item. Upon scanning, a financial object is displayed on the phone that indicates what the price is the consumer will end up paying for this item. This price can be set differently for different times of day, different consumer demographics, or specific conditions, thus allowing a unique consumer centric dynamic pricing to be provided to consumer ( 901 ). A cold cola could be priced at higher amount during a festival. This can be used to sell items that are close to their expiration dates, such as—but not limited to—milk products and eggs. Eggs with only 14 days left until use by date can be charged less than those with 21 days left until use by date. Different consumers would experience different prices thus allowing consumer per consumer, item per item pricing. Upon scanning of item ( 911 ), the consumer is prompted by one or more new digital objects to purchase cereals. In this embodiment, there are two providers of cereals: CPG A ( 914 ) who sells cereal A ( 915 ) at a regular price ( 916 ) and CPG B ( 917 ) who sells cereal B ( 918 ) at the regular price ( 919 ). In this embodiment, CPG A and CPG B are competing/bidding for business of consumer ( 901 ). The consumer will indicate by scanning the chosen produces with a phone based scanner, he/she chooses to scan an item ( 914 ), he/she would indicate to CPG A that he/she is choosing its product. Should he/she choose item ( 918 ), he/she would indicate to CPG B that he/she's is choosing its product. The CPGs have now the opportunity to offer complementation products. CPG A can offer an offer for item ( 920 ) regularly priced at ( 921 ). CPG B can offer an offer for item ( 922 ) regularly priced at ( 923 ). The discount of price or credit ( 924 ) offered for item ( 920 ) can be made different if the consumer has purchased ( 915 ) or not. The discount of price or credit ( 925 ) offered for item ( 922 ) can be made different if the consumer has purchased ( 918 ) or not. To highlight and induce the consumer, the mobile device will display information about the product ( 926 ) tailored to the consumer, along with regular ( 927 ) as well as effective ( 982 ) price. Purchases are registered at a POS ( 929 ) terminal. It should be noted that this POS might be a mobile POS, or an application running on the mobile device itself. A credit clearing house—or equivalently bank—( 930 ) can transfer credit the consumer credit card ( 931 ) or the consumer loyalty card ( 932 ).
[0076] Referring to FIG. 10 , another embodiment is illustrated. A consumer ( 1001 ) who may have a loyalty card ( 1002 ) uses her cell phone ( 1003 ) while shopping. The cell phone is brought up close to a food package ( 304 ), a merchandising display ( 305 ), a shopping basket ( 306 ), or a shopping cart ( 307 ). The cell phone includes microcontroller ( 1004 ), memory ( 1005 ) and software ( 1006 ) and one more transceiver ( 1007 ). The memory also holds information about the consumer such as consumer ID ( 1008 ), consumer history ( 1009 ) and consumer preferences ( 1010 ). The memory also holds an object store ( 1011 ) with one or more digital objects ( 1012 ). The consumer seeks to purchase item ( 1013 ) and places it in the vicinity of shopping cart ( 1014 ) or shopping cart ( 1015 ). She uses a store provided scanner ( 1016 ). It can be attached to the cart ( 1015 ) or basket ( 1014 ). The scanner includes a microcontroller ( 1017 ), a scanning device ( 1018 ), memory ( 1019 ) to store software ( 1020 ). The scanning device might scan barcodes. It includes a digital object Store ( 1021 ) that includes one or more digital objects ( 1022 ). The scanner is associated with the mobile device. The scanner scans the product ( 1013 ) and extracts a unique identifier. As in previous examples, the mobile phone presents one or more digital objects based on the unique identifier. The store maintains a server ( 1023 ) that is used in conjunction with the consumer cell phone to provide context aware interaction. The server includes a digital object store ( 1024 ) that includes one or more digital objects ( 1025 ). The server is controlled by a central processing unit ( 1026 ). Program memory ( 1027 ) maintains the computing, customization, processing or presentation (e.g. display of images or text, play of video or audio, control of vibration), rules of the digital objects organized by ID ( 1028 - 1029 ). These ID can be the same as or related through database manipulation, taxonomy or algorithmically to the consumer ID ( 1008 ). Based on unique identifier, all or part of consumer history ( 1009 ) or all or part of preference ( 1010 ) or unique ID of specific packages, the store server presents one or more digital objects to the mobile phone (directly or through the scanner). When those digital objects are used to support a real-time pricing/binding service, the store server might be connected to one or more supplier servers ( 1030 ).
[0077] Emphasis was given herein to visual scanning. As RFID systems become deployed at the item level, information can be exchanged between portable devices, and said item, using radio-wave rather than optical scanning, supporting functionality enabled by this invention and is thus claimed.
[0078] The presentation of digital objects can be done using one or more of the following techniques: Display of images and text, playing of video clips, playing of audio, vibrating patterns, change in temperature, changes in textures, changes in shape, changes in patterns, generation of smells, and relational dependencies between these. All these techniques are claimed.
[0079] Servers described in this invention can be found in a multitude of devices including, but not limited, personal computer, server farms, enterprise computers, blade servers, mainframe, portable devices, cellphones, tablets, standalone, or shared servers, and cloud based portable devices. For instance, the same mobile device may have scanning software, extraction software, and a server running as separate functions on the same hardware. All these realizations are claimed. Servers can be inter-networked, inter-connected, and connected to other servers, at times under the same administration or security framework, at times under different administration or security frameworks. For instance, a store computer might interface with a consumer database managed by another server. Likewise, a food supplier server might subscribe (as in RSS) to information broadcasted by a specific association server. Functionality enabled by this interconnection or subscription is claimed.
[0080] When considering associated devices such as scanner associated with a mobile device, communication to servers can be performed using either communication capability; that is using the scanner wireless capabilities or the mobile device capabilities interchangeably. All these communication methods are claimed.
[0081] While this invention describes interactions in terms of food products, nothing precludes the implementation of this invention to other items, including items found around the home and stores such as detergent, cleaning supplies, clothing, receipts, posters, and magazines.
EMBODIMENT LIST
[0082] The following list includes particular embodiments. The list, however, is not limiting and does not exclude alternate embodiments otherwise described or as would be appreciated by one of ordinary skill in the art.
[0000] 1. A computer-implemented method comprising:
[0083] providing a first set of instructions configured to cause a portable device to:
[0084] i) scan all or a portion of packaging,
[0085] ii) locate a visual indicator in the visible portion of packaging,
[0086] iii) map said visual indicator into at least one index, access one or more extraction attributes;
[0087] identifying one or more digital objects based on the at least index and the one or more extraction attributes; and
[0088] presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects.
[0000] 2. The computer-implemented method of embodiment 1, wherein the one or more extraction attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
3. The computer-implemented method of any one or more of embodiments 1-2 further comprising storing use of the particular digital object into non-volatile memory upon a user selecting the control.
4. The computer-implemented method of any one or more of embodiments 1-3, wherein the step of identifying further comprises:
[0089] transmitting the at least one index and the one or more extraction attributes to a second portable device;
[0090] accessing, by the second portable device, the at least one index and the one or more extraction attributes; and
[0091] identifying one or more digital objects by the second portable database based on the at least one index and the one or more extraction attributes.
[0000] 5. The computer-implemented method of any one or more of embodiments 1-4 further comprising sending at least one of the one or more digital objects to a third portable device.
6. The computer-implemented method of any one or more of embodiments 1-5 further comprising sending information identifying the particular digital object to a server upon a consumer selecting the control.
7. The computer-implemented method of any one or more of embodiments 1-6, wherein the step of identifying further comprises:
[0092] transmitting the at least one index and the one or more extraction attributes to a second portable device;
[0093] accessing a second set of one or more extraction attributes by the second portable device; and
[0094] identifying one or more digital objects based on the at least one index, the one or more extraction attributes, and the second set of one or more extraction attributes by the second portable device.
[0000] 8. The computer-implemented method of any one or more of embodiments 1-7, wherein the second set of one or more extraction attributes by the second portable device are selected from the group consisting of location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
9. The computer-implemented method of any one or more of embodiments 1-8 further comprising sending at least one of the one or more digital objects to a third portable device.
10. The computer-implemented method of any one or more of embodiments 1-9 further comprising sending at least one of the one or more digital objects to a second portable device.
11. The computer-implemented method of any one or more of embodiments 1-10, wherein the one or more digital objects includes at least one of a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information.
12. The computer-implemented method of embodiment 11, wherein the financial instrument is at least one of a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
13. The computer-implemented method of any one or more of embodiments 1-12, wherein where selecting the particular digital objects is based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, preferences or restrictions.
14. The computer-implemented method of any one or more of embodiments 1-13 further comprising:
[0095] creating a second index to the particular digital object;
[0096] generating one or more unique transaction identifiers based on that second index; and
[0097] transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0000] 15. A computer-implemented method comprising:
[0098] providing a first set of instructions configured to cause a portable device to:
i) scan all or a portion of packaging, ii) locate a visual indicator in the visible portion of packaging, iii) map said visual indicator into at least one index, iv) access one or more extraction attributes, and v) send the at least one index and the one or more extraction attributes to a server;
[0104] receiving, at the server, from the portable device, a first request comprising the at least one index and the one or more extraction attributes;
[0105] identifying one or more digital objects by the server, based on the at least one index and the one or more extraction attributes;
[0106] sending to the portable device a second set of instructions by the server in response to the first request, configured to cause the portable device to:
i) present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) send information identifying the particular digital object to a server upon a consumer selecting the control; and iii) send to the server, from the portable device, a second request identifying the particular digital object.
16. The computer-implemented method of embodiment 15 further comprising receiving the second request at the server.
17. The computer-implemented method of any one or more of embodiments 16-17, wherein the one or more extraction attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
18. The computer-implemented method of any one or more of embodiments 1-17, wherein the step of identifying further comprises:
[0110] querying a second server based on at least one of a context attribute; and
[0111] identifying the one or more digital objects based on the context attribute from the second server, the at least one index and the one or more extraction attributes.
[0000] 19. The computer-implemented method of any one or more of embodiments 1-18 further comprising sending at least one of the one or more digital objects to a second portable device.
20. The computer-implemented method of any one or more of embodiments 1-18, wherein the one or more digital objects includes at least one of a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information.
21. The computer-implemented method of embodiment 20, wherein the financial instrument is at least one of a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
22. The computer-implemented method of any one or more of embodiments 1-21, wherein selecting the particular digital objects is based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, preferences or restrictions.
23. The computer-implemented method of any one or more of embodiments 1-22 further comprising:
[0112] creating a second index to the particular digital object;
[0113] generating one or more unique transaction identifiers based on that second index; and
[0114] transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0000] 24. A computer-implemented method comprising:
[0115] providing a first set of instructions configured to cause a first portable device to:
[0116] i) scan a portion of packaging,
[0117] ii) locate a visual indicator in the visible portion of packaging,
[0118] iii) map said visual indicator into an index, and access one or more of a first set of extraction attributes;
[0119] transmitting the index and the first set of extraction attributes to a second portable device;
[0120] accessing one or more of a second set of extraction attributes;
[0121] sending the index and the first or second set of extraction attributes to a server by the second portable device;
[0122] receiving, at the server, from the second portable device, a first request comprising the index and said attributes;
[0123] identifying one or more digital objects by the server based on the index and said attributes;
[0124] sending a second set of instructions to the second portable device by the server, in response to the first request, configured to cause the second portable device to:
[0125] i) present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects,
[0126] ii) send information identifying the particular digital object to a server upon a consumer selecting the control, and
[0127] iii) send to the server, from the second portable device, a second request identifying the particular digital object.
[0000] 25. The computer-implemented method of embodiment 24 further comprising receiving the second request at the server.
26. The computer-implemented method of any one or more of embodiments 24-25, wherein the one or more of a first set of extraction attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; distance to packaging; portable device parameters; application parameters; and identification parameters.
27. The computer-implemented method of any one or more of embodiments 24-26, wherein the one or more of a second set of extraction attributes by the second portable device are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
28. The computer-implemented method of any one or more of embodiments 24-27 further comprising sending at least one of the one or more digital objects to a second portable device.
29. The computer-implemented method of any one or more of embodiments 24-28, wherein the one or more digital objects includes at least one of a game, a virtual machine, a form-based questionnaire, a coupon, a discount, an advertisement, a financial instrument, pricing information, nutritional information, allergy information, a recipe, inventory information, geographical information, environmental information or social networking information.
30. The computer-implemented method of embodiment 29, wherein the financial instrument is at least one of a currency, a contract, a bid, an equity, a security, a tax, a fixed security, or indexes thereof.
31. The computer-implemented method of any one or more of embodiments 24-30, wherein selecting the particular digital objects is based on one or more of extraction attributes, purchase history, credit history, membership in group, time of day, day of week, environmental conditions, or preferences or restrictions.
32. The computer-implemented method of any one or more of embodiments 24-31 further comprising:
[0128] creating a second index to the particular digital object;
[0129] generating one or more unique transaction identifiers based on that second index; and
[0130] transmitting one or more transaction data each associated with said identifier to one or more remote servers.
[0000] 33. A non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, perform actions including:
[0131] scanning a portion of packaging;
[0132] locating a visual indicator in the visible portion of packaging:
[0133] mapping said visual indicator into at least one index;
[0134] accessing one or more context attributes;
[0135] presenting an interactive interface comprising information about one or more digital objects;
[0136] presenting to a consumer a control for selecting a particular digital object of the one or more digital objects; and
[0137] sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0000] 34. The non-transitory machine-readable storage medium of embodiment 33, wherein the one or more context attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
35. The non-transitory machine-readable storage medium of any one or more of embodiments 33-34, further comprising:
[0138] sending the index and one or more extraction attributes to a server; and
[0139] receiving a set of instructions, prior to presenting an interactive interface comprising information about one or more digital objects.
[0000] 36. A non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including:
[0140] providing a first set of instructions configured to cause a portable device to:
[0141] i) scan all or a portion of packaging,
[0142] ii) locate a visual indicator in the visible portion of packaging,
[0143] iii) map said visual indicator into at least one index,
[0144] iv) access one or more extraction attributes;
[0145] identifying one or more digital attributes based on the at least one index and the one or more extraction attributes,
[0146] presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; and
[0147] storing use of the particular digital object into non-volatile memory upon a consumer selecting the control.
[0000] 37. The non-transitory machine-readable storage medium of embodiment 36, wherein one or more extraction attributes selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
38. A non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including:
[0148] providing a first set of instructions configured to cause a portable device to:
[0149] i) scan all or a portion of packaging,
[0150] ii) locate a visual indicator in the visible portion of packaging,
[0151] iii) map said visual indicator into at least one index,
[0152] iv) access one or more extraction attributes;
[0153] identifying one or more digital objects based on the at least one index and the one or more extraction attributes;
[0154] presenting an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; and
[0155] sending information identifying the particular digital object to a server upon a consumer selecting the control.
[0000] 39. The non-transitory machine-readable storage medium of embodiment 38, wherein the one or more extraction attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
40. An interactive packaging processing system comprising:
[0156] one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory, and a user interface;
[0157] the one or more portable devices capable of extracting one or more extraction attributes;
[0158] at least one of the one or more portable devices capable of selecting one or more digital objects based on information from scanning the packages and the one or more attributes and presenting the one or more digital objects to the portable device user interface.
[0000] 41. The interactive packaging processing system of embodiment 40, wherein the one or more attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
42. An interactive packaging processing system comprising:
[0159] one or more portable devices capable of scanning packages, said portable devices comprising a processing unit, memory and user interface and said portable devices capable of extracting one or more extraction attributes;
[0160] one or more servers comprising one or more digital objects stores, a central processing unit and memory, said one or more digital objects stores storing one or more digital objects;
[0161] at least one portable device capable of scanning a package, extracting a first of set of one or more of said attributes and transmitting information about scanned package;
[0162] at least a second portable device capable of extracting a second set of one or more of said attributes;
[0163] said at least one portable device capable of exchanging said first set of attributes to a second device;
[0164] said portable devices capable of transmitting first set of attributes, second set of attributes and information about scanned package to one or more servers,
[0165] said one or more servers capable of selecting one or more digital objects based on scanned package information and attributes, and
[0166] said servers capable of transmitting one or more digital objects to one or more portable devices.
[0000] 43. The interactive packaging processing system of embodiment 42, wherein the one or more attributes are selected from the group consisting of: location; speed; time; velocity; orientation; sound; lighting; vibration; repeated motion; distance to packaging; distance between packaging and nearby related objects; portable device parameters; application parameters; and identification parameters.
44. A computer-implemented method comprising:
b) Providing a first set of instructions configured to cause a portable device to:
i) Scan all or a portion of packaging; ii) Locate a visual indicator in the visible portion of packaging; iii) Map said visual indicator into an index, and/or indices; iv) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters;
c) Based on the index and attributes, the portable device identifying one or more digital objects;
i) Present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; and, ii) Upon a consumer selecting the control, store use of the particular media into non-volatile memory.
45. A computer-implemented method comprising:
d) Providing a first set of instructions configured to cause a portable device to:
i) Scan all or a portion of packaging; ii) Locate a visual indicator in the visible portion of packaging; iii) Map said visual indicator into an index, and/or indices; iv) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters;
e) Based on the index and attributes, the portable device identifying one or more digital objects;
i) Present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) Upon a consumer selecting the control, send information identifying the particular digital object to a server.
46. A computer-implemented method comprising:
f) Providing a first set of instructions configured to cause a portable device to:
i) Scan all or a portion of packaging; ii) Locate a visual indicator in the visible portion of packaging; iii) Map said visual indicator into an index, and/or indices; iv) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters; v) Send the index and attributes to a server;
g) Receiving, at the server, from the portable device, a first request comprising the index and attributes; h) Server querying a second server based on at least one of context attributes; i) Based on the response from second server to said query, index and attributes, the server identifying one or more digital objects; j) In response to the first request, the server sending to the portable device a second set of instructions configured to cause the portable device to:
i) Present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) Upon a consumer selecting the control, send information identifying the particular digital object to a server; iii) Receiving at the server, from the portable device, a second request identifying the particular digital object.
47. A computer-implemented method comprising:
k) Providing a first set of instructions configured to cause a first portable device to:
i) Scan all or a portion of packaging; ii) Locate a visual indicator in the visible portion of packaging; iii) Map said visual indicator into an index, and/or indices; iv) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters; v) Transmitting index and attributes to a second portable device; vi) Second portable device accessing location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters;
l) Based on the index and attributes, the second portable device identifying one or more digital objects;
i) Present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) Upon a consumer selecting the control, store use of the particular media into non-volatile memory.
48. A computer-implemented method comprising:
m) Providing a first set of instructions configured to cause a first portable device to:
i) Scan all or a portion of packaging; ii) Locate a visual indicator in the visible portion of packaging; iii) Map said visual indicator into an index, and/or indices; iv) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters; v) Transmitting index and attributes to a second portable device; vi) Second portable device accessing one or more second set extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters;
n) Based on the index and attributes, the second portable device identifying one or more digital objects;
i) Present an interactive interface comprising information about the one or more digital objects and a control for selecting a particular digital object of the one or more digital objects; ii) Upon a consumer selecting the control, send information identifying the particular digital object to a server.
49. A non-transitory machine-readable storage medium having recorded and stored thereon instructions that, when executed, performs actions including:
iii) Scan all or a portion of packaging; iv) Locate a visual indicator in the visible portion of packaging; v) Map said visual indicator into an index, and/or indices; vi) Access one or more extraction attributes from the group consisting of: location, speed, time, velocity, orientation, sound, lighting, vibration, repeated motion, distance to packaging, distance between packaging and nearby related objects, portable device parameters, application parameters, identification parameters; o) Send the index and attributes to a server; p) Receiving a set of instructions; q) Presenting an interactive interface comprising information about one or more digital objects; r) Presenting to a consumer a control for selecting a particular digital object of the one or more digital objects; s) Upon a consumer selecting the control, sending information identifying the particular digital object to a server.
[0225] All numbers expressed given in the form for some type of ingredients, goods, properties, and/or other parameters used in this specification, and claims, are to be understood as optionally modified in all instances by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits, and by applying ordinary rounding techniques.
[0226] The references cited throughout this application, are incorporated for all purposes apparent herein and in the references themselves as if each reference was fully set forth. For the sake of presentation, specific ones of these references are cited at particular locations herein. A citation of a reference at a particular location indicates a manner in which the teachings of the reference are incorporated. However, a citation of a reference at a particular location does not limit the manner in which all of the teachings of the cited reference are incorporated for all purposes.
[0227] The skilled artisan will readily appreciate that the methods and systems herein may be implemented with multiple consumers, multiple prospective consumers, and/or multiple registered consumers.
[0228] The methods herein may be implemented on myriad types of devices and/or combinations of devices. Combinations of devices may be functionally connected by physical or wireless connections as known in the art. A device may include a processor, a memory device, a communication interface, a data storage device, and a display, which may be a touchscreen display. These components may be connected via a system bus in the device, and/or via other appropriate interfaces within the device.
[0229] The memory device may be or include a device such as a Dynamic Random Access Memory (D-RAM), Static RAM (S-RAM), or other RAM or a flash memory.
[0230] The data storage device may be or include a hard disk, a magneto-optical medium, an optical medium such as a CD-ROM, a digital versatile disk (DVDs), or Blu-Ray disc (BD), or other type of device for electronic data storage. The data storage device may store instructions that define the application, and/or data that is used by the application.
[0231] The communication interface may be, for example, a communications port, a wired transceiver, a wireless transceiver, and/or a network card. The communication interface may be capable of communicating using technologies such as Ethernet, fiber optics, microwave, xDSL (Digital Subscriber Line), Wireless Local Area Network (WLAN) technology, wireless cellular technology, and/or any other appropriate technology.
[0232] The touchscreen display may be based on one or more technologies such as resistive touchscreen technology, surface acoustic wave technology, surface capacitave technology, projected capacitive technology, and/or any other appropriate touchscreen technology. When the touchscreen receives data that indicates user (e.g., a consumer, prospective consumer, or registered consumer) input, the touchscreen may provide data to an application implementing at least a portion of a method herein.
[0233] Although actions are described herein as being performed by the application, this is done for ease of description and it should be understood that these actions are actually performed by the processor (in conjunction with a persistent storage device, network interface, memory, and/or peripheral device interface) in the device, according to instructions defined in the application. The instructions may be stored on a computer readable medium. Alternatively or additionally, the memory device and/or the data storage device in the device may store instructions which, when executed by the processor, cause the processor to perform any feature or any combination of features described above as performed by the application. Alternatively or additionally, the memory device and/or the data storage device in the device may store instructions which, when executed by the processor, cause the processor to perform (in conjunction with the memory device, communication interface, data storage device, and/or the display, which may be a touchscreen display) any feature or any combination of features described above as performed by the application.
[0234] As used herein, the term “processor” broadly refers to and is not limited to a single- or multi-core central processing unit (CPU), a special purpose processor, a conventional processor, a Graphics Processing Unit (GPU), a digital signal processor (DSP), a plurality of microprocessors, one or more microprocessors in association with a DSP core, a controller, a microcontroller, one or more Application Specific Integrated Circuits (ASICs), one or more Field Programmable Gate Array (FPGA) circuits, any other type of integrated circuit (IC), a system-on-a-chip (SOC), and/or a state machine.
[0235] As used to herein, the term “computer-readable medium” broadly refers to and is not limited to a register, a cache memory, a ROM, a semiconductor memory device (such as a D-RAM, S-RAM, or other RAM), a magnetic medium such as a flash memory, a hard disk, a magneto-optical medium, an optical medium such as a CD-ROM, a DVDs, or BD, or other type of device for electronic data storage.
[0236] The features described herein may also be implemented, mutatis mutandis, on a desktop computer, a laptop computer, a netbook, a cellular phone, a personal digital assistant (PDA), or any other appropriate type of computing device or data processing device.
[0237] Although features and elements are described above in particular combinations, each feature or element can be used alone or in any combination with or without the other features and elements. For example, each feature or element as described above may be used alone without the other features and elements or in various combinations with or without other features and elements. Sub-elements of the methods and features described above may be performed in any arbitrary order (including concurrently), in any combination or sub-combination.
[0238] Further embodiments herein may be formed by supplementing an embodiment with one or more element from any one or more other embodiment herein, and/or substituting one or more element from one embodiment with one or more element from one or more other embodiment herein.
[0239] It is understood, therefore, that this invention is not limited to the particular embodiments disclosed, but is intended to cover all modifications which are within the spirit and scope of the invention as defined by the appended claims; the above description; and/or shown in the attached drawings.
[0240] It is understood, therefore, that this invention is not limited to the particular embodiments disclosed, but is intended to cover all modifications which are within the spirit and scope of the invention as defined by the appended claims; the above description; and/or shown in the attached drawings.
|
The subject matter described herein enhances the interaction of consumers with food packaging using cellphones and other portable scanners. Specifically, it enhances consumer's purchase decision and use decisions at key moments at home and store.
| 6
|
RELATED U.S. APPLICATION DATA
This is a continuation of Ser. No. 08/727,836 filed Oct. 15, 1996 and issued Feb. 17, 1998 as U.S. Pat. No. 5,719,817, which was a continuation of Ser. No. 08/407,721 filed Mar. 20, 1995 and issued Oct. 15, 1996 as U.S. Pat. No. 5,566,122, which was a continuation of Ser. No. 08/000,066 filed Jan. 4, 1993 and issued May 9, 1995 as U.S. Pat. No. 5,414,670, which was a continution of Ser. No. 07/608,125, filed Oct. 31, 1990 and issued Oct. 26, 1993 as U.S. Pat. No. 5,257,233.
FIELD OF THE INVENTION
This invention relates to packaging configurations for integrated circuit devices (ICs) and more particularly to packaging configuration is directed to logic arrays such as memory modules for computers or other electronic devices. More specifically, it describes an improvement to the design of a memory array which requires fewer random access memories (RAMs) to be turned on during a read or write cycle than present designs, thereby using less current.
BACKGROUND OF THE INVENTION
Current generation single in-line memory modules (SIMMs) for certain brands of computers use eight one-megabit (1M) dynamic random access memories (DRAMs) arranged in a x1 configuration (having one data out signal), which supplies the computer with one megabyte (MB) of memory. Since the DRAMs are arranged in a x1 configuration, one data bit can be extracted from each chip at a time. When a module with eight 1M×1 DRAMs is installed in a computer capable of handling eight bits of data at a time (i.e. an 8-bit computer), it accesses one bit location from each of eight DRAMs on a module simultaneously, thereby receiving eight bits of data. In 16-bit computers, modules containing eight 1M×1 DRAMs are installed in groups of two in the computer. To obtain 16 bits of data, all 16 DRAMs are accessed simultaneously, and the computer receives one bit of data from each DRAM for a total of 16 data bits. Each time a 1M×1 DRAM is accessed, it requires about 80 mA of current to be supplied. To access the 16 DRAMs simultaneously requires approximately 640 mA of current per module, or 1,280 mA total.
Some SIMMs use 1M×4 DRAMs, with each DRAM having four bits of data. A module using two 1M×4 chips supplies 1 MB of memory, as does a module using eight 1M×1 chips. A module with two 1M×4 devices is functionally equivalent to a module using eight 1M×1 devices, but has fewer parts, thereby being easier to assemble and somewhat more reliable due to fewer solder joints. There is not much power savings using a module with two 1M×4 DRAMs over a module using eight 1M×1 DRAMs, as all the devices on either module are turned on each time one of the devices is accessed in order to access eight data bits, and to access two 1M×4 DRAMs requires about as much power as accessing eight 1M×1 DRAMs.
In most computers, addressed words are an even number of bits, such as eight, sixteen or thirty-two bits. This fits into memory array blocks which use X4 chips but the arrangement is complicated by the fact that a system of memory parity has proven to be very effective in error detection. The parity is an additional bit for each word, so that an eight bit word ("byte") is addressed as nine bits, the ninth bit being parity.
Reducing power consumption in a computer or other electronic device is a design goal, as overtaxing a computer's power supply is a common concern. With the addition of modem cards, memory boards, graphics cards, hard disk controller cards, printer buffer cards, and mouse cards, the chances of burning out the computer's power supply from drawing too much current becomes a possibility. Even if the power supply is not unduly stressed, a component which uses more power than a similar component will release more heat, thereby increasing the temperature of the component as well as the inside of the computer or electronic device. Elevated temperatures within the component or within the chassis of a computer can cause other components in the computer to operate more slowly or to fail prematurely.
Reducing the amount of current used by the components in a computer is also a concern to designers of portable computers. The length of time between battery recharges for various brands and types of computers ranges from about two hours to 12 hours. Reducing the amount of current the computer uses, thereby extending the length of time the computer can be run off the battery, is a design concern as well as a marketing concern.
Reducing the power consumption of components installed in a computer is a goal of computer component designers and computer manufacturers.
SUMMARY OF THE INVENTION
An object of this invention is to provide a memory array which uses less power than previous arrays.
This object of the present invention is attained by fabricating an array using a number of memory chips, where each memory chip can be accessed independently, and where, for example, only the DRAM or DRAMs accessed is turned on while all other DRAMs remain in standby mode. A DRAM in standby mode uses much less current than activating the DRAM.
The invention can be applied to modules using DRAMs with multiple data out lines (DQ's). For instance, if a module supplying 1 MB of memory contains eight 1M×1 DRAMs is installed in an 8-bit computer, all eight DRAMs would have to be accessed simultaneously to supply the computer with 8 bits of data. On a 1 MB module using eight 256K×4, only two DRAMs would have to be accessed to supply the 8-bit computer with 8 bits of data.
Chips containing x16 data widths have recently been developed by Micron Technology, Inc. To manufacture these 64K×16 DRAMs, a current generation 1M die is packaged with 16 DQ pins to provide a chip in a 64K×16 configuration. Each of the 1,048,576 bits are uniquely addressed through the 16 address bits multiplexed on eight address lines (A0-A7) during a read or a write cycle.
A common memory configuration supplying 16 bits of data is to use two modules with each module comprising eight 1M×1 devices. A read cycle from two of these modules, as stated previously, requires about 640 mA of current. A functional equivalent of these modules would be two modules with each module comprising eight 64K×16 DRAMs. If these equivalent modules not comprising the invention are used, all 16 DRAMs would be turned on during a read cycle, even though the desired data comes from a single DRAM. A read would require 1280 mA of current. A module of this type comprising the invention, however, would enable only one DRAM during a read, thereby using about 90 mA of current.
When used in applications where an additional bit is used, as for parity, the additional bit may be incorporated into the multiple data out (DQ) architecture as an additional DQ connection. Alternatively, partially operational DRAMs may be used, provided at least one good sector may be addressed.
A module of this type would have signals conforming to JEDEC standards or, in custom uses, to specifications specific to the intended use of the module. In any case, a module containing eight 64K×16 devices would require one CAS line and eight RAS lines. The CAS line selects the desired column number in each of the eight DRAMs. The RAS lines are used as a bank select with each RAS line being used only by a single device, thereby accessing a row address from a single DRAM.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows an overview of the circuitry of the inventive module;
FIG. 2 details the decode circuitry of FIG. 1;
FIG. 3 shows a simple circuit which disables the write-per-bit mode of a DRAM containing multiple DQ's;
FIG. 4 shows the logic associated with the signals AR9 and AC9 which selects one of four groups of RAS signals;
FIG. 5 shows the logic associated with the signals AR8 and AC8 which selects a single DRAM from a group of four DRAMs;
FIG. 6 shows the logic associated with the write-per-bit lockout circuit of FIG. 3;
FIG. 7 depicts a partial view of the FIG. 1 structure and includes a plurality of subarrays in each RAM.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows an overview of the circuitry of one embodiment of the inventive array, including the data bus (DQ1-DQ16), the address bus (AD0-AD7), and output enable (OE). The address bus allows the computer to select individual DRAM cells to be written to or read from, while data is passed between the computer and the DRAMs along the bi-directional data bus. The OE signal controls the output buffers of the DRAM. During a READ cycle, the data is output on the data bus when the OE signal goes low.
All DRAMs share a single write enable (WE) signal, a single V CC , a common V SS , and a common CAS.
The signals AR8, AR9, AC8, and AC9 output by the computer to the module are altered by the decode circuitry (described below) to function as 16 RAS lines, which function as a select line to select one of 16 DRAMs on the module. Note that FIG. 1 shows eight RAMs; RAMs 9-16 operate in a fashion similar to RAMs 1-8, being addressed by RAS9-RAS16 as shown.
Following JEDEC standards, a computer or electronic device has only one RAS and one CAS input to a memory module. With only these two inputs, every time the electronic device accesses the memory, the same address on every DRAM is read or written, and as a result every device turns on. In a module comprising x1 DRAMs, this is not a problem because, as stated previously, a 16-bit computer accesses all 16×1 DRAMs to receive the 16 bits of data it is capable of handling. In a module comprising DRAMs with multiple DQ's, however, not every DRAM is accessed, but every DRAM is turned on. This requires that power be used unnecessarily.
In the inventive module, turning on all the DRAMs would defeat the purpose of the invention, which is to save power by turning on only those RAMs that are accessed. The decode circuitry in FIG. 2 solves this problem by using the two RAS address select bits (AR8 and AR9) and the two CAS address select bits (AC8 and AC9) output from the computer to the module in conjunction with the decode circuitry of FIG. 2 to turn on a single device. As shown, the two bits input on AR9 and AC9 are used to select one of four RAs signals internal to the decode circuitry, RASA, RASB, RASC, or RASD, depending on the state of the two bits as shown in FIG. 4.
Each of the four groups of signals in FIG. 4, RASA, RASB, RASC, and RASD have four unique RAS signals as shown in FIG. 2 which are internal to the decode circuitry and are output to the DRAMs. Referring to FIG. 2, after either RASA, RASB, RASC, or RASD is turned on, the bits supplied on AR8 and AC8 are used to select a single location from RAS1 through RAS16, each RAS line corresponding to a unique DRAM (not shown). FIG. 5 shows the decode logic which selects a specific DRAM. As shown in FIG. 2, RASA is divided into RAS1-RAS4, RASB is divided into RAS5-RAS8, RASC is divided into RAS9-RAS12, and RASD is divided into RAS13-RAS16. So, for example, if AR9 goes high and AC9 is a low, the signal RASC goes high. Then, if both AR8 and AC8 go high, RAS12 goes high and accesses its associated DRAM, thereby leaving RAS1-RAS11 and RAS13-RAS16 unselected and the 15 DRAMs corresponding to those RAS lines in a power-conserving standby mode.
Write-per-bit mode is an industry standard on DRAMs having multiple DQ's. A DRAM with multiple DQ's can be written to in either a normal write mode or in write-per-bit mode. When a DRAM with more than one DQ is in a normal write mode, the number of bits corresponding to the number of DQ's are written at the same time. On a x16 device (a device having 16 subarrays) for example, the chip logic begins writing one bit of data onto each of the 16 DQ's at the falling edge of CAS or WE (whichever is later) as long as RAS is low. (During a normal write, the status of WE is a "don't care" when RAS initially goes low.) The address signals, RAS, and CAS then toggle to select the proper address to be written to, and the desired data is input through the Data In (Din) signals.
During a write-per-bit (also called a "masked write"), any combination (or even all) of the 16 bits can be written to without writing to any of the other locations. To set up a write-per-bit signal, WE goes low. Next, the data for the "mask" is set on the DQ's, with a logic 1 corresponding to "write" and a logic 0 corresponding to a "don't write" (the mask data simply indicates which of the locations are to be written, and which are to be left unaltered). After the data for the mask is set, RAS drops, and the mask information on the data lines is changed to the desired data to be written to the selected locations. Finally, when CAS is pulled low, the write begins. The address signals, RAS, and CAS toggle to input the data into the correct addresses.
As can be seen from the information above, users of memory modules which contain x1 DRAMS which don't use write-per-bit mode may consider WE a "don't care" as RAS goes low, and allow WE to toggle. Depending on the state of the other signals, the unwary user may put the module containing DRAMs with multiple DQ's into write-per-bit mode (which, as previously stated, occurs at the DRAM level if RAS goes low when WE is low). The simple circuit of FIG. 3, if incorporated into the decode circuitry of the module or into the design of the electronic device using the inventive module, will make the WE signal a don't care except when RAS is low, thereby preventing the chips on the modules from entering write-per-bit mode. The circuit incorporates a three input NAND gate 10. RAS, WE, and a RAS signal delayed by the three NAND gates 12, 14, 16 as shown in FIG. 3 are inverted, input to the NAND gate 10, and outputs as WE(out). (Note that three NAND gates is not an absolute--the number of NAND gates is determined only by the delay required to ensure that WE does not go low until after RAS goes low). The truth table for the circuit of FIG. 3 is shown in FIG. 6.
A jumper, electronic switch, or a functional equivalent 18 incorporated into the circuit would allow users who desire the write-per-bit mode to disable the circuit, thereby enabling write-per-bit mode to the DRAMs.
While a preferred embodiment of the invention has been disclosed, various modes of carrying out the principles described herein are contemplated as being within the scope of the following claims. Any memory array comprising RAMs (SRAMs, DRAMs, etc.) having multiple DQ's could have a power savings by using the invention. For instance, in 1 MB module comprising eight 256K×4 RAMs, all eight DRAMs are turned on for each read, even though the 16 bits of data are received from only four of the DRAMs. The description of the invention could be easily modified by those skilled in the art for a x4 module.
In addition, modules with data widths other than those which are a multiple of four are possible with the addition of another device, such as a x1 device. For example, a x17 module is possible on a module containing 64K×16 devices with the addition of a 64K×1 device. Note that this device would require another RAS line, but would use the common CAS signal, and at least two devices would be turned on simultaneously to access the 17 bits of data required, one x16 DRAM for the 16 data bits, and the x1 device for the parity bit.
Finally, the described invention does not pertain only to memory supplied in module form. The invention would work equally well with memory placed directly on the motherboard (embedded memory) or with any other memory addressed by the computer.
It is therefore understood that the scope of the invention is not to be limited except as otherwise set forth in the claims.
|
A method for accessing a memory array for an electronic device comprises a design which requires fewer memory devices to be activated to access a plurality of data bits, thereby reducing the amount of power required to access the data bits. The design comprises the use of a plurality of memory devices, each of which has a plurality of arrays and data out lines.
| 6
|
FIELD OF THE INVENTION
The invention relates to a batch mixer and, more particularly, to a batch mixer equipped with a plunger for pushing material from the batch mixer.
BACKGROUND OF THE INVENTION
Several techniques are available to process polymers, including twin screw extruders and batch mixers. Batch mixers provide for increased residence time of polymeric materials, which improves shearing history of the polymeric materials.
Batch mixers, such as a Banbury® mixer, are known in the art of mixing polymeric materials. These batch mixers have several shortcomings, however. For example, in known batch mixers, after blending or mixing of the material is complete, the mixers are opened and the polymeric materials are manually scooped out from the mixer. This is done with the material in a molten state. This process is time consuming, expensive and complicated. When the polymeric material is solidified as a molten chunk, the polymeric material may be put in a crusher to form polymer granules. However, this form of materials cannot be pelletized.
Accordingly, there exists a need in the art to overcome the deficiencies and limitations described hereinabove.
SUMMARY OF THE INVENTION
In a first aspect of the invention, a batch mixer comprises a mixer tank structured to accommodate material. The mixer further comprises a mixer head comprising at least one blade structured to blend the material within the mixer tank. The mixer further comprises a plunger mechanism structured to push the blended material directly from the mixer tank.
In another aspect of the invention, a batch mixer comprises a mixer tank having an interior portion structured to accommodate polymeric material. The mixer further comprises a mixer structured to blend the polymeric material within the interior portion of the mixer tank. The mixer is rotatable and moveable in a vertical direction along a shaft. The mixer further comprises a plunger mechanism structured to push the blended polymeric material through a die in fluid communication with the interior portion of the mixer tank. The plunger mechanism is rotatable and moveable in the vertical direction along the shaft. The mixer further comprises a plurality of limiters structured to limit the vertical movement of the plunger mechanism and the mixer.
In yet another aspect of the invention, a method of mixing material comprises: placing material within a tank; placing a mixing head on the tank, and mixing the material within the tank with the mixing head; removing the mixing head from the tank; placing a plunger mechanism on the tank; moving the plunger mechanism within the tank to push the mixed material from a die; and removing the plunger mechanism from the tank.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is described in the detailed description which follows, in reference to the noted plurality of drawings by way of non-limiting examples of exemplary embodiments of the present invention.
FIG. 1 shows a batch mixer according to aspects of the present invention;
FIG. 2 shows the batch mixer with a mixer head on a mixer tank according to aspects of the present invention;
FIG. 3 shows the batch mixer with a plunger head on the mixer tank according to aspects of the present invention;
FIG. 4 shows material being pushed from the batch mixer according to aspects of the present invention; and
FIG. 5 shows material being formed into pellets according to aspects of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention relates to a batch mixer and, more particularly, to a batch mixer equipped with a plunger for pushing material from the batch mixer. More specifically, in embodiments, the batch mixer includes a plunger mechanism to push material through a die of a mixer tank. Advantageously, the present invention provides for semi-continuous operation while controlling the residence time of a mixing and compounding process of, e.g., polymeric materials. Accordingly, polymeric materials may be easily and efficiently discharged from the batch mixer and fabricated into desired pellet shapes. As such, the present invention provides for a more cost-effective removal of polymeric materials from the batch mixer.
In the area of polymer processing, mixing and blending, whether in solution or molten form, of different polymers with each other and blending them with organic and/or inorganic fillers and additives is important. The quality of mixing, blending, and compounding of polymeric materials, e.g., plastics, determines the properties of the final product. The benefit of using batch mixers over conventional systems, e.g., twin screw extruders, is that the residence time is higher in batch mixers such that shearing history of the polymeric material is considerably improved.
Advantageously, the batch mixer of the present invention is capable of pushing material, e.g., polymeric material or food products, from the batch mixer, using a plunger mechanism. This avoids the shortcomings of known mixers, which require the user to open the mixer and manually scoop out the material, e.g., polymeric material, from the mixer, in a molten state (which is a time consuming and costly process). Thus, compared to conventional systems, in the batch mixer of the present invention, processed material, e.g., polymeric material or food products, may be easily and efficiently drawn out of the mixer and fabricated to a desired shape using a plunger and die system. Also, advantageously, the material exiting from the die may automatically be guided through a water bath to a pellitizer to obtain material in pellet form. The batch mixer is also equipped with an opening to introduce inert or purging gas into the batch mixer and/or to suck air out of the batch mixer, thus allowing the batch mixer to operate under vacuum.
In embodiments, the material may be related to the research and development of food products. Many food products undergo a mixing process in order to achieve characteristics such as texture, homogeneity, composition and temperature. In embodiments, food mixing can include nano-emulsions, large particle suspensions, highly viscous pastes, or dry powders, with or without the incorporation of gas. In embodiments, the mixing may be: solid-solid mixing, such as powders or textural effects; liquid-solid mixing, such as butters, pastes and dough; liquid-liquid mixing, such as emulsions, margarines, and spreads; or gas-liquid mixing, such as fermentation or chlorination. Accordingly, mixing and blending of food products with additives, flavorings, texture, and other fillers is provided herein. In embodiments, the production of food pellets and flakes such as cereals, pastas, and candies require longer mixing times. As such, the present invention may be of great help to food research and development and food product mixing.
FIG. 1 shows a batch mixer according to aspects of the present invention. More specifically, FIG. 1 shows a batch mixer 1 having mixer tank 5 supported on support bases 15 a , 15 b by support bars 10 a , 10 b , respectively. It should be understood by those of skill in the art that any number of support bars and support bases are contemplated by the present invention. In embodiments, the mixer tank 5 has a diameter of about 10 cm and a height of about 20 cm; although other dimensions are contemplated by the present invention. The mixer tank 5 includes an interior portion that accommodates material, e.g., mixing, blending, and compounding, whether in solution or molten form, different polymers with each other and blending them with organic and/or inorganic fillers and additives.
The mixer tank 5 also includes a die 20 in fluid communication with the interior portion. The die 20 is structured to discharge materials from the interior portion of the mixer tank 5 , as discussed below. A valve 22 is provided for controlling the flow rate of the material being discharged through the die 20 . In embodiments, the die 20 can be customized to any desired shape such as a slit, annular, etc.
In embodiments, the mixer tank 5 further includes an opening 25 (e.g., pipe in fluid communication with an interior of the mixer tank) which can be used to introduce an inert or purging gas into the mixer tank 5 to prevent undesired chemical reactions from taking place within the mixer tank 5 . In alternate embodiments, the opening 25 is used to remove air or other gases from the mixer tank 5 , thus creating a vacuum.
As further shown in FIG. 1 , the batch mixer 1 includes a mixer head 29 . The mixer head 29 includes a cover 30 , and one or more mixer blades 35 which are operable by a high-torque motor 45 . In embodiments, the high-torque motor 45 is connected to the one or more mixer blades 35 by a shaft 40 , in order to rotate the one or more mixer blades 35 . In this way, the high-torque motor 45 drives the shaft 40 thereby causing the one or more mixer blades 35 to mix and blend the materials, e.g., molten polymer blends and compounds or food products, within the mixer tank 5 . The one or more mixer blades 35 may be of different shapes and designs to ensure well mixed and/or blended materials. For example, the one or more mixer blades 35 can be paddle blades. In embodiments, the mixer blades 35 can also be gyrated in a rotational or partial rotational manner, as well as configurations which act as a vertical chopping.
Still referring to FIG. 1 , the batch mixer 1 further includes a plunger head 49 . The plunger head 49 includes a plunger 50 attached to a screw driven shaft 55 . In embodiments, the screw driven shaft 55 is connected to a motor 60 in order to lower and raise the plunger 50 , when in the mixer tank 5 . In this way, in operation, the plunger 50 can discharge materials from the mixer tank 5 , through the die 20 . The plunger 50 is preferably made of stiff and thermal stable materials capable of withstanding temperatures up to about 300° C., while being able to push molten materials through the die 20 .
In embodiments, the mixer head 29 and plunger head 49 are rotatably attached to a shaft 65 using an arm 70 a and an arm 70 b , respectively. Specifically, the mixer head 29 is connected to (mounted to) and spaced from the shaft 65 by the arm 70 a extending between the shaft 65 and the mixer head 29 , and the plunger head 49 is connected to (mounted to) and spaced from the shaft 65 by the arm 70 b extending between the shaft 65 and the plunger head 49 . In embodiments, the arms 70 a , 70 b are rotated manually; however, in alternate embodiments, the arms 70 a , 70 b can be rotated automatically using a motor 75 . In further embodiments, the mixer head 29 and plunger head 49 move vertically along the shaft 65 . Specifically, both the mixer head 29 and the plunger head 49 are rotatably mounted to the shaft 65 and moveable relative to the shaft and along a length of the shaft. Similar to the rotational movement of the arms 70 a , 70 b , in embodiments, the vertical movement of the arms 70 a , 70 b may be performed either manually or automatically. The vertical movement of the arms 70 a , 70 b is limited by the pins 75 a - 75 c (e.g., mechanical structures or limiters). The pins 75 a - 75 c can also lock the arms 70 a , 70 b to the shaft 65 at certain operational positions. In alternate embodiments, other pins or other locking mechanisms are contemplated by the present invention.
More specifically, the pins 75 a and 75 b limit the movement of the mixer head 29 , in the vertical direction; whereas, the pins 75 b and 75 c limit the movement of the plunger head 49 , in the vertical direction. In embodiments, the pins 75 a - 75 c can also lock the mixer head 29 and plunger head 49 at certain operational positions along the shaft 65 . In particular, the pin 75 a can lock the mixer head 29 in the raised position, and the pin 75 b can lock the mixer head 29 in a lower position (i.e., when the mixer head 29 is sealed to the mixer tank 5 ). Similarly, the pin 75 c can lock the plunger head 49 in the lower position, and the pin 75 b can lock the plunger head 49 in a raised position (i.e., when the plunger head 49 is sealed to the mixer tank 5 ). As one of skill in the art should recognize, in embodiments, the plunger head 49 is located in the raised position (sealed to the mixer tank 5 ), while the mixer head 29 is in the raised position (remote from the mixer tank); whereas the mixer head 29 is in the lowered position (sealed to the mixer tank 5 ), while the plunger head 49 is in the lowered position (remote from the mixer tank). It should be understood by those of skill in the art, that the plunger head 49 and the mixer head 29 can also be arranged vice versa, depending on the configuration of the batch mixer, e.g., the plunger head 49 can be arranged above the mixer head 29 .
FIG. 2 shows the batch mixer with the mixer head sealed on the mixer tank according to aspects of the present invention. More specifically, in FIG. 2 , the cover 30 is placed on the mixer tank 5 with the one or more mixer blades 35 inserted in the mixing tank 5 . In this operational position, the arm 70 a is locked onto the shaft 65 by the pin 75 b , and the mixer blades 35 are moved (e.g., rotated) by the high-torque motor 45 . FIG. 2 further shows the plunger head 49 in the lowered position, with the arm 70 b , in embodiments, locked to the shaft 65 by the pin 75 c . Alternatively, the arm 70 b can rest on the pin 75 c.
FIG. 3 shows the batch mixer with the plunger head sealed on the mixer tank according to aspects of the present invention. More specifically, in FIG. 3 , the plunger head 49 is in the raised position, sealed on the mixer tank 5 . In this operational position, the arm 70 b is in the raised position, and locked to the shaft 65 by the pin 75 b . Also, in this operational position, after the materials in the mixer tank 5 have had a sufficiently high residence time within the mixer tank 5 , the plunger 50 will begin to discharge the material through the die 20 of the mixer tank 5 . The flow rate of the material can be based on the valve setting 22 , as well as the force applied by the plunger 50 . As should be understood by those of skill in the art, the residence time of the materials will vary in accordance with the nature of the blending and compounding process.
FIG. 4 shows material being pushed from the batch mixer according to aspects of the present invention. In this operational stage of FIG. 4 , the motor 60 will supply power to the plunger 50 in order to push material through the die 20 . More specifically, in embodiments, the plunger 50 is sealed on the mixer tank 5 and the motor 60 supplies power to the screw driven shaft 55 to lower the plunger 50 within the mixer tank 5 . In this way, the plunger 50 forces material 80 through the die 20 of the mixer tank 5 . In embodiments, the plunger 50 is a screw type plunger; however, it should be understood by those of skill in the art that other types of plungers are contemplated by the present invention.
FIG. 5 shows material 80 being discharged from the die 20 of the mixer tank 5 and guided through a water bath 85 . The water bath 85 is used to maintain a stable temperature of the material 80 . FIG. 5 further shows the material 80 guided through a pellitizer 90 , which produces pellets 95 of different sizes and with different mechanical properties depending on the desired pellet type. In embodiments, the pelletizer 90 uses both mechanical force and thermal processes to produce the desired pellet properties. As a result, the discharged material 80 is transformed into pellets 95 .
As thus should now be understood, a method of mixing and blending material, e.g., polymeric material and/or food products, can be achieved with the batch mixer of the present invention. For example, material is placed within the mixer tank 5 , and the mixing head 29 is placed on the mixer tank 5 . The mixing head 29 is activated, and more specifically, the one or more mixer blades begin to mix the material within the mixing tank 5 . Once a desired residence time is achieved, the mixing head 29 is removed from the mixing tank 5 . For example, the mixing head 29 can be lifted in a vertical direction, and rotated away from the mixing tank. The mixing head 29 can be locked into place by a pin or other equivalent locking mechanism. Thereafter, the plunger head 49 is placed on the mixing tank, by moving it in the vertical direction and rotating it to align with the mixing tank 5 . The plunger mechanism, e.g., screw plunger, is activated in order to discharge the mixed material from the die 20 . The valve 22 can be adjusted in order to adjust the flow rate of the mixed material. The plunger mechanism can then be removed from the mixing tank 5 .
The foregoing examples have been provided for the purpose of explanation and should not be construed as limiting the present invention. While the present invention has been described with reference to an exemplary embodiment, changes may be made, within the purview of the appended claims, without departing from the scope and spirit of the present invention in its aspects. Also, although the present invention has been described herein with reference to particular materials and embodiments, the present invention is not intended to be limited to the particulars disclosed herein; rather, the present invention extends to all functionally equivalent structures, methods and uses, such as are within the scope of the appended claims.
|
A batch mixer is equipped with a plunger for pushing material from the batch mixer. The batch mixer includes a mixer tank structured to accommodate material. The mixer further includes a mixer head comprising at least one blade structured to blend the material within the mixer tank. The mixer further includes a plunger mechanism structured to push the blended material directly from the mixer tank.
| 1
|
FIELD OF THE INVENTION
This invention relates to a packaging tray which includes a divider for separating rows of articles. More particularly, it relates to a packaging tray of this type adapted to be formed from a paperboard blank.
BACKGROUND OF THE INVENTION
In the packaging of fragile food products, such as cookies, molded plastic trays incorporated in an outer bag have been used to support the cookies. The trays typically contain a center divider spaced from the side panels. Both the dividers and the side panels have sloped walls which form channels or troughs on either side of the divider in which rows of cookies are supported.
Such trays have a number of drawbacks. Although the plastic molding operation allows them to readily take any desired shape, the trays have to be shipped in molded form to the packaging plant. Even when nested, the number of trays which can be shipped in a truckload is limited, resulting on overall higher shipping costs than desired. In addition, the cost of the resin used in forming the trays has increased significantly and can be expected to continue to increase, which will make the use of plastic trays impractical from a cost standpoint at some point in the future. Separate from cost considerations is the threat of legislation against the packaging of food products in certain types of plastics due to the possible absorption into the food of gases released from the plastic material.
It would be highly desirable to be able to substitute paperboard trays for the plastic trays now in use in order to overcome the possible health threat and to reduce the cost of the trays. Ideally, such trays would be formed from paperboard blanks capable of being shipped to the packaging location in flat condition, which would enable a great many more trays to be produced from a single truckload. The problem, however, is to design a paperboard tray which can be readily and rapidly formed from a single flat sheet of minimal size and which has the desired final shape.
SUMMARY OF THE INVENTION
In accordance with the invention, a paperboard tray is provided which is comprised of spaced bottom panel portions connected by fold lines to end panels, to side panels and to divider means. Sloped walls of the divider means form obtuse angles with the bottom planel portions. The portions of the tray between the divider means and the side panels comprises channel means adapted to receive and support rows of articles. Preferably, the side panels also contain sloped wall portions so that the sloped walls of both the divider means and the side panels are adapted to support substantially flat rounded-edge articles such as cookies.
To enable a tray to be formed from a flat blank the end panels are comprised of overlapping flaps which are connected to the bottom panel sections by fold lines but which are basically unconnected to the divider walls. This allows the divider walls to be folded into place without interference from the end flaps. At one location, however, means are provided between a portion of a divider wall and an outer end panel flap to properly position the inner flap to allow the divider walls to be folded up to form the divider. In a preferred embodiment such means takes the form of a web which extends from an adjacent end edge of an adjacent divider wall into the outer end flap. By connecting the web to the divider wall along one fold line and to the outer end flap along a second fold line, the end flaps are automatically placed in proper relative positions during the forming of the tray from the blank. This enables the tray to be quickly and accurately formed even though a divider must be created during the folding process from connected portions of the blank.
The blank is inexpensive yet capable of being readily formed into a tray of the desired shape and dimensions.
Other features and aspects of the invention, as well as other benefits thereof, will readily be ascertained from the more detailed description of the invention which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a pictorial view of the packaging tray of the invention;
FIG. 2 is a plan view of the inside surface of a blank for forming the tray of FIG. 1;
FIG. 3 is an enlarged plan view of a portion of the blank of FIG. 2;
FIG. 4 is a plan view of the blank of FIG. 2 after it has been subjected to an initial folding step;
FIG. 5A is an enlarged pictorial view of a portion of the blank of FIG. 2 during the initial folding step;
FIG. 5B is an enlarged pictorial view of the same portion of the blank of FIG. 2 after the initial folding step;
FIG. 6 is a plan view of the tray of FIG. 1;
FIG. 7 is a transverse sectional view taken along line 7--7 of FIG. 6;
FIG. 8 is an end elevation of the tray of FIG. 1; and
FIG. 9 is a side elevation of the tray of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, the packaging tray 10 of the present invention comprises bottom panel portions 12 and 14 separated by a center divider 16. The center divider comprises sloping walls 18 and 20 connected at their uppermost point along a fold line 22 which extends parallel to the side panels 24 and 26. The side panel 24 consists of an upper vertical portion 28 and a lower sloped portion 30. Similarly, the side panel 26 consists of an upper vertical portion 32 and a lower sloped portion 34. Although the final shape and dimensions of the tray are dependent upon the shape and size of the articles to be packaged, in many cases the angle formed by the sloped side panel portions 30 and 34 with the adjacent bottom panel portions 14 and 12 will be the same as the angle formed by the sloped walls 20 and 18 with the bottom panel portions. Thus fragile articles such as cookies A, illustrated in FIG. 1 in dotted outline, will be supported along their circumference just below their midpoint by the sloped walls of the side panels and divider. If desired, the dimensions may be made so that the cookies are also supported at their lowermost edges by the bottom panels. Completing the construction of the tray 10 are end panels 36 and 38. Additional details of the tray construction will be discussed later.
Referring now to FIG. 2, a blank 40 to be used in forming the tray of FIG. 1 has various sections identified by reference numerals corresponding to those employed in identifying the elements of the tray. Side panel section 32, which becomes the vertical panel portion in the erected tray, is connected by fold line 42 to side panel section 34, which becomes the sloped wall portion in the erected tray. A similar arrangement exists at the opposite end of the blank wherein side panel sections 28 and 30 are connected to each other by fold line 44. The blank side panel sections 34 and 30 are connected by fold lines 46 and 48, respectively, to bottom panel sections 12 and 14, which in turn are connected by fold lines 50 and 52, respectively, to the divider wall sections 18 and 20. The divider wall sections are connected together along fold line 22. The ends of the side panel sections 28 and 32 are connected to glue tabs 29 and 31, respectively, by fold lines 33 and 35.
Still referring to FIG. 2, the end panel sections 36 and 38 are comprised of separate flaps intended to overlap each other in the tray. Thus inner flaps 54 and 56 are separated from outer flaps 58 and 60, respectively, by slits 62 and 64 which are aligned with the fold line 22. Inner flaps 54 and 56 are connected to the bottom panel section 14 along end fold lines 66 and 68, respectively, and outer flaps 58 and 60 are connected to the bottom panel section 12 along end fold lines 70 and 72, respectively. The inner end panel flaps 54 and 56 are not connected to the adjacent divider wall portion 20, but instead are separated from it by slits 74 and 76. In like manner the outer end panel flaps 58 and 60 are separated from the adjacent divider wall portion 18 by slits 78 and 80. The slits 78 and 80, however, do not extend along the entire width of the divider wall section 18 as the slits 74 and 76 do in connection with divider wall section 20. Instead, divider wall section 18 is connected adjacent one corner to the flaps 58 and 60 by webs 82 and 84.
As shown more clearly in FIG. 3, which is an enlarged view of the portion of the blank containing the web 84, it will be seen that the web is connected to the divider panel section 18 by fold line 86 and to the outer end panel flap 60 by the fold line 88. The web is separated from the flap 60 between the fold lines 86 and 88 by the connecting slit 90.
Referring back to FIG. 2, the first step in forming a tray from the blank 40 is to apply adhesive to the stippled areas 92 and 94 of the outer end panel flaps 58 and 60, the stippled areas extending from the edges of the flaps at slits 62 and 64 to a point aligned with the fold line 50. Then the side panel sections 28 and 32 are moved toward each other so that the divider walls 18 and 20 fold up about the fold lines 50 and 52, causing the inner end flaps 54, 56 and the outer end flaps 58, 60 to move toward each other due to their being connected to the bottom panel sections 12 and 14. The inner end flaps 54 and 56 as a result slide over the stippled area 92 and 94 of outer end flaps 58 and 60 until they reach the position shown in FIG. 4. In this position the interior edges of the inner end panel flaps 54 and 56 are substantially aligned with the fold line 50 and the interior edges of the outer flaps 58 and 60, shown in dotted lines, are substantially aligned with the fold line 52.
This action is illustrated more clearly in FIG. 5A, which shows the blank at an intermediate stage of the relative sliding movement between the flaps 56 and 60. The upward bending of the divider wall sections 18 and 20 about the fold lines 50 and 52 and the resulting relative downward folding movement of the sections 18 and 20 about central fold line 22 can be seen. Because the web 84 is attached to the divider wall section 18 by fold line 86, upward movement of the section 18 lifts the web 84 out of the plane of the end flap 60. By this action the web folds upwardly about the fold line 88, causing the edges forming the slit 90 to separate. The separation of these edges and the connection of the web 84 at fold line 88 form a pocket into which the leading interior corner area 96 of the inner flap 56 can move.
Continued upward folding of the divider section walls 18 and 20 causes continued relative sliding movement between the flaps 56 and 60 until movement is stopped by the leading edge of the flap corner area 96 encountering the inside face of the web 84 adjacent the fold line 88. This condition is shown in FIG. 5B, which corresponds to the condition of the blank illustrated in FIG. 4. The desired angle of the divider walls is thereby determined by the automatic stopping of further movement of the flap 56, which prevents further folding of the divider walls 18 and 20 and allows the angle reached by the divider walls at the time the web is contacted to be maintained. The same action is of course occurring at the web 82 to stop movement of the flap 54. Although webs are not necessarily required on both sides of the blank in order to stop further sliding movement of both flaps 54 and 56, it is preferred that both be provided in order to prevent any misalignment of the flaps and the possible resulting tilting or skewing of the divider.
Referring back to FIG. 4, the next step in the fabrication of the tray is to apply adhesive to the glue tabs 29 and 31 as shown by the stippling. The connected flaps 54 and 58 and the connected flaps 56 and 60 are then folded up along fold lines 66, 70 and 68, 72, respectively, after which the side panels 32, 34, 28 and 30 are folded upwardly about their fold lines 42, 46, 44 and 48. This folding action continues until the side panel sections 32 and 28 are in a vertical position so that the glue tabs can be folded over the adjacent end wall flaps 54, 56, 58 and 60. This results in the blank being formed into the final tray shape shown in FIG. 6.
As shown in FIGS. 6, 7, 8 and 9, as well as FIG. 1, the resulting tray is held in place simply by the adhered overlapping end flaps and by the glue tabs extending from the side panel sections 28 and 32. Just as the automatic positioning of the inner and outer end flaps with respect to each other determines the final angle which the divider walls 18 and 20 form with the bottom panel portions 12 and 14, the upward folding of the upper side panel sections 28 and 32 to the vertical determines the angle formed by the sloped side panel portions 30 and 34 with the bottom panel portions. By proper selection of dimensions, these angles can be varied as dictated by the shape of the product to be supported, and can be made equal to each other.
It is to be understood that although the term "fold line" has been used in connection with all of the lines in the blank along which the paperboard is intended to be folded, some of the fold lines may be made more pliable and easier to fold about than others. For example, the fold lines 22, 50 and 52 should preferably be easier to fold than the other parallel fold lines in the main body of the blank so that when forces are exerted on the blank to cause relative sliding movement of the end flaps, these fold lines will yield and allow the formation of the center divider. Accordingly, it may be desirable to form the fold lines 42, 44, 46 and 48 from relatively stiff score lines rather than relatively yielding fold lines.
Although the tray has been described as being held in place by glued connections, it will be understood that mechanical locks could be utilized instead. Glued connections are preferred, however, because they allow a smoother, sleeker appearance uninterrupted by bulky mechanical locks, and they also allow speedier assembly of the trays. Moreover, trays formed from glued connections are not as likely to come apart or tear due to excessive handling or shipping stresses as are trays formed with mechanical locks.
It will now be appreciated that the tray of the present invention is simple to form from the disclosed blank and that it will function to suitably support fragile articles such as cookies. The angled walls of the center divider and the sloped portions of the side panels support the articles along substantial portions of their circumference, while the vertical end panels and the vertical portions of the side panels protect the rows of articles against forces coming from the side or end of the package.
It should also be understood that the invention is not necessarily limited to all the specific details described in connection with the preferred embodiment, but that changes to certain features of the preferred embodiment which do not affect the overall basic function and concept of the invention may be made by those skilled in the art without departing from the spirit and scope of the invention, as defined in the appended claims.
|
A paperboard tray for holding spaced rows of flat articles. A divider separating the rows includes sloped walls which, along with sloped wall portions in the side panels of the tray, serve to support the articles. A web connecting an outer end flap to a divider wall acts as a stop member to automatically position the end of the inner end flap as the overlapping flaps are moved into position during the formation of the tray from a blank.
| 1
|
FIELD OF THE INVENTION
[0001] The invention relates to garment steamers, particularly, relates to garment steamers with inclinable ironing board.
BACKGROUND OF THE INVENTION
[0002] Conventional garment steamer offers a convenient way of removing wrinkles. However when compared to conventional ironing method, the level of wrinkle removal performance is much lower since there is nothing to support the hanged garment. Tough wrinkles cannot be pressed out like in the process of conventional ironing method which uses a horizontal board to support the garment.
[0003] Referring to FIG. 1 , a garment steamer 200 is introduced trying to solve the above problem. The stand garment steamer 200 comprises a fixed vertical ironing board 210 for steaming. However, such vertical ironing board 210 is not ergonomic and difficult to use, users have to operate in vertical direction, which is not comfortable. Furthermore, such vertical ironing board 210 is very unstable, when exerting force onto the ironing board 210 , it tends to fall over. Therefore, this type of garment steamer cannot really support any significant pressing force for removing wrinkles.
[0004] An ironing board for multifunctional use is known from U.S. 2010/0095565. This document discloses an ironing board having a base and a body with a work surface which is connected to the base by a column. The column has a tilting means for tilting the body about a tilting axis which extends perpendicularly to the column.
OBJECT AND SUMMARY OF THE INVENTION
[0005] It is an object of the invention to propose a stable and compact garment steamer with inclinable ironing board which can be inclined relative to its support structure.
[0006] The invention is defined by the independent claims. The dependent claims define advantageous embodiments.
[0007] According to the present invention, a garment steamer with inclinable ironing board is provided, the garment steamer comprises a base and a support structure extending upwardly from the base, the support structure comprises an upper part and a lower part, an ironing board is attached to the upper part, an inclining structure comprising an inclining linkage that connects the upper part and the lower part in such a way that the upper part is inclinable relative to the lower part and can be fixed in a position in which the upper part is inclined from the lower part at an angle between horizontal and vertical, wherein the inclining linkage comprises first and second link arms extending side-by-side between the upper and lower parts of the support structure, each of the first and second link arms having an upper end pivotably connected to the upper part and a lower end pivotably connected to the lower part, the first link arm being longer than the second link arm such that upper part assumes an inclined position relative to the lower part when the upper and lower ends of the link arms are pivoted about the upper and lower parts, respectively, of the support structure.
[0008] Preferably, the incline angle is between 15 to 45 degrees relative to vertical direction, and a support structure extends upwardly from both sides of the base. The inclining structure may be part of the support structure.
[0009] According to a first embodiment of the present invention, the first inclining linkage comprises a top link rigidly connected to the upper part of the support structure; a bottom link rigidly connected to the lower part of the support structure; wherein the upper ends of the first and second link arms are pivotably connected to the top link and the lower ends of the first and second link arms are pivotally connected to the bottom link.
[0000] In a preferred embodiment, the garment steamer comprises a sleeve mounted to the support structure and slidable between a first position in which it encloses the first and second link arms to hold the first and second link arms in a first position in which the upper and lower ends of the link arms are free to pivot about the upper and lower parts, respectively, of the support structure. The incline angle may be determined by the difference in length of the first and second link arms. Preferably, the top link is part of the upper part of the support structure, and the bottom link is part of the lower part of the support structure.
[0010] According to a second embodiment of the present invention, there is provided a garment steamer with inclinable ironing board comprising a base, a support structures extending upwardly from the base, the support structure comprising an upper part and a lower part, an ironing board attached to the upper part, an inclining structure, comprising an inclining linkage, connecting the upper part and the lower part in such a way that the upper part is inclinable relative to the lower part and can be fixed in a position in which the upper part is inclined from the lower part at an angle between horizontal and vertical, wherein the inclining linkage comprises: an upper link pivotably connected to an lower link, the lower link comprising a rounded end and a plurality of recesses radially defined in the rounded end; and a spring loaded plunger arranged inside the upper link, and biased against the rounded end of the lower link such that when the plunger is aligned to one of the recesses, it locates in said recess to lock the upper link in an inclined position relative to the lower link.
[0000] The upper link may be integral with, or rigidly connected to, the upper part of the support structure. The lower link may be integral with, or rigidly connected to, the lower part of the support structure.
The incline angle may be determined by the angle between the recess and the vertical direction. In one embodiment, a spring housing is secured inside the upper link, the plunger extends through the spring housing, a spring is housed in the spring housing and arranged between an inner face of the spring housing and a shoulder on the plunger in order to exert a spring force on the plunger.
[0011] By the inclining structure of the present invention, the ironing board of the garment steamer can be inclined relative to the lower part of the support structure so that users can operate the steamer comfortably. The incline angle can be fixed by employing the first inclining linkage, and alternatively the incline angle can be adjustable by employing the second inclining linkage. The support structure of the garment steamer with inclinable ironing board can be implemented as a pair of support poles which extends upwardly from both sides of the base, which enable the steamer to stand stably when force is exerted on the ironing board. A selected sized board can also strengthen the stability of the steamer. The support structure is preferably implemented as retractable structure, when not in used, the inclining structure together with the support structure can be retracted in order to save storage space.
[0012] Detailed explanations and other aspects of the invention will be given below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Particular aspects of the invention will now be explained with reference to the embodiments described hereinafter and considered in connection with the accompanying drawings, in which identical parts or sub-steps are designated in the same manner:
[0014] FIG. 1 shows a garment steamer with fixed vertical ironing board that is known from a prior art;
[0015] FIG. 2 shows a garment steamer with inclinable ironing board with ironing board which can be inclined via an inclining structure according to the present invention;
[0016] FIG. 3 shows a first embodiment of the inclining structure of the present invention;
[0017] FIG. 4A to 4C show the inclining process of the first inclining linkage shown in FIG. 3 ; and
[0018] FIG. 5A to 5C show a second embodiment of the inclining structure of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0019] To make users feel comfortable when operating the garment steamer, its ironing board need to be ergonomic, which required the ironing board can be inclined to a certain angle.
[0020] Referring to FIG. 2 , the present invention proposes a garment steamer with inclinable ironing board to meet the above requirement. The garment steamer with inclinable ironing board 100 comprises a base 10 . A steam generator 20 is attached to or separately positioned from the base 10 . A steamer head 30 is connected to the steam generator 20 by a steam hose 40 . A support structure 50 extends upwardly from the base 10 , the support structure 50 can be a pole. In a preferred embodiment, there are two poles extends upwardly from both sides of the base 10 , and the poles are preferably retractable which can be retracted when they are not in use in order to make the garment steamer compact. It is understandable that the number of the pole and the position of the pole can be varied depend on its size, the requirement of stability, and other consideration.
[0021] The support structure 50 has an upper part 51 and a lower part 52 . The upper part 51 and lower part 52 are connected via an inclining structure 70 . In a preferred embodiment of the invention, the inclining structure 70 is part of the support structure 50 . In an alternatively embodiment of the invention, the inclining structure 70 is separate component which is attached upper part 51 and lower part 52 of the support structure 50 .
[0022] In a preferred embodiment of the invention, the ironing board 60 is attached to the upper part 52 of the support structure 50 . Therefore the ironing board 60 moves together with the upper part 52 . The inclining structure 70 is connected to the support structure 50 such that the upper part 51 of the support structure 50 is inclined relative to the lower part 52 of support structure 50 and can be fixed in a position in which the upper part 51 is inclined from the lower part 52 at an angle between horizontal and vertical. As a result of being attached to and moving together with the upper part 51 of the support structure 50 , the ironing board 60 is therefore inclined from the lower part 52 of the support structure 50 at an angle between horizontal and vertical. The ironing board 60 can be a full board, or for compact consideration, a half board or a board with a size within the footprint of the base 10 .
[0023] FIG. 3 shows a first embodiment of the inclining structure 70 , which is described here as a first inclining linkage 80 .
[0024] The first inclining linkage 80 comprises a top link 81 , a bottom link 82 , a front link 83 , a rear link 84 , and a sleeve 85 . The upper part 51 of the support structure 50 is rigidly connected to the top link 81 . The lower part 52 of the structure 50 is rigidly connected to the bottom link 82 . In a preferred embodiment, the top link 81 is part of the upper part 51 of the support structure 50 , and the bottom link 52 is part of the lower part 52 of the support structure 50 . In an alternative embodiment, the top link 81 and bottom link 82 are separate components which are rigidly connected respectively to the upper part 51 and lower part 52 .
[0025] The front link 83 and rear link 84 are, respectively, pivotably connected to a lower end of the top link 81 and an upper end of the bottom link 82 . There is a height difference between the ends of the front link 83 and rear link 84 at where they connect the top link 81 or the bottom link 82 . Therefore, when pivoting, the front link 83 and the rear link 84 form a step which defines an incline angle between the top link 81 and bottom link 82 which connect to the front link 83 and rear link 84 respectively. Since the upper part 51 of the support structure 50 is rigidly connected to the top link 81 , and the lower part 52 of the support structure 50 is rigidly connected to the bottom link 82 , the upper part 51 of the support structure 50 is therefore inclined from the lower part 52 of the support structure 50 at a predetermined incline angle defined by said height difference. Furtherly, the ironing board 60 attached to the upper part 51 of the support structure 50 moves together with the upper part 51 and is therefore inclined from the lower part 52 of the support structure 50 at a predetermined incline angle defined by said height difference. By varying the height difference, the incline angle can be varied between horizontal and vertical. A comfortable incline angle for users' steaming operation is commonly from 15 to 45 degrees, preferably 30 degrees.
[0026] The sleeve 85 is arranged slidably enclosing the top link 81 , bottom link 82 , front link 83 and rear link 84 in a vertical position. The overall outside dimension of the top link 81 , bottom link 82 , front link 83 and rear link 84 , when in a vertical position, is smaller than the inner opening of the sleeve 85 . This allows the sleeve 85 to slide up or down along the top link 81 , bottom link 82 , front link 83 and rear link 84 . When the sleeve 85 slides to a first position where it encloses the front link 83 and rear link 84 , the front link 83 and rear link 84 are held substantially in a vertical position without pivoting; when the sleeve 85 slides to a second position where it does not enclose the front link 83 and rear link 84 , that is, the front link 83 and rear link 84 are exposed from the sleeve 85 , the front link 83 and rear link 84 pivot relative to the top link 81 and bottom link 82 so that a step is formed which leads to incline angle between the top link 81 and bottom link 82 , and therefore between the upper part 51 and lower part 52 of the support structure, and further between the ironing board 60 and the lower part 52 of the support structure 50 .
[0027] Preferably, the overall outside size and profile of the sleeve 85 are the same as the support structure 50 , therefore, in the case of the support structure 50 is implemented as retractable pole, it enables the whole first inclining linkage 80 to be refracted together with the retractable pole for a compact storage purpose.
[0028] FIG. 4A to 4C show the inclining process of the first inclining linkage 80 . Referring to FIG. 4A , the sleeve 85 is initially in the first position where it encloses the front link 83 and rear link 84 , in this case, the front link 83 and rear link 84 are held inside the sleeve 85 and cannot pivot, the first inclining linkage 80 is therefore locked in a vertical position. To release the first inclining linkage 80 , the sleeve 85 slides upwardly to the second position where it clears both the front link 82 and rear link 83 . Referring to FIG. 4B , at the second position, the sleeve 85 is slightly pulled towards the front link 83 in order to break the straight line of the first inclining linkage 80 . After which, due to gravity, the weight of the top link 81 , sleeve 85 , upper part 51 of the support structure 50 , and ironing board 60 will actuate the front link 83 and rear link 84 to pivot relative to the top link 81 and bottom link 82 . Referring to FIG. 4C , when the pivoting stops, a step is formed between the front link 83 and the rear link 84 , the top link 81 is therefore inclined to an angle relative to the bottom link 82 .
[0029] To reset the first inclining linkage 80 , the top link 81 is lifted up to a vertical position. Due to the connection between the top link 81 and the front link 83 and rear link 84 , the front link 83 and rear link 84 are pulled up to a vertical position. Due to gravity, the sleeve 85 drops down to a position where it encloses and holds the front link 83 and rear link 84 so as to lock the top link 81 and bottom link 82 in a vertical position without inclining.
[0030] FIG. 5A to 5C shows a second embodiment of the inclining structure 70 , which is described here as a second inclining linkage 90 . The first and second inclining linkages ( 80 , 90 ) may be used together or, they may be used independently.
[0031] The second inclining linkage 90 comprises an upper link 91 and a lower link 92 , the upper link 91 is pivotably connected to the lower link 92 via a pivot 93 . The upper part 51 of the support structure 50 is rigidly connected to the upper link 91 , and the lower part 52 is rigidly connected the lower link 92 . In a preferred embodiment, the upper link 91 is part of the upper part 51 of the support structure 50 , and the lower link 92 is part of the lower part 52 of the support structure 50 . In an alternative embodiment, the upper link 91 and lower link 92 are separate components which are respectively rigidly connected to the upper part 51 and lower part 52 of the support structure 50 .
[0032] The lower link 92 comprises a rounded end 921 which faces the upper link 91 when the lower link 92 is connected to the upper link 91 . A plurality of recesses 922 are radially defined in the rounded end 921 . Inside the upper link 91 , a spring housing 94 is secured at a bottom of the upper link 91 . A plunger 96 extends through the spring housing 94 , one end of the plunger 96 is fixed to a release button 97 arranged on a surface of the upper link 91 , the other end of the plunger 96 rides along the rounded end 921 of the lower link 92 . The plunger 96 comprises a shoulder 961 . A spring 95 is housed in the spring housing 94 , one end abuts against an inner face of the spring housing 94 , and the other end abuts against the shoulder 961 of the plunger 96 .
[0033] When the upper link 91 pivots relative to the lower link 92 , the plunger 96 rides along the rounded end 921 of the lower link 92 , when the plunger 96 is aligned to one of the recesses 922 , the plunger 96 is pushed by the spring 95 to plug into the recess 922 . In this case, the upper link 91 is locked in a position where it is inclined relative to the lower link 92 at an incline angle. Since the upper part 51 of the support structure 50 is rigidly connected to the upper link 91 , and the lower part 52 of the support structure 50 is rigidly connected to the lower link 92 , the upper part 51 of the support structure 50 is therefore inclined from the lower part 52 of the support structure 50 at an incline angle defined by the angle between the recess 922 and vertical direction. Furtherly, the ironing board 60 attached to the upper part 51 of the support structure 50 moves together with the upper part 51 and is therefore inclined from the lower part 52 of the support structure 50 at an angle defined by the angle between the recess 922 and vertical direction. The incline angle can be adjusted by aligning the plunger 96 to different recesses 922 . To reset the upper link 91 and lower link 92 to vertical position, the release button 97 is pushed upward, the spring 95 is therefore compressed, and the plunger 96 is released from the recess 922 . Preferably, a recess 922 is defined in a vertical direction so that when the upper link 91 and lower link 92 is reset to the vertical position, they can be locked by the plunger 96 plugging into this recess 922 .
[0034] The width of the ironing board 50 of the present invention is preferably equal to the width of a hanger of the garment steamer with inclinable ironing board 100 . The length of the ironing board 50 is preferably shorter than or equal to the length of a typical top garment, for example a shirt.
[0035] The above embodiments as described are only illustrative, and not intended to limit the technique approaches of the present invention. Although the present invention is described in details referring to the preferable embodiments, those skilled in the art will understand that the technique approaches of the present invention can be modified or equally displaced without departing from the spirit and scope of the technique approaches of the present invention, which will also fall into the protective scope of the claims of the present invention. In the claims, the word “comprising” does not exclude other elements or steps, and the indefinite article “a” or “an” does not exclude a plurality. Any reference signs in the claims should not be construed as limiting the scope.
|
The invention relates to a garment steamer with inclinable ironing board, which comprises a garment steamer with inclinable ironing board ( 100 ) comprising a base ( 10 ) and a support structure ( 50 ) extending upwardly from the base ( 10 ). The support structure ( 50 ) comprises an upper part ( 51 ) and a lower part ( 52 ) and an ironing board ( 60 ) attached to the upper part ( 51 ). An inclining structure ( 70 ) comprising an inclining linkage ( 80 ) connects the upper part ( 51 ) and the lower part ( 52 ) in such a way that the upper part ( 51 ) is inclinable relative to the lower part ( 52 ) and can be fixed in a position in which the upper part ( 51 ) is inclined from the lower part ( 52 ) at an angle between horizontal and vertical. The inclining linkage ( 80 ) comprises first and second link arms ( 83,84 ) extending side -by-side between the upper and lower parts of the support structure ( 50 ), each of the first and second link arms ( 83,84 ) having an upper end pivotably connected to the upper part ( 51 ) and a lower end pivotably connected to the lower part ( 52 ). The first link arm ( 83 ) is longer than the second link arm ( 84 ) such that upper part ( 51 ) assumes an inclined position relative to the lower part ( 52 ) when the upper and lower ends of the link arms ( 83,84 ) are pivoted about the upper and lower parts ( 51,52 ), respectively, of the support structure ( 50 ).
| 3
|
TECHNICAL FIELD
The present invention pertains to the field of locks. More particularly, the invention concerns a barrel lock assembly with axial pin tumblers and method for changing the combination. Further, the invention conceives such a lock which may be reconfigured converting the assembly to a different lock combination.
BACKGROUND OF THE INVENTION
The present invention concerns locks of the axial pin tumbler type. This form of lock is well known in the art as exemplified by U.S. Pat. Nos. 3,261,188 and 3,258,945. A barrel lock derives its name from the fact that it includes a barrel-like structure disposed within a housing. Typically, the barrel is employed in vending machines and coin operated vending machines. The actuating element often consists of a pivoted lever or latch which toggles between unlocked and locked positions when rotated through a short arc. In the case of coin operated bulk vending machines, the actuating element is a threaded connection between the barrel lock, itself, and a threaded rod.
Referring to U.S. Pat. No. 3,258,945, it describes a conventional barrel lock where the combination, defined by axial pins, can be changed. The patent describes a removable pilot shaft, the position of which is fixed relative to the housing due to the cooperation of a positioning lug in the housing wall and a mating groove on the pilot shaft. With respect to changing the barrel lock combination, it exemplifies the prior art, i.e. the requirement to completely disassemble the tumblers once the pilot shaft is removed to reset the combination.
Often for security reasons, there is a need to change the lock combination of a barrel lock, and in some instances, changing the combination on a regular basis is a matter of management policy. A barrel lock combination is changed by disassembling the lock and replacing the tumblers. The new installed tumbler arrangement has different tumbler pin pairs (split pins) of different lengths and the new split pin tumbler combination provides an assembly having a different pin depth configuration. Accordingly, a new key corresponding to the new depth configuration is required.
Tumbler conversion of conventional barrel locks have the following principal disadvantages. The conversion of the lock combination is complicated, time consuming and troublesome in that a large number of delicate parts must be disassembled, removed and reassembled. Typically, there are many split pin tumblers (four to seven) where each tumbler comprises two pins and a small spring. These pins and springs are small and difficult to manipulate. Consequently, care and accuracy must be exercised to install the tumbler components in their proper plan location according to the new combination to correspond with the new key. In other words, to change the combination, accurate matching of each pin of the upper pin set with its mating pin of the lower set and placement in the barrel lock is required.
Clearly, the great number of small parts greatly increases the likelihood of mishandling and loss. Furthermore, in most assemblies, a number of other parts must also be removed even before achieving access to the tumbler assembly. Thus, yet more parts must be removed, accounted for and replaced.
Another disadvantage related to changing the combination is the need for careful stockpiling of parts (new tumbler sets and corresponding keys). This is inconvenient and increases cost in that the new pins must be ordered, purchased and inventoried. Consequently, not only are part costs increased but also labor costs.
In terms of a functional disadvantage, only the depth-wise configuration of the tumbler assembly can be modified in conventional barrel locks. The planar configuration remains the same.
SUMMARY OF THE INVENTION
It is an object of the present invention to overcome the above-mentioned problems of the prior art and provide an improved barrel lock.
It is another object to furnish a barrel lock assembly which provides a plurality of barrel lock combinations from a single assembly using identical parts.
It is another object to provide a tumbler barrel lock maximizing cost savings and labor efficiency while minimizing parts loss and parts requirements.
It is another object of the present invention to provide a barrel lock which can be modified to realize a new lock combination corresponding to a new key without the need for additional lock components.
According to another object of the invention, a barrel lock is provided which is convertible to a new lock combination through a simple disassembly, retaining the tumbler assembly, and by repositioning only a pilot post.
It is another object to provide a barrel lock in which the planar configuration of the lock combination can be changed.
These and other objects are satisfied by an axial pin tumbler lock comprising:
a tumbler arrangement having a predetermined orientation;
a removable pilot post; and
pilot post adjustment means for enabling assembly of the lock with the pilot post in one of a plurality of possible orientations relative to the tumbler arrangement.
Further objects of the present invention are satisfied by a method for changing a barrel lock combination where the barrel lock features a lock casing, a barrel dimensioned to fit within the casing and having a bore passing therethrough, a plurality of prearranged tumblers housed in the barrel, a removable pilot post extending through the barrel bore, a lock plug for securing the pilot post in the barrel and lock casing, and means for rotationally fixing the pilot post to the barrel in any one of a plurality of predetermined orientations relative to the orientation of the tumbler arrangement, the method comprising the steps of:
a) removing the lock plug from the lock casing,
b) sliding the pilot post through the upper and lower lock barrels,
c) rotating the pilot post relative to the lock barrels,
d) inserting the pilot post into the lock barrels, and
e) securing the lock plug on the lock casing.
For the purpose of the description herein, the following terms are defined:
"Barrel lock" includes a housing, a pilot post, a fixed barrel, and a rotatable barrel disposed end-to-end with the fixed barrel. The bottom barrel rotates relative to the pilot post and top barrel but is fixed to the lock housing. The top barrel is fixed relative to the pilot post but rotates with the pilot post relative to the lock housing. In other words, the definition of "fixed" and "rotatable" derives from the fact that the rotatable barrel, while fixed to the housing, rotates relative to the pilot post while the fixed barrel is rotationally fixed to the pilot post. The respective axial facing barrel ends are referred to as the inside ends while the other ends are denominated outside ends.
"Split pin" tumblers refers to two sets of pins, an upper set and a lower set where each individual tumbler consists of two pins which abut at their inside axial ends when aligned. Each set of tumblers is housed in a corresponding one of the two barrels.
"Socket" refers to the annularly disposed, elongated, axial apertures in the barrels which receive and retain a tumbler. Each tumbler pin is housed in a corresponding socket formed in one of the barrels. In the fixed barrel, each socket extends through the barrel thereby defining two open ends. In the rotatable lower barrel, each socket has one blind end disposed near the outside end of the barrel, and one end opening toward the inside end of the barrel.
"Lock combination" defines the geometry of a key which will actuate the lock. The two basic elements defining the lock combination are the plan configuration and the depth configuration of the tumbler assembly.
"Plan configuration" refers to the number and the planar arrangement or position pattern of the split pin tumblers. This arrangement is assumed in a plane normal to the longitudinal axis of the barrels.
"Depth configuration" refers to the arrangement of different axial lengths of the pins. The predetermined axial position pattern comprising the depth configuration is established because each pin has an axial length predetermined in correspondence to its planar position. Hence, when viewed from the exterior of the lock, the outside ends of the upper pins lay in the same axial plane (a level appearance). This conceals the depth configuration to prevent the lock from being "picked" or actuated improperly by unauthorized personnel.
"Key" indicates a tubular, coded key for a barrel lock which possesses a plurality of tumbler actuating features. These features correspond to and complement the lock combination (tumbler number, planar arrangement, and depth configuration of the tumbler arrangement). The key also includes an alignment keeper, an internal groove and internal lug which dimensionally correspond to a lug and groove in the lock barrel. This alignment feature restricts the key insertion to only one position relative to the barrel lock. Consequently, when the appropriate key is inserted, it engages the upper tumbler pins, depresses the pins such that their inside ends are positioned precisely between the fixed and rotatable barrels, and releases the previously interlocked barrels. Thus, the rotatable barrel is free to rotate.
In essence, the invention, in the four position embodiment described below, permits establishment of four different combinations (requiring four different keys), employing the exact same lock parts and requiring only rotation of the pilot post barrel relative to the lower barrel and, hence, the lock casing. There is no need to remove or change the tumblers.
Given the following enabling description of the drawings, the inventive barrel lock as well as the scope of the invention will become evident to a person of ordinary skill in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a barrel lock according to the present invention.
FIG. 2 is a partial cutaway disassembled side view of the barrel lock.
FIG. 3 is a top view of the barrel lock.
FIG. 4 is a side view of the pilot post with ghost representations of the barrels and a partial cutaway of the tapped cylinder.
FIG. 5 is a cross-sectional view of the lower rotatable barrel.
FIG. 6 is a top view of the lower rotatable barrel.
FIG. 7 is a top view of the lock plug.
FIG. 8 is a top view of the upper fixed barrel.
FIG. 9 is a partial cutaway assembly view of the pilot post, upper fixed and lower rotatable barrels and tumblers.
FIG. 10 is a side view of a tubular key for the barrel lock.
FIG. 11 is a front view of the key tube.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1-3, the barrel lock 10 includes a barrel lock casing 12 including a top flange 11, housing a top barrel 30, a bottom barrel 50, a pilot post 70, and a lock plug 20.
The pilot post 70 is ultimately connected to rotate an actuating element. In this case, representing a coin operated bulk vending machine, the actuating element is a tapped threaded cylinder 78 abutting the outer rotatable barrel surface (see FIG. 4). The threaded cylinder 78 is of a diameter corresponding to the inner diameter of casing 12 and is attached to the pilot post 70 with a rivet or screw. Since the aperture in plug 20 has a smaller diameter than the outer diameter of cylinder 78, cylinder 78 abuts rim 22 of plug 20. Plug 20 is screwed onto a threaded rod secured to the machine base to lock the unit (not depicted). The pilot post 70 is rotationally fixed to top barrel 30. Pilot post 70 and top barrel 30 may rotate freely within the casing 12. The bottom barrel 50 is rotationally fixed to the casing 12.
While the casing 12 can be variously configured, in the preferred embodiment, the casing 12 has generally cylindrical outside and inside walls 14, 16, respectively. The inside wall 16 defines a bore 18 of sufficient diameter to accept the two barrels 30, 50 and cylinder 78. The plug 20 is secured to the bottom of the casing 12 to retain the assembly of the cylinder 78, the two barrels 30, 50, and the pilot post 70 within the bore 18.
The plug 20 is secured by screws mating with holes 23a-23d tapped into the plug. The plug 20 provides a rim 22 abutting the bottom surface of the cylinder 78 in assembly. The rim 22 defines a bore 24 passing through the plug 20. The bore 24 permits passage therethrough of the threaded rod (not depicted) to the cylinder 78.
The bottom barrel 50 is rotationally fixed to the casing 12 with a set screw which passes through hole 17 (it may be desired to use multiple set screws) tapped through the casing 12 and mates with indent or hole 52 a tapped in the barrel 50 (see FIG. 5). Thus, the set screw is accessible from the exterior of the barrel lock casing 12.
Referring to FIGS. 4, 6, and 8, the pilot post 70 is received within central bores 54 and 34 defined in the bottom and top barrels 50 and 30, respectively. The pilot post 70 has four, equicircumferentially spaced lugs 72 and key guide 76. Correspondingly, the barrel bores 54 and 34 define four grooves 56 and 36, respectively, dimensionally matching the lugs 72, 76. (This arrangement is easily reversed, i.e. the pilot post possesses grooves and the barrel bores, lugs.)
To assemble the lock 10, the pilot post 70 is translated axially within the bore 54 of the bottom rotatable barrel with the lugs 72 and lug guide 76 aligned to pass through and beyond the grooves 56. Translation of the pilot post 70 continues into the top (fixed) barrel bore 34. The axial position of pilot post 70 is established with the lugs 72 and key guide 76 received within and engaging the top fixed barrel grooves 36.
The lugs 72, 76 and grooves 36 transmit torque from the pilot post 70 to the top fixed barrel 30, which rotationally fix the pilot post 70 and barrel 30 together. The pilot post 70 is journaled free to rotate within the bore 54 relative to the bottom rotatable barrel 50. This construction allows the pilot post 70 to be removed from the assembly by axially sliding the pilot post out of the barrel bores 34, 54. Once removed, the pilot post 70 can be rotated, in the exemplary embodiment, by an angle of 90° relative to the barrels 30, 50, and reinserted into assembly in the new position. Hence, the pilot post is convertible such that it can be removed from the assembly and reassembled in another of the selected plurality of possible positions in relation to the rotatable barrel and, thus, provide the significant aspect of the invention.
Referring to FIG. 9, a split pin tumbler arrangement 90 is housed within the top (fixed) and bottom (rotatable) barrels 30, 50. The tumbler arrangement includes sets of top and bottom pins 91, 92 respectively. The pins of the top set 91 are nested in cylindrical sockets 37 in the fixed top barrel 30 and the exposed outer-half of the pins abut and are retained by the underside of flange 11 of casing 12 (see FIGS. 2 and 3). In the preferred embodiment, these sockets 37 constitute four bores arranged in a circumferential planar pattern about the wall of the barrel as illustrated. The sockets 37 pass through the barrel and have apertured ends opening to the inside axial ends of fixed top barrel 30 and opening to an outside axial end.
The pins of the bottom set 92 are similarly nested in cylindrical sockets 57 in the rotatable bottom barrel 50. The planar pattern or arrangement of the sockets 57 matches that of sockets 37. Hence, the sockets 37 and 57 align when the fixed barrel 30 assumes a predetermined orientation with respect to the rotatable barrel 50. The bottom sockets 57 have apertured ends at the inside axial end of the barrel 50 which open toward the top barrel 30. However, the sockets 57 have blind ends toward the outside end of the barrel 50.
The tumbler arrangement further includes springs 93. The springs are nested between the blind ends of the bottom sockets 57 and the pins of the bottom set 92. The springs 93 and pins of the fixed set 92 are dimensioned such that the springs urge the pins to protrude beyond the inside socket apertures when the springs are relaxed. When the barrels 30, 50 align, these springs 93 urge the pins of bottom set 92 into the top sockets 37. With the pins 92 crossing the threshold of the top inside socket apertures, the two barrels 30, 50 are interlocked. Because the bottom rotatable barrel 50 is rotationally fixed to the housing, the top barrel 30 and the pilot post 70 rotationally fixed thereto, are also rotationally locked.
In another important aspect of the invention, the pilot post 70 comprises at least one key-guide with which a mating guide on an actuating key is conformed to register. Thus, another function of the pilot post is to define, in part, the geometric form for an actuating key.
In the illustrated embodiment, the pilot post 70 includes two key-guides. These consist of a groove guide 74 and a lug guide 76 (see FIG. 4). As indicated previously, lug guide 76 also acts as a pilot post positioning lug. Correspondingly, FIGS. 10 and 11 depict an actuating key 110 having guides of its own formed to mate with those on the pilot post 70. Thus, the key 110 has a hollow cylinder 112 adapted to accept the pilot post 70 therein. The cylinder 112 has an internal lug guide 114 configured to mate with the pilot post groove guide 74. The cylinder 112 also has an internal groove guide 116 formed to engage the pilot post lug guide 76.
As noted above, an actuating key is also formed with actuating abutments configured to register with and actuate the pins of the tumbler arrangement. Accordingly, as depicted in FIGS. 10 and 11, the key 110 further has kerfs 118 ending in lands 120 which serve as the abutments. The kerfs 118 are arranged in number and planar position corresponding to the plan configuration of the tumbler assembly 90. Similarly, the axial depth pattern of the lands 120 corresponds to the depth configuration of the tumbler assembly 90.
To unlock the barrel lock 10, the key 110 is engaged with the pilot post 70. Pressing down on the tumbler assembly 90 actuates the pins against the springs 93 releasing the fixed barrel 30 from rotatable barrel 50. The key-guides on the pilot post 70 and the key 110 mate to transmit torque from the key to the pilot post, and thus the pilot post and fixed barrel 30 can rotate independently of barrel 50 which is fixed to the housing. Finally, since cylinder 78 is rotationally fixed to pilot post 70, it rotates with pilot post 70 and screws or unscrews onto the rod.
In a lock according to the present invention, the lock combination is defined as agreement between the following two pairs of factors. The first factor comprises agreement between the tumbler configuration of the lock and the kerf configuration of the actuating key. Further, this actually comprises agreement in both planar formation and the depth configuration.
The second factor comprises agreement between the key-guide configurations on the pilot post of the lock and that on the key. Similarly, this agreement also has depth and planar characteristics associated therewith. The planar attribute comprises the number and planar location of the guides. The depth attribute relates to the predetermined axial extent of the guides, for example, agreement in the axial dimension of the key groove guide 116 and that of the matching pilot post lug guide 76.
Also very importantly, the pilot post key-guide provides a geometric reference relative to which an orientation of the pilot post may be assumed. As previously noted, the pilot post may be removed from assembly and reinstalled in a different orientation while maintaining the original tumbler arrangement. The tumbler arrangement in the present invention represents all of the tumbler pins housed within the lock. The tumbler arrangement is regarded as being fixed with respect to the lock in that none of the tumblers need to be moved in the lock as the pilot post is adjusted with respect to the tumbler arrangement. This significant feature allows the lock combination to be changed by merely reinstalling one part, pilot post 70. With the pilot post 70 disposed in a different rotational position, the relationship between the pilot post guides and the tumbler planar formation is changed. Thus, a new key 110 is required to actuate the lock.
In another advantage of the present invention, is that, if necessary to void all four original combinations and keys, the lock combination can be converted in the conventional manner by substituting new pins of the tumbler assembly.
A number of modifications to the described embodiment are considered to be within the purview of the present invention. A description of some specific alternatives contemplated follows.
As noted above, the lug and groove construction between the fixed top barrel and the pilot posts, for example, are considered interchangeable. Thus, the barrel bore may be formed with lugs registering in grooves in the pilot post. Alternatively, the pilot post and fixed barrel may be rotationally secured by means of a set screw or pin similar to that disclosed to rotationally fix the casing and bottom barrel. In this adaptation, an access port would be drilled through the casing wall. The barrel would be rotated to align the set screw positions with the port through which a tool, for example, an allen wrench or screw driver, could gain access to the set screw.
In yet another alternative, the pilot post and the internal bore of the top barrel may have mating non-circular plan forms, for example, elliptical, rectangular or triangular profiles which transmit torque therebetween. Also, the pilot post may have different segments comprising cross-sections of varying profiles or dimensions.
Referring to the barrels, one variation contemplates that the fixed and rotatable barrels be inverted such that the top barrel be rotatably fixed relative to the housing and the bottom barrel be allowed to rotate with the pilot post. However, the preferred embodiment disclosed provides the advantage that, since the rotatable bottom barrel is fixed to the barrel lock casing, the tumbler assembly is held in place within the housing when the pilot post is removed.
Also, the rotatable barrel, being either on the top or bottom, need only be rotatably fixed to the casing. Therefore, any of the alternatives outlined above for rotatably fixing the pilot post and fixed barrel apply here.
The key guides may assume a variety of geometric formations formed on the pilot post. These geometric formations may be in the form of material added, for example, a lug or dowel formed on the pilot post, or may be in the form of material removed, for example, a groove or chamfer on the pilot post. Alternatively, the key guide may comprise the plan form of the pilot post generally. Thus, the key bore and pilot post may have mating non-circular plan forms configured to transmit rotation therebetween.
In another alternative construction, the pilot post may comprise a female member while the mating key has a corresponding male member formed thereon.
Given the foregoing, modifications and variations of the invention should now be evident to the person of ordinary skill in the art. Such modifications and variations are intended to fall within the spirit and scope of this invention as defined by the following claims.
|
A barrel lock includes a circumferential axial pin tumbler arrangement housed in the barrel. A removable pilot post is disposed among the tumblers and has key-guides which register with mating key-guides on an actuating key. To change the lock combination, the lock can be reassembled with the pilot post located in a new rotational orientation relative to the tumbler arrangement. A particular application includes locking merchandise compartments in vending machines, for example.
| 8
|
BACKGROUND OF THE INVENTION
This invention relates to an apparatus for the discrimination of myoelectric potential patterns, to be used in a drive mechanism which is controlled by using, as instruction signals, various myoelectric potentials issuing from a given part of the human body.
The external-prosthesis, which aims to give relief to persons disabled by the absence of or defect in their body parts, is most advanced in the field of artificial legs and artificial arms. Artificial arms, in particular, are required to produce complicated motions. Drive mechanisms developed for operating such artificial arms by effective use of electric motors and hydraulic drive means have reached a high degree of perfection. The control of a drive mechanism, however, calls for highly complicated processing. Various methods have heretofore been proposed for the purpose of this control. Unfortunately, these methods tend to entail the common disadvantage that the control devices which embody their respective principles are unproportionately large in size for the number of modes of motions the artificial arms are expected to produce. Different methods have also been proposed for the discrimination of control signals used for causing artificial arms to produce motions. One of these methods involves use of a plurality of independent input devices and another utilizes prescribed voice sounds uttered by the user as instruction signals. All of these conventional methods are deficient, in varying measures, of the ability to provide artificial arms with perfect control devices fully satisfactory for actual use.
For a disabled person to enjoy the smoothest natural use of an artificial arm for example, the prime and sole requisite is that the entire control system should be amply small and light and it should enable the muscles in certain relevant part of the subject, such as his shoulder or remaining brachium, to issue instruction signals to the drive mechanism for the artificial arm in entirely the same manner as the above mentioned relevant part would do in moving a natural arm. The best way to fulfill this requisite resides in limiting the number of modes of motions of the artificial arm to the irreducible minimum and thereby decreasing the size and weight of the device to the fullest possible extent and using, as instruction signals for the control device, the myoelectric potentials (hereinafter referred to as "EMG") issued by the muscles of the relevant part of the subject in moving his natural arm.
Such instruction signals are effectively extracted from the muscles of the relevant part of the subject by attaching a plurality of electrodes for extracting EMG signals to as many positions around the relevant region and converting the EMG signals generated in the relevant region into a corresponding EMG pattern by means of the aforementioned extraction electrodes. Where such an EMG pattern is used as an instruction signal, a plurality of EMG patterns are generally classified on a basis of the linear discriminant principle. Methods proposed heretofore are invariably based on a principle that the control of an artificial arm is accomplished by prescribing a definite number of modes of motions the artificial arm is expeced to produce, fixing discriminant functions one each for the aforementioned different modes of motions, and providing the same number of circuits adapted to perform arithmetic operations on the discriminant functions as that of modes of motions, whereby the circuit, upon receiving incoming EMG signals, will carry out arithmetic operations on corresponding discriminant functions, compare the results of these operations with one another and single out the largest value which determines the exact motion to be imparted to the artificial arm. Devices embodying such conventional methods are required to incorporate as many circuits as there are modes of motions and, therefore, tend to make up much space. Since the discrimination devices heretofore known to the art mostly depend for the aforementioned processing of arithmetic functions upon general-purpose computers, their hardware structures take up too much space to be applied advantageously to artificial limbs.
An object of this invention, therefore, is to provide a compact apparatus for the discrimination of EMG patterns for use in a drive mechanism adapted to impart motions to an artificial limb, which apparatus extracts EMG signals issuing from a given part of a disabled person and uses them as instruction signals for the control of the drive mechanism, performs arithmetic operations on the corresponding discriminant functions at high speed and enables the artificial arm to produce smooth natural motions faithfully in response to the results of the operations.
SUMMARY OF THE INVENTION
To accomplish the object described above according to this invention, there is provided an apparatus for the discrimination of EMG patterns, which apparatus comprises an input unit for detecting EMG signals from myoelectrodes on the body of a disabled person; a processing unit provided with memories for storing the weight coefficients of discriminant functions fixed on the basis of average EMG data obtainable with the prescribed modes of motions and adapted to perform arithmetic operations successively on the EMG signals issued from the input unit and the values of coefficients from the memories in accordance with linear discriminant functions; and a maximum-value detection unit serving to single out the maximum-value signal from among the output signals from the processing unit and retain a category number signal corresponding to the maximum-value signal.
The aforementioned apparatus for the discrimination of EMG patterns, at the time that linear discriminant functions are processed, allows the EMG patterns of magnitudes each formed of a plurality of EMG signals issuing from the body to be successively subjected to arithmetic operations against each of the different modes of motions and, at the same time, compares sequentially the results of the arithmetic operations one by one. As a result, the desire to reduce the size and weight of the apparatus to the fullest possible extent is gratified. Further, this apparatus acquires an ability to preclude the possible production of erroneous motions in response to EMG signals on the noise level when the input unit is adapted to perceive as instruction signals a plurality of EMG signals only on condition that the total sum of the plurality of EMG signals surpasses the reference level. The apparatus, because of its particular configuration, permits the number of classified categories to be readily increased as required.
The other objects and characteristics of the present invention will become apparent from the further disclosure of the invention to be made hereinafter with reference to the accompanying drawing.
BRIEF EXPLANATION OF THE DRAWING
FIG. 1 is a block diagram schematically illustrating the apparatus for the discrimination of EMG patterns according to the present invention.
FIG. 2(A), FIG. 2(B) are block diagrams illustrating in detail one preferred embodiment of the apparatus for the discrimination of EMG patterns according to the present invention.
FIG. 3 is a time chart concerning the operations of the component units as indicated in FIG. 2.
FIG. 4 is a schematic diagram illustrating the state of coefficients stored in the memories of FIG. 2(B).
FIG. 5 is a block diagram illustrating the function of the decoder to be used in one preferred embodiment of this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
This invention relates to an apparatus for the discrimination of myoelectric potential (EMG) patterns to be used in the formation of instruction signals for the control of a drive mechanism adapted to operate by use of EMG signals.
When, for example, an artificial arm fitted to the body of a disabled person is bent and rotated at the elbow joint thereof by operating driving mechanisms which are provided at the joint, it is advantageous to utilize EMG signals in forming control signals for driving the motors as the driving mechanisms, for example. Also when the disabled person wishes to operate various mechanical implements other than his own artificial arm, it is likewise advantageous to rely upon instruction signals which are derived from such EMG signals, depending on the degree of his disability. In this case, when the mechanical implements are desired to produce numerous kinds of motions, there are inevitably required as many kinds of control signals. When the wrist and hand of the artificial arm are desired to produce motions in numerous directions by the operation of a plurality of motors disposed at the joints in the artificial arm, for example, it becomes necessary to issue widely varying control signals for designating relevant motors out of the whole group of motors available and selecting directions in which such designated motors are to be driven.
Concerning the issuance of such numerous kinds of control signals by use of EMG signals, it has been ascertained that when the EMG signals which the muscles in certain relevant regions of the human body generate in response to motions to be produced by the natural arm are detected and compared one with another against several fixed modes of motions, the EMG patterns consequently obtained with respect to the different motions vary one from another. Based on this knowledge, the present invention accomplishes the desired issuance of control signals by predetermining average EMG patterns corresponding to various modes of motions the artificial arm is expected to produce, comparing the pattern of actually extracted EMG signals with these predetermined average EMG patterns to select the preset average EMG pattern most closely approximate to the extracted EMG pattern and giving rise to a control signal corresponding to a mode of the EMG pattern selected in consequence of the comparison.
With reference to FIG. 1 which represents a block diagram of the apparatus for the discrimination of EMG patterns according to this invention, the processing function of the apparatus will be described in outline.
A plurality of electrodes E serve the purpose of extracting EMG signals. For the extraction of instruction signals from the muscular motions by the detection of changes in the EMG signals resulting from the vertical and horizontal motions produced by the clavicle in the human body, for example, the plurality of electrodes E are attached to the trapezius, the pectoralis major, the latissimus dorsi, the teres major, etc. which govern the motions of the clavicle. The present embodiment represents a case wherein control signals for n-modes of motions of the artificial are are obtained by using four electrodes. As a matter of course, the number of electrodes and the number of control signals can be freely fixed. Generally the number of control signals to be required increases in proportion as the number of modes of the motions the artificial arm is expected to produce increases. When the number of modes of the motions and that of control signals are increased, it becomes necessary to increase proportionally the number of positions of the human body used for the extraction of EMG signals and improve the fineness with which the produced EMG pattern is identified.
As the person wearing the artificial arm attempts to move the arm to a desired position, the four EMG signals reaching the electrodes E exhibit their respective magnitudes characteristic of the motion involved. Thus a pattern is formed by one set of four EMG signals. Through discrimination of the EMG pattern, there can be obtained control signals corresponding to the motion the clavicle is required to produce. These four EMG signals, x 1 to x 4 , generally exhibit irregularly alternating magnitudes. They are, therefore, amplified, rectified and smoothened in the input circuit 2 of the input unit 1 to be converted into corresponding direct-current signals. These direct-current signals are held in the holding circuit 7 tobe used in the subsequent processing step.
EMG signals are generated, though very feebly, even while the issuance of control signals for the production of motions is suspended. To preclude possible production of motions by such idle myoelectric potentials, the EMG signals must be deprived of those EMG signals of the noise level before they are applied to the holding circuit 7. The elimination of those EMG signals of the noise level is effected by the level-setting circuit 5, so that only the EMG signals, x 1 to x 4 , which are required for the production of motions are stored in the holding circuit 7. The EMG pattern thus obtained relative to the motions to be produced is identified by means of linear discrimination.
Classification of the patterns by the linear-discrimination method is effected as follows. As the preparatory step, the subject is caused to move his clavicle in various directions to determine in advance what EMG signals are generated, on the average, in response to the motions produced by the clavicle. This experiment is repeated many times. As a result of this experiment, category numbers, 1, . . . n, are assigned one each for the different motions produced by the clavicle. The average EMG signals obtained as described above are generally called "standard patterns", which are indicated by the expression: x i =(x 1 i , x 2 i , x 3 i , x 4 i ). After completion of this preliminary experiment, the subject is again caused to move his clavicle similarly to give rise to actual input patterns x.sup.α =(x 1 .sup.α, x 2 .sup.α, x 3 .sup.α, x 4 .sup.α). The classification of the pattern with respect to the categories mentioned above is effected by performing the calculation: ##EQU1## with respect to each of the different categories, comparing the terms, P 1 , . . . , P n corresponding to the n-categories, to single out P l (1≦l≦n) as the term having the smallest value and concluding that the pattern in question belongs to Category l. The classification of Formula (1) indicated above is generally considered to be equivalent to the classification which comprises carrying out the calculation of the array of linear functions shown below with respect to the input pattern (x 1 .sup.α, x 2 .sup.α, x 3 .sup.α, x 4 .sup.α) and finding the term y l having the maximum value to which the caterogy l corresponds. ##EQU2##
In the formula given above, a ij (i=1, 2, . . . , n, j=1, 2, . . . , 5) represents a constant (weight coefficient) to be determined by this value of the standard pattern.
In the processing unit indicated in the diagram of FIG. 1, the calculation of the righthand side of the equation of Formula (2) is carried out. These calculations of function are not carried out all at once but are performed one by one in accordance with the clock generated by the synchronizing unit 10.
In the processing unit 20, the weight coefficients are set in the memories 21 and are successively subjected to arithmetic operation in the processing circuit 23, with the result that signals y i are successively issued through synchronization with the clock.
The signals y i issued from the processing unit 20 are received in the subsequent maximum-value detection unit 30, in which the particular category number corresponding to the signal y max having the maximum value is singled out. It is forwarded through the decoder 40 to the artificial arm A and used for the selection of the mode for the motion of the artificial arm. Now, the operation of the apparatus will be described in detail with reference to FIGS. 2(A) and 2(B).
FIG. 2(A) is a detailed block diagram of the input unit 1 (lower side) and the synchronizing unit 10 (upper side). From the clock-pulse (CP) generator 11 of the synchronizing unit 10, a pulse train s 1 with a pulse separation P as shown in FIG. 3 is issued. This pulse serves as the standard pulse for the calculation performed with respect to each of n-discriminant functions. The pulse separation P is fixed so as to satisfy P>p wherein p denotes the operation time, namely the length of time required for the performance of the abovementioned calculation of one discriminant function. In the meantime, the EMG signals extracted by the electrodes from the different positions are amplified by the myoelectric amplifiers 3, then rectified and smoothened by the rectifying and smoothening (R/S) circuits 4 and, consequently, converted into direct-current signals x m . They are subsequently held in the holding circuits (I)-(IV) until all the calculations of the discriminant functions of Formula (2) are completed. The hold signal s 2 , as illustrated in FIG. 3, is a signal obtained by dividing the output s 1 from the CP generator 11 by the frequency divider 12. The hold signal is issued once for each machine cycle. This signal s 2 assumes a length of time which is (n+1) times the length of the pulse separation P.
It is imperative that before they are subjected to the arithmetic operations by the apparatus of this invention, the EMG signals issued from the muscles in consequence of the motions produced by the clavicle should be examined to determine whether or not they constitute control signals for the artificial arm. For the purpose of this particular examination, the apparatus of this invention is provided with a level-setting circuit 5, which is adapted to permit the processing for the calculation of the discriminant functions only when the total sum of the rectified and smoothened values of all the EMG signals exceeds a fixed level. Specifically with reference to FIG. 2(A), the aforementioned examination is accomplished by summing the output values from the R/S circuits 4 in the adder(I) 5, comparing the resultant sum of output values with the reference-level value preset in the comparator(I) 5b, opening the gate 6 only when the output of the comparator(I) is ON, enabling the output of the frequency divider 12 to be delivered to the hold circuit, and retaining the EMG signals. The signal s 3 shown in FIG. 3 is the output from the comparator(I) 5b.
When a motion of some form or other is produced and the total sum of EMG signals consequently generated exceeds the aforementioned level, the gate(I) 6 is opened and the hold signal is issued synchronously with the signal s 2 from the divider 12 to hold the EMG signals from the R/S circuits 4. At the same time, the analog switch 8 is opened by the output of the comparator(I) 5b and the EMG signals are applied to the multipliers 24 of the processing circuit 23 shown in FIG. 2(B). To the remaining input terminals of these multipliers 24 are delivered, through the digital-to-analog converters (D/A) 22, the outputs from the memories(I)-(IV) 21 which keep the weight coefficients of discriminant functions in the form of digital numerals as shown in FIG. 4. The result is that the operation of the multipliers 24 gives rise to the products of the rectified and smoothened values of EMG signals (x 1 , x 2 , x 3 , x 4 ) and the coefficients (a i1 , a i2 , a i3 , a i4 , a i5 ). The coefficients in the memories(I)-(V) 21 are successively delivered to the multipliers 24 in accordance with the timing of the output of the CP generator 11 when the remaining gate(II) 29 is ON. In this timing, the value "n" (the number of discriminant functions) corresponding to the number of categories involved in the classification is set in advance in the preset register 27 and the content in the preset register 27 is transferred via the gate(II) 29 into the counter 26 by order of the pulse obtained by processing the leading of the output of the comparator(I) 5b in the monostable circuit(I) 28. When the content of the counter 26 is decreased by one for each pulse s 1 of the output from the CP generator 11, the content of the counter becomes n-1 and, consequently, the address n-1 in the memories(I)-(V) is designated as illustrated in FIG. 4. The result is that the contents (a n1 , a n2 , . . . a n5 ) of the memories are transferred via the D/A converters 22 into the multipliers 24. The contents of the counter 26 are decreased to n-2, n-3, . . . 0 as the 2nd, 3rd, . . . output pulses are issued from the CP generator 11. Consequently, the contents (a n-1 ,1 ; a n-1 ,2 ; . . . a n-1 ,5) . . . (a 1 ,1 ; a 1 ,2 ; . . . a 1 ,5) of the memories(I)-(V) at the addresses n-2, n-3, . . . 0 are successively delivered to the multipliers 24.
The output of the multipliers 24 is then fed to the adder(II) 25. This means that the signals y 1 to y n are calculated, as synchronized with the pulse from the CP generator 11, in the order of y n , y n-1 , . . . y 1 in accordance with n to l of Formula (2). The outputs y i (i=1, 2, . . . , n) are further applied successively to the maximum-value detection unit 30. The content of the holding circuit(V) 31 is reset to the level 0 by the signal s 2 of the divider 12 as illustrated in FIG. 3. Also, the output level of the maximum-value detection unit 30 is maintained at the level 0 when the input remains at the level 0. When the outputs y i from the adder(II) 25 are fed into the maximum-value detection unit 30 synchronously with the clock pulse, they are compared by the comparator(II) 32 with the outputs from the holding circuit(V) 31 (the output 0 where i=1). When y i is greater than 0, the output y max of the maximum-value detection unit assumes the status of ON. Consequently, the monostable circuit(II) 33 is driven to issue the latch signal L i to the latch circuit 34. At the same time, the signal is fed back to the holding circuit(V) 31 to hold the output y i . On receiving this latch signal L i , the latch circuit 34 latches at that moment the content of the counter 26 corresponding to the number of the categories, namely the signal i-1. As the next clock pulse is issued from the CP generator 11 and the output y i-1 from the processing unit 20 is calculated by the aformentioned procedure and then forwarded to the maximum-value detection unit, the output y i and the output y i-1 are compared in the state as illustrated in FIG. 2(B) because, at this stage, the output y i is held in the holding circuit(V) 31. If the output y i-1 is greater than the output y i , the signal of i-2 is latched in the latch circuit 34 and the output y i-1 is held in the holding circuit(V) 31 and, thereafter, the issuance of the output y i-2 by the subsequent clock pulse is awaited. If the output y i-1 is smaller than the output y i , the existing status is left unchanged and the issuance of the next value from the adder(II) is awaited. When the outputs y n to y l are successively compared, the value resulting from the subtraction of 1 from the number "i" corresponding to the i'th signal designating the maximum value y max among the outputs y n to y l will eventually remain in the latch circuit 34.
The content of the counter 26 is successively decreased by one for each pulse issued from the CP generator 11. When the content of the counter 26 is lowered below 0 by the (n+1)th subtractive pulse, namely when all the comparisons of the outputs y l to y n are completed, the borrow signal s 4 is issued by the timing illustrated in FIG. 3. By this borrow signal, the content of the latch circuit 34 is forwarded to the latch register 35 and latched therein and, at the same time, with the issuance of END PULSE, the contents of the holding circuits(I)-(IV) 7 are also cleared. In the latch register 35 is stored the value which is obtained by subtracting 1 from the category number corresponding to the signal having the maximum value among the outputs y 1 to y n . Thereafter, upon the arrival of the subsequent clock pulse generated by the CP generator at t o ' time, the same operation is repeated when the EMG signals are in their active state. As a result, the data corresponding to the category number having the maximum value in the discriminant function are issued as the output from the latch register 35 by the machine cycle of (n+1)P. The content to be stored in this latch register 35 is similar in form to the signal which is held in the counter 26. For this content to be converted into the control signal for the artificial arm, the output from the register 35 is decoded by the decoder 40. The control signal thus produced is sent to the driving unit 50 adapted to operate the drive mechanisms corresponding to the joints in the artificial arm.
As described above, the apparatus of the present invention enjoys perfect freedom from possible erroneous operation by passing feeble EMG signals through the level-setting circuit of the input unit 1 and discriminating instruction signals precisely from noise signals and warrants quick and accurate performance by having weight coefficients stored in memories and then subjected to DA conversion and thereby permitting analog processing of discriminant functions. Alteration of weight coefficients can be very easily effected by revision of the contents of memories. Further the fact that the arithmetic operations on the different formulas involving discriminant functions are sequentially carried out and the results of the operations are successively compared enables the apparatus of this invention to provide efficient processing of data and, at the same time, permits the apparatus to function effectively with an extremely small number of circuit elements and occupy a very small space. Moreover, this invention can be applied to the control of the other artificial limbs and other ordinary machine tools besides the control of artificial arms.
|
An apparatus for the discrimination of myoelectric potential patterns, which operates with a procedure comprising the steps of discriminantly screening instruction signals from myoelectric potential signals issuing from the subject's body, performing arithmetic operations of the linear-discriminant functions on the instruction signals against the gravity coefficients fixed in advance based on the data of average myoelectric potential patterns from the modes of motions involved, and classifying the signal of the largest value selected from the results of said arithmetic operations with respect to the prescribed mode of motion.
| 0
|
FIELD OF INVENTION
[0001] The present invention generally relates to the field of circuit testing. More specifically, an embodiment of the present invention provides instruction-based built-in-self-test (BIST) of external memory.
BACKGROUND OF INVENTION
[0002] As the complexity of integrated circuits (ICs) increases and access to their internal circuit nodes becomes harder, properly testing such devices becomes a major bottleneck during their prototyping, development, production, and maintenance. As a result, designs with BIST implementation have become commonplace. In a BIST implementation, circuitry (which is intended solely to support testing) is included in an IC or in a system including ICs.
[0003] With 64-bit support in the latest generation of microprocessor families, it is customary to find large (e.g., up to 40 GB) external memories. Although the memory provider normally guarantees a reasonably high level of test coverage before shipping the memory chips to their customers, it is common to find defects in the memory chips after they are mounted on boards or modules. As a result, some memory tests need to be done on the system to detect defects that either remained undetected due to gaps in the manufacturer's test process or were introduced during the board or module manufacturing process.
[0004] Current board and system test strategies often rely on standard “invasive” test techniques involving either “Bed of Nails” or OBN type probing, or a “Hot Mock Up” type interconnection technique. These different methods of testing enables the physical “stitching” together of a system to allow booting to the local operating system (OS) or test kernel. Once the system has booted, diagnostic testing can proceed. However, with the escalation of board operating frequencies and bus speeds at the connectors (sometimes reaching 150 MHz and beyond), the “stitching” introduces signal integrity or timing issues that render these techniques often unreliable or non-repeatable. This fundamental problem results in higher test costs due to higher manufacturing retest rates, higher no-trouble found (NTF) rates, and/or higher test capital consumption.
[0005] A solution can be using power-on self-test (POST). However, an important prerequisite for using POST is a functional and reliable central processing unit (CPU) and a programmable read-only memory (PROM) boot path. To fulfill this requirement, the functionality and integrity of several parts of the chip or module (such as PROM, bus interface, peripheral component interface (PCI) bus) has to be assured first. This, in turn, requires a significant investment in expensive test hardware and test fixture capital.
[0006] Furthermore, while POST can be utilized as a board system level test feature, any enhancement to POST requires significant development time and cost. This, along with the fact that POST development requires a “golden” board as a precondition, makes it logistically difficult to rely completely on POST enhancements to cover memory test and diagnosis. Consequently, the test infrastructure (test host, instrumentation, fixtures, etc.) costs have quadrupled from last generation to the current generation of product testing. This increase in test costs has necessitated some fundamental changes in testing strategies for external memories and other board or system level components. This change has mainly been in the form of an increased reliance on embedded and structured test methodologies that are independent of the OS and require only a minimal set of system level resources (power, clocks, and the Institute of Electrical and Electronics Engineers (IEEE) 1149.1 standard interface)) to be functional.
[0007] External memory BIST (EBIST) is one such methodology. Not having to boot to a local OS relieves the requirement of having to “stitch” together a system with costly or unreliable invasive probing or interconnection techniques. Memory BIST is used today in the industry for testing embedded memories (such as that available commercially from LogicVision of San Jose, Calif.). Such solutions are generally based on hard-coding a predefined test algorithm and data patterns. Another approach is based on multiplexing EBIST logic into the memory bus input/outputs (IOs), thus bypassing all internal logic. With advances in technology and processes, and a wide range of available memory designs, however, there is an increasing need for more flexibility in the kind of test algorithms and the test patterns.
[0008] To address this issue, one proposed approach is to implement a processor-based engine with two separate instruction storage memories. This approach offers a fair degree of flexibility but suffers from high area overhead. Another proposed approach is implementing an EBIST that reduces area overhead by coding BIST features into register transfer level (RTL). However, this approach results in less flexibility of test algorithms and may not be applicable to many memory chips available on the market today. Some of the issues with past EBIST techniques can be summarized as follows: (a) they require intrusion at a chip's IOs, which are usually in the critical paths, resulting in timing problems and design iterations to accommodate EBIST; (b) they require reimplementing the random access memory (RAM) access protocol inside the BIST engine, resulting in unnecessary area overhead (not to mention the risk of implementing and, hence, testing an incorrect protocol); and/or (c) they generally hardcode the test algorithm, the data background, and/or both, resulting in low test coverage of the memory subsystem and not providing the flexibility required for diagnosis or for targeting memories from different vendors.
SUMMARY OF INVENTION
[0009] The present invention includes novel methods and apparatus to efficiently provide instruction-based BIST of external memory. In an embodiment, a built-in self-testing system is disclosed. The system includes an external memory module, an on-chip memory controller coupled to the external memory module, an on-chip built-in self-test (BIST) module coupled to the on-chip memory controller, and an interface controller coupled to the BIST module to provide an interface to access the BIST module. The on-chip memory controller may send and receive data to and from the external memory module. And, the BIST module may include an instruction register to store a plurality of instructions.
[0010] In another embodiment, the BIST module may utilize the on-chip memory controller to perform tests on the external memory module.
[0011] In a further embodiment, the interface controller may include a test access port (TAP) (such as that provided by the IEEE 1149.1 standard).
[0012] In yet a further embodiment, the system may further include an I/O interface coupled between the on-chip memory controller and the external memory module to provide communication between the on-chip memory controller and the external memory module.
[0013] In a different embodiment, the instruction register may include at least six 7-bit registers.
[0014] In yet another embodiment, the instructions may have an opcode selected from a group comprising March element, inversion, increment/decrement address, and/or address uniqueness.
BRIEF DESCRIPTION OF DRAWINGS
[0015] The present invention may be better understood and its numerous objects, features, and advantages made apparent to those skilled in the art by reference to the accompanying drawings in which:
[0016] [0016]FIG. 1 illustrates an exemplary high-level EBIST system 100 in accordance with an embodiment of the present invention;
[0017] [0017]FIG. 2 illustrates an exemplary block diagram for an EBIST engine 200 in accordance with an embodiment of the present invention; and
[0018] [0018]FIG. 3 illustrates an exemplary instruction register 300 in accordance with an embodiment of the present invention.
[0019] The use of the same reference symbols in different drawings indicates similar or identical items.
DETAILED DESCRIPTION
[0020] In the following description, numerous details are set forth. It will be apparent, however, to one skilled in the art that embodiments of the invention may be practiced without these specific details. In other instances, well-known structures, devices, and techniques have not been shown in detail, in order to avoid obscuring the understanding of the description. The description is thus to be regarded as illustrative instead of limiting.
[0021] Reference in the specification to “one embodiment” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least an embodiment of the invention. The appearances of the phrase “in one embodiment” in various places in the specification are not necessarily all referring to the same embodiment.
[0022] To provide access to BIST functionality on a chip, a TAP may be utilized. TAP can be a general-purpose port that provides access to test support functions built into a component. Further information on by IEEE 1149.1 standard interface may be found in IEEE Standard Test Access Port and Boundary-Scan Architecture, IEEE Std 1149.1-1990 (includes IEEE Std 1149.1a-1993), Chapter 3, entitled “The Test Access Port,” which is hereby incorporated herein for all purposes.
[0023] [0023]FIG. 1 illustrates an exemplary high-level EBIST system 100 in accordance with an embodiment of the present invention. A standard IEEE 1149.1 standard interface controller 102 may be used to program an EBIST engine 104 through, for example, a serial link synchronized to the internal core clock. In an embodiment, it is envisioned that other types of links may be utilized to program the EBIST engine 104 such as Ethernet, Fast Ethernet, wireless, modem, cellular, universal serial bus (USB and its varieties such as USB II), and/or FireWire. In one embodiment, the EBIST engine 104 may be implemented inside a CPU. The CPU may be a SPARC microprocessor available from several vendors (including Sun Microsystems of Santa Clara, Calif.). Those with ordinary skill in the art understand, however, that any type of a CPU may be utilized to embody the present invention, including those made by Hewlett Packard of Palo Alto, Calif., and IBM-compatible personal computers utilizing Intel microprocessor, which are available from several vendors (including IBM of Armonk, N.Y.). In addition, instead of a single processor, two or more processors (whether on a single chip or on separate chips) can be utilized. It is further envisioned that the CPU may be a complex instruction set computer (CISC) microprocessor, a reduced instruction set computing (RISC) microprocessor, a very long instruction word (VLIW) microprocessor, a processor implementing a combination of instruction sets, and the like.
[0024] In the EBIST system 100 , the EBIST engine 104 may, in turn, use an on-chip memory controller 106 to access an external memory 108 through, for example, an I/O interface 110 . In FIG. 1, a boundary of the chip that the BIST engine 104 resides on is shown as item 112 . In an embodiment, the BIST engine 104 may be compatible with the interface protocol of memory controller 106 . The BIST engine 104 may generate four sets of signals (e.g., address, data, read/write controls, and service requests) to talk to the memory controller 106 . The BIST engine 104 may also decode the requests from the memory controller 106 to the external memory 108 in order to predict expected values from the external memory 108 . Such an embodiment is envisioned to permit implementation of the EBIST with little area overhead, in part, by reusing existing on-chip features for memory access. Additionally, there would be no need to reimplement the memory access protocol.
[0025] In a further embodiment, the features of the EBIST system 100 may include any combination of the following:
[0026] The IEEE 1149.1 standard interface 102 may reduce pin requirements for accessing the EBIST engine 104 down to the five existing IEEE 1149.1 standard interface pins. This, along with in-flight programming (i.e., being programmable while the clock is running at full frequency, e.g., when the associated phase-locked loop (PLL) is in lock, to allow debugging of complex, intermittent failures) means that the transfer of data from the IEEE 1149.1 standard interface 102 to the EBIST engine 104 may need to be synchronized to the internal (i.e., faster) core clock.
[0027] The EBIST system 100 may provide for a highly flexible and programmable test algorithm. There can be six instruction registers that allow the user to program the test algorithm. It is envisioned, however, that the number of instructions may be reduced or extended in various embodiments. In one embodiment, the EBIST engine 104 may implement three basic March elements (e.g., read, write, and read-write-read) that can be sequenced in a number of ways, based on the six instruction registers, for example. This allows the user to define several different test algorithms from a simple 2N and up to xN (where x=3* number of instruction registers, for example). For example, a 2N test may involve writing data to all address locations, reading back, and comparing the data with the expected value. Moreover, a 13N may involve the following:
Address (0) −> Address (max) write X (i.e., writing X to Address (0) through Address (max)); Address (0) −> Address (max) read X, write Y, read Y (where Y is the inverted value of X); Address (0) −> Address (max) read Y, write X, read X; Address (Max) −> Address (0) read X, write Y, read Y; and Address (Max) −> Address (0) read y, write X, read X.
[0028] The EBIST engine 104 may also provide a prepackaged address uniqueness test where the address ranges can be programmed through the IEEE 1149.1 standard interface 102 . Furthermore, the address uniqueness may be implemented as a mod of operation (such as 2N, 3N, and the like). Accordingly, the programming of the address range may be done independently of the mode of operation.
[0029] The EBIST engine 104 may implement true checkerboard pattern testing by, for example, allowing consecutive addresses to write inversions of the programmed data background.
[0030] In one embodiment, a loop option may let the EBIST engine 104 to iterate the programmed sequence of March elements. This may allow the user to better distinguish between intermittent and permanent failures in a board or system environment. This approach can also be used during bum-in for controlling the amount of stress the device under test (DUT) should be put through.
[0031] The range of addresses to be tested may be programmable using a start and end address.
[0032] The EBIST engine 104 may also provide a programmable address step size to allow quick screening of large memories without going through the complete address space, thus reducing test times in production as well as reducing verification times.
[0033] The data backgrounds for testing memories may also be programmable. This fulfils requirements associated with high coverage memory tests that are independent of address and data scrambling.
[0034] An error counter in the BIST engine may keep track of the number of errors detected during a test session. This feature may be especially useful in debug.
[0035] The BIST engine 104 may also allow the user to stop BIST on the Nth failure where N is programmable to any number such as below 256. This may further assist in debugging memory failures.
[0036] A second stop option that allows the user to stop BIST at a predefined address also helps in debugging. The stop address may be programmable.
[0037] [0037]FIG. 2 illustrates an exemplary block diagram for an EBIST engine 200 in accordance with an embodiment of the present invention. In one embodiment, the EBIST 104 of FIG. 1 may be implemented as shown in FIG. 2. As shown, the EBIST engine 200 may be partitioned into three blocks: (1) an EBIST controller 202 ; (2) an EBIST data block 204 ; and/or (3) an EBIST address block 206 . It is envisioned that other partitioning may be utilized in various embodiments to provide the EBIST engine 200 .
[0038] In an embodiment, the EBIST controller 202 can include an EBIST instruction register, an EBIST instruction decoder, and/or other logic to provide, for example, flexibility to the user for defining system level tests. In one embodiment, the EBIST controller 202 may start upon receiving a reset signal and an EBIST mode selection signal. The EBIST controller 202 may in turn send control signals to a data generator (such as the EBIST data block 204 ), an address generator (such as the EBIST address block 206 ), and/or an output evaluator (for example, to test the output signals against a known value). Programming of the EBIST controller 202 may be done through an IEEE 1149.1 standard interface (such as that discussed with respect to FIG. 1) and may involve serially shifting in six instructions, a loop bit, and an address step-size through a test data in (TDI) such as those discussed in the IEEE Std 1149.1.
[0039] In a further embodiment, the instruction register may be a 6×7-bit register that can hold six 7-bit instructions. The instruction opcode may be divided into four fields as shown in Table 1 below.
TABLE 1 Fields in the EBIST Instruction Bit Function 0-1 March Element 2-4 Inversion 5 Increment/Decrement Address 6 Address Uniqueness
[0040] In an embodiment for March elements, bits 0 and 1 may be used to encode one of three March elements: 1. “01” for read; 2. “10” for write; and/or 3. “11” for read-write-read. The “00” code may be used to assert the done flag (e.g., indicating that an operation has finished). Using the six instructions, a sequence of six March elements can thus be defined. This allows defining March test algorithms whose complexity can vary between 2N and 18N.
[0041] In another embodiment, the three inversion bits (i.e., bits 2 - 4 ) may be used to specify whether the corresponding March element should use the inverted or non-inverted values of the data background. The function of the three bits may not be limited to just specify the data used for a March element. Instead, these three bits may be used for any combination of the following functions: (1) to define the inversion of the data used for each operation in a read-write-read March element; (2) the inversion bits can be used for forcing an error (this is very useful, for example, as a sanity check to test the EBIST circuitry itself before starting true tests); and/or (3) the same bits may also indicate whether the programmed data background is intended to be used, for example, as part of a checkerboard test where consecutive addresses need to use inverted data. With respect to item (3) above, the case for non-checkerboard tests may be different. In other words, these bits may allow the user to distinguish between a regular March test algorithm and a checkerboard test in an embodiment.
[0042] In one embodiment, bit 5 may indicate whether the address counter should increase or decrease through the address space. In another embodiment, bit 6 may be used to perform a special test on the external memory, referred to as the address uniqueness test. This test can check for address decoder faults that could map one address to many memory locations or many addresses to a single memory location. Bit 6 may override the data background as well as the inversion bits to allow for writing a unique bit vector to each location in the memory and/or read it back. Bit 6 also may override the operand bits by restricting the usage of the address uniqueness test to a single write and/or a single read.
[0043] [0043]FIG. 3 illustrates an exemplary instruction register 300 in accordance with an embodiment of the present invention. The instruction register 300 of FIG. 3 illustrates a configuration in a loop mode as a circular first in, first out (FIFO) buffer. A loop signal 302 may select a loop mode for the instruction register 300 , as illustrated in FIG. 3. The loop signal 302 may act as a select signal for a multiplexer 304 . The loop signal 302 may be provided by a loop register (not shown). In an embodiment, the loop register can be used to allow multiple iterations of the sequence of six March elements programmed through the six instructions discussed with respect to the Table 1. The loop register may be utilized as a high-level loop within which the loops, e.g., in each March element, may be nested. Such an embodiment may be utilized during board/system level debug to determine whether a detected failure is permanent and repeatable and/or is intermittent and dependent on environmental parameters, for example. The loop register may allow the user to run the same tests as many times as desired, for example, under varying environmental parameters, without having to restart the test every time.
[0044] In an embodiment, the instruction register 300 includes six 7-bit registers ( 305 a - f , where 305 c - e are illustrated by the dotted lines) as discussed with respect to the Table 1. The multiplexer 304 receives two input signals 306 and 308 . As illustrated in FIG. 3, in a loop mode, the signal 308 may be fed back to the register 305 a through the multiplexer 304 (via, for example, a 2-bit wide path 310 ), whereas, in a non-loop mode, the signal 306 may be fed back to the register 305 a through the multiplexer 304 . In one embodiment, the seven bits of each instruction can be shifted in parallel in the instruction register 300 (e.g., as a circular FIFO). For example, in one embodiment, the March element field of the register 305 f (Instruction 1) may be fed back into that of the register 305 a (Instruction 6) through the multiplexer 304 (via, for example, a 2-bit wide path 310 ), so that when the loop signal 302 is not set, a “00” vector (as signal 306 ) is automatically loaded into the register 305 a (Instruction 6) indicating completion of the six instruction March test.
[0045] In an embodiment, an address step size register (not shown) can be utilized to program the step size associated with the addresses. The address step size may be coupled with the address incrementer/decrementer for generating the test address. The address step size register may be programmable through a 3-bit step size register that allows address steps of 4, 8, 16, 32, 64, 128, or 512 bits. In an embodiment, the EBIST implementation described herein may send requests to the external RAM in bursts of four addresses in each transaction with the memory. This may be a restriction of the existing external memory controller. This feature allows the user to reduce test time, if needed, at the expense of some loss of test coverage. This is especially useful in production test flows where a full EBIST test is run at a first test step and a smaller test is run at subsequent test steps. The step size information may be sent to an address generator (such as 206 of FIG. 2) as well as a data generator (such as 204 of FIG. 2) to effect proper control of write and read operations to the memory.
[0046] In one embodiment, the address generator (such as 206 of FIG. 2) can be an ordinary up-down counter that takes inputs from the step size register and the instruction register (specifically its increment/decrement bit), such as that discussed with respect to FIG. 3. For the address uniqueness test purpose, the address generator may send the current address to the data generator. For start and end addresses, a user may program a specific start address and an end address used by the address generator as first and last addresses, respectively. This feature may be another way to reduce test time. One of its uses may be in debug where the user may need to narrow down the search for a failing address to within a range, for example. This address range may be specified using a start and an end address. Another use of this feature may be during verification where it would be infeasible to simulate EBIST operations running through a relatively large (e.g., 16 GB) address space. For example, in the case of a 16-GB memory with a 30-bit address bus, simulation of EBIST for the full address space at the gate level can result in simulation times in the range of weeks. By programming the address space, one may be able to target corner cases and run regressions with reasonable simulation times (e.g., reducing simulation time from weeks to less than an hour).
[0047] In a further embodiment, the data generator (such as 204 of FIG. 2) can include two main functions: (1) generating data that is written to the memory in write mode; and (2) comparing the data read from the memory with the expected data in read mode. In addition, some debug capabilities may be also implemented in the data generator such as: (a) dump on error; (b) dump on address; and (c) an error counter. Such additional features may be helpful, especially as the size of the memory circuits increase.
[0048] In another embodiment, a data background register (not shown) can be coupled to an IEEE 1149.1 standard interface for programming (i.e., input) and connect to the output data of the BIST module. The data background register may hold the bit vector (or its inversion) that is written into the memory by the test algorithm. The width of the data background register can be the same as the data width of the memory, in an embodiment. This value may also be used as expected data for comparison with data read from the memory. The data background can be programmable through the IEEE 1149.1 standard interface. This permits the user to perform March and checkerboard test algorithms with different data backgrounds to ensure relatively high test coverage of the external memory.
[0049] In yet another embodiment, either (or both) of two debug capabilities can be implemented inside the data generator (such as 204 of FIG. 2), namely, a dump-on-error and dump-on-address. The data generator may include three registers to implement the two modes in one embodiment. In an embodiment, an error counter may be utilized. The error counter can be initialized to, for example, “0” at the beginning of an EBIST run and then incremented whenever an error is detected. In an embodiment of the present invention, the dump-on-error register may be implemented as a 5-bit register that can be programmed (e.g., through the IEEE 1149.1 standard interface) with an integer up to 31, for example. If the error counter value becomes equal to the value of the dump-on-error register, the failing address and the failing data may be captured into copy (or shadow) register(s). At the end of the test run, the contents of the copy registers may be shifted out through, for example, the IEEE 1149.1 standard interface.
[0050] Moreover, in an embodiment of the present invention, a dump-on-address register may be programmed to contain a specific address. Whenever the read address becomes equal to the one stored by the dump-on-address register, the content of the failing address and the failing data may be captured into copy (shadow) register(s). The stored data can subsequently be shifted out at the end of the test session. In one embodiment, only one of the two debug capabilities can be active at any time. For example, the built-in priority may allow the dump-on-address function to be active only when the dump-on-error register is set to “0” or inactive. These two modes may be used either to perform a fail address man or to debug the memory controller and/or EBIST interface.
[0051] Furthermore, in an embodiment, the data generator may have one or more of two operation modes, such as a standard mode and an address uniqueness mode. In the standard mode, during a write sequence, the data generator may use the inversion bits (e.g., bits 2 - 4 , see Table 1) of the active instruction sent by a controller (such as 202 of FIG. 2) to determine whether to write the stored data background or its inversion. For a read operation, the data generator may use a “data valid” signal, for example, sent by a memory controller, to decide when to perform a compare. The data generator may provide the expected data as well as the data received from the memory to a comparator. The comparator may receive as inputs the read data from the memory and the expected value. The comparator's output may be provided as an output of the IC and/or stored in a register (for example, for future retrieval). In an embodiment, the comparator may reside within the data generator. In the event of an error, the comparator may send a signal to a primary output that is held at that value for a certain number of clock cycles to satisfy the CPU/system clock ratio. The output of the comparator may also be used to increment an error counter that can be shifted out at the end of the test sequence, for example.
[0052] The address uniqueness mode may implement a 2N test, in one embodiment, where:
[0053] 1. In a first pass through the address space a unique bit vector is written into each location of the memory. The data generator may accomplish this by taking the current address from the address generator and replicating it to fit the data width.
[0054] 2. In a second pass, a “data valid” signal may be used to control a counter that is initialized to the first written address location (e.g., in step 1 above). The counter may then keep track of subsequent data received from the memory by incrementing its contents. The counter may also replicate the read unique data (in this case the address) to fit the data width.
[0055] In one embodiment, when the chip comes out of a reset, the default state of the EBIST controller can be setup to perform a March C test with the full address range and the background set to a All-0 pattern.
[0056] To program a simple March C test, five of the six instruction registers (such as those of FIG. 3) may be used as shown in Table 2 below.
TABLE 2 Instruction Sequences for a March 13N Test Register March Element Inv I/D U Register 1 10 000 0 0 Register 2 11 011 0 0 Register 3 11 100 1 0 Register 4 11 011 1 0 Register 5 11 100 0 0
[0057] This kind of programmability is also useful for initializing the contents of the memory. In such a case, it may only be necessary to use the first register.
[0058] To program a simple test sequence, the sequence of instructions shown in Table 3 may be utilized (which performs an address uniqueness test followed by a 10N March test).
TABLE 3 Alternative Sequence of Instructions Defining a 12N Test of the Memory Register March Element Inv I/D U Register 1 10 XXX 0 1 Register 2 01 XXX 0 1 Register 3 10 000 0 0 Register 4 11 011 0 0 Register 5 11 100 1 0 Register 6 11 011 1 0
[0059] In one embodiment, the implementation of the EBIST engine (such as 200 of FIG. 2) may be done for a processor or application-specific IC (ASIC), available for example from Sun Microsystems, Inc., of Santa Clara, Calif. The control block may be synthesized using Synopsys' Design Compiler. The place and route may be done using Cadence's SiliconEnsemble. The area of the controller may reach about 1350μ×147μ for a 0.15μ technology. The address generator and data generator may be constructed as data paths using an appropriate placement tool and Cadence's ICCraftsman router, for example. The address block size may reach about 825μ×463μ and the data block may reach about 1369μ×1456μ for a 0.15μ technology.
[0060] Accordingly, in an embodiment, an implementation of an instruction-based on-chip BIST engine for testing external memories/caches has been presented. The proposed scheme offers high quality tests along with a significant level of flexibility for board level and system level test and debug of external memories. Some of the goals achieved by various embodiments of the present invention, individually or in combination, include, but are not limited to: enabling at-speed and high coverage testing of external memories, reducing test costs by reducing the test fixture capital, reducing test costs by allowing test at an earlier stage, reducing test costs by reducing test time by a factor of about ten compared to conventional POST programs used today, reducing test costs by increasing the reliability of measurements compared to that of conventional POST, significantly improving debug capabilities for failures detected in the memory subsystem, providing an adaptable environment for test (e.g., the test sequence can be programmed depending of the memory vendor and customer requirement), and/or minimizing the impact on the existing design by reusing features of the memory controller engine and/or by leaving the critical paths untouched.
[0061] The foregoing description has been directed to specific embodiments. It will be apparent to those with ordinary skill in the art that modifications may be made to the described embodiments, with the attainment of all or some of the advantages. For example, the techniques of the present invention may be applied to very large-scale integrated (VLSI) logic and/or circuit modules. In addition, any type of memory may be tested in accordance with various embodiments of the present invention regardless of the memory's logic, organization, and/or structure, for example. Therefore, it is the object of the appended claims to cover all such variations and modifications as come within the spirit and scope of the invention.
|
Disclosed are novel methods and apparatus for efficiently providing instruction-based BIST of external memory. In an embodiment, a built-in self-testing system is disclosed. The system includes an external memory module, an on-chip memory controller coupled to the external memory module, an on-chip built-in self-test (BIST) module coupled to the on-chip memory controller, and an interface controller coupled to the BIST module to provide an interface to access the BIST module. The on-chip memory controller may send and receive data to and from the external memory module. And, the BIST module may include an instruction register to store a plurality of instructions.
| 6
|
RELATED APPLICATIONS
[0001] The present application is related to U.S. Pat. No. 6,788,796 for DIFFERENTIAL MICROPHONE, issued Sep. 7, 2004; and copending U.S. patent application Ser. No. 10/689,189 for ROBUST DIAPHRAGM FOR AN ACOUSTIC DEVICE, filed Oct. 20, 2003, and Ser. No. 11/198,370 for COMB SENSE MICROPHONE, filed Aug. 5, 2005, all of which are incorporated herein by reference.
[0002] This invention was made with U.S. Government Support under contract R01DC005762 awarded by the NIH. The government has certain rights in the invention.
FIELD OF THE INVENTION
[0003] The present invention pertains to microphones and, more particularly, to micromachined differential microphones and optical interferometry to produce an electrical output signal.
BACKGROUND OF THE INVENTION
[0004] Low noise and low power are essential characteristics for hearing aid microphones. Most high performance microphones, and particularly miniature microphones, consist of a thin diaphragm along with a spaced apart, parallel back plate electrode; they use capacitive sensing to detect diaphragm motion. This permits detecting the change in capacitance between the pressure-sensitive diaphragm and the back plate electrode. In order to detect this change in capacitance, a bias voltage must first be imposed between the back plate and the diaphragm.
[0005] This voltage creates practical constraints on the mechanical design of the diaphragm that compromise its effectiveness in detecting sound. Specifically, inherent in the capacitive sensing configuration are a few limitations. First, viscous damping caused by air between the diaphragm and the back plate can have a significant negative effect on the response. Second, the signal to noise ratio is reduced by the electronic noise associated with capacitive sensing and the thermal noise associated with a passive damping. Moreover, due to the viscosity of air, a significant source of microphone self noise is introduced. Third, while the electrical sensitivity is proportional to the bias voltage, when the voltage exceeds a critical value, the attractive force causes the diaphragm to collapse against the back plate.
[0006] To illustrate the limitations imposed on the noise performance of the read-out circuitry used in a capacitive sensing scheme, consider the buffer amplifier having a white noise spectrum given by N volts/√Hz. If the effective sensitivity of the capacitive microphone is S volts/Pascal then the input-referred noise is N/S Pascals/√Hz.
[0007] In a conventional capacitive microphone, the sensitivity may be approximated by:
[0000]
S
=
V
b
A
hk
(
1
)
[0000] where V b is the bias voltage, A is the area, h is the air gap between the diaphragm and the back plate, and k is the mechanical stiffness of the diaphragm.
[0008] For purposes of this discussion, assume that the resonant frequency of the diaphragm is beyond the highest frequency of interest. The input referred noise of the buffer amplifier then becomes:
[0000]
N
S
=
Nhk
V
b
A
pascals
/
MHz
(
2
)
[0009] Theoretically, this noise can be reduced by increasing the bias voltage, V b , or by reducing the diaphragm stiffness, k. Unfortunately, these parameters cannot be adjusted independently because the forces that are created by the biasing electric field can cause the diaphragm to collapse against the back plate. In a constant voltage (as opposed to constant charge) biasing scheme, the collapse voltage is given by:
[0000]
V
collapse
=
8
27
kh
3
ɛ
A
0
(
3
)
[0000] where ε is the permittivity of the air in the gap. Diaphragms that have low equivalent mechanical stiffness, k, have low collapse voltages. To avoid collapse, V b <<V collapse .
[0010] Equation 3 clearly shows that the collapse voltage can be increased by increasing the gap spacing, h. Increasing h, however, reduces the microphone capacitance, which is inversely proportional to the nominal gap spacing, h. Since miniature microphones, and particularly silicon microphones, have very small diaphragm areas, A, the capacitance tends to be rather small, on the order of 1 pF. The small capacitance of the microphone challenges the designer of the buffer amplifier because of parasitic capacitances and the effective noise gain of the overall circuit.
[0011] For these reasons, the gap, h, used in silicon microphones tends to be small, on the order of 5 μm. The use of a gap that is as small as 5 μm introduces yet another limitation on the performance that is imposed by capacitive sensing. As the diaphragm moves in response to fluctuating acoustic pressures, the air in the narrow gap between the diaphragm and the back plate is squeezed and forced to flow in the plane of the diaphragm. Because h is much smaller than the thickness of the viscous boundary layer (typically on the order of hundreds of μm), this flow produces viscous forces that damp the diaphragm motion. It is well known that this squeeze film damping is a primary source of thermal noise in silicon microphones.
[0012] The optical sensing approach hereinafter described is intended to be used with the microphone diaphragms described in Cui, W. et al., “Optical Sensing in a Directional MEMS Microphone Inspired by the Ears of the Parasitoid Fly, Ormia Ochracea ”, January, 2006. These diaphragms incorporate carefully designed hinges that control their overall compliance and sensitivity. By combining the inventive optical sensing approach with these microphone diaphragm concepts, miniature microphones can be manufactured with extremely high sensitivity and low noise. Low noise, directional miniature microphones can be fabricated with high sensitivity for hearing aid applications. Incorporation of optical sensing provides high electrical sensitivity, which, combined with the high mechanical sensitivity of the microphone membrane, results in a low minimum detectable pressure level.
[0013] Although optical interferometry has long been used for low noise mechanical measurements, the high voltage and power levels needed for lasers and the lack of integration have prohibited the application of this technique to micromachined microphones. These limitations have recently been overcome by methods and devices as described by Degertekin et al. in U.S. Pat. No. 6,567,572 for “Optical Displacement Sensor,” copending U.S. patent application Ser. No. 10/704,932, filed by Degertekin et al. on Nov. 10, 2003 for “Highly-Sensitive Displacement Measuring Optical Device”, and copending U.S. patent application Ser. No. 11/297,097, for “Displacement Sensor”, filed by Degertekin et al. Dec. 8, 2005
[0014] , all hereby incorporated by reference in their entirety.
[0015] It is, therefore, an object of the invention to provide a MEMS differential microphone having enhanced sensitivity.
[0016] It is another object of the invention to provide a MEMS differential microphone having optical means for converting sound-induced motion of the diaphragm into an electronic signal.
[0017] It is an additional object of the invention to provide a MEMS differential microphone exhibiting a first order differential response to provide a directional microphone.
[0018] It is a further object of the invention to provide a MEMS differential microphone having a silicon membrane diaphragm and protective front screen fabricated using silicon micro-fabrication techniques.
[0019] It is yet another object of the invention to provide a MEMS differential microphone having low power consumption.
[0020] It is a still further object of the invention to provide a MEMS differential microphone suitable for use in hearing aids.
[0021] It is another object of the invention to provide a MEMS differential microphone using a optical interferometer to convert sound impinging upon the microphone to an electrical output signal.
[0022] It is an additional object of the invention to provide a MEMS differential microphone wherein the optical interferometer is implemented using a miniature laser such as a vertical cavity surface emitting laser (VCSEL).
SUMMARY OF THE INVENTION
[0023] In accordance with the present invention, there is provided a microphone having optical means for converting the sound-induced motion of the microphone diaphragm into an electronic signal. A diffraction device (e.g., a diffraction grating or, in alternate embodiments, inter-digitated fingers) is integrated with the microphone diaphragm to implement an optical interferometer which has the sensitivity of a Michelson interferometer. Because of the unique construction, the bulky and heavy beam splitter normally required in a Michelson interferometer is eliminated allowing a miniature, lightweight microphone to be fabricated. The microphone has a polysilicon diaphragm formed as a silicon substrate using a combination of surface and bulk micromachining techniques.
[0024] The approximately 1 mm×2 mm microphone diaphragm has stiffeners formed on a back surface thereof. The diaphragm rotates or “rocks” about a central pivot or hinge thereby providing differential response. The diaphragm is designed to respond to pressure gradients, giving it a first order directional response to incident sound.
[0025] The inventive microphone diaphragm coupled with a diffraction-based optical sensing scheme provides directional response in a miniature MEMS microphone. This type of device is especially useful for hearing aid applications where it is desirable to reduce external acoustic noise to improve speech intelligibility.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] A complete understanding of the present invention may be obtained by reference to the accompanying drawings, when considered in conjunction with the subsequent detailed description, in which:
[0027] FIGS. 1 a and 1 b are schematic, side, sectional and schematic perspective views, respectively, of the optical sensing, differential microphone of the invention;
[0028] FIGS. 2 a , 2 b , and 2 c are schematic plan views of a diaphragm of the microphone of FIGS. 1 a and 1 b incorporating a diffraction apparatus comprising a diffraction grating, interdigitated fingers, and slits, respectively;
[0029] FIGS. 3 a , 3 b and 3 c are calculated reflected diffraction patterns using scalar far-field diffraction formulation for gap values of λ/2, λ/4, and λ/8, respectively;
[0030] FIG. 4 is a plot of normalized intensity vs. gap for the microphone of FIG. 1 ;
[0031] FIG. 5 is a plot of calculated minimum detectable displacement of the diaphragm of the microphone of FIG. 1 as a function of total optical power incident on the photodetectors;
[0032] FIGS. 6 a - 6 d are a fabrication process flow showing a set of possible fabrication steps useful for forming the microphone of FIGS. 1 a and 1 b;
[0033] FIGS. 7 a and 7 b are a front side optical and a rear side SEM view of the diaphragm of the microphone of FIGS. 1 a and 1 b ; and
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0034] Generally speaking, the present invention is a directional microphone incorporating a diaphragm, movable in response to sound pressure and an optical sensing mechanism for detecting diaphragm displacement. The diaphragm of the microphone is designed to respond to pressure gradients, giving it a first order directional response to incident sound. This mechanical structure is integrated with a compact optical sensing mechanism that uses optical interferometry to generate an electrical output signal representative of the sound impinging upon the microphone's diaphragm. The novel structure overcomes adverse effects of capacitive sensing of microphones of the prior art.
[0035] One of the main objectives of the present invention is to provide a differential microphone suitable for use in a hearing aid and which uses optical sensing in cooperation with a micromachined diaphragm. Of course other applications for sensitive, miniature, directional microphones are within the scope of the invention. Optical sensing provides high electrical sensitivity, which, in combination with high mechanical sensitivity of the microphone membrane, results in a small minimum detectable sound pressure level.
[0036] Although optical interferometry has long been used for low noise mechanical measurements, the large size, high voltage and power levels needed for lasers, and the lack of integration have heretofore prohibited the application of optical interferometry to miniature, micromachined microphones. These limitations have recently been overcome by methods and devices as described in U.S. Pat. No. 6,567,572 for OPTICAL DISPLACEMENT SENSOR, issued May 20, 2003 to Degertekin et al. and U.S. patent application Ser. No. 10/704,932, for HIGHLY SENSITIVE DISPLACEMENT MEASURING OPTICAL DEVICE, filed Nov. 10, 2003 by Degertekin et al.
[0037] Referring first to FIGS. 1 a and 1 b , there are shown schematic, side, cross-sectional and schematic, perspective views, respectively, of a microphone assembly incorporating an optical interferometer in accordance with the present invention, generally at reference number 100 . A diaphragm 102 having stiffeners 104 disposed upon a rear surface 106 thereof is free to “rock” (i.e., rotate) about a hinge 108 in response to sound pressure (shown schematically as arrow 110 ) impinging thereupon. A diffraction mechanism 120 is operatively connected to diaphragm 102 . Diffraction mechanism 120 may be implemented in a variety of ways. As shown in FIGS. 1 a and 1 b , diffraction mechanism 120 is a diffraction grating 120 a ( FIG. 2 a ), typically disposed centrally in diaphragm 102 close to its edge where deflection is large. A reflective diffraction grating 120 a having a period of approximately 1 μm has been found suitable for use in the application. It will be recognized, however, that a laser operating at a different wavelength may require a different periodicity in a diffraction grating. The diffraction grating can be curved to implement a diffractive lens to steer and focus the reflected beam to obtain a desired light pattern on the photodetector plane.
[0038] In alternate embodiments, slits 120 c ( FIG. 2 c ) may be disposed in diaphragm 102 to provide the required diffraction function. In still other embodiments, interdigitated fingers 120 b ( FIG. 2 b ) can provide the required diffraction function. An embodiment using interdigitated fingers is described in detail hereinbelow. It will be recognized that other means for implementing diffraction mechanism 120 may exist and the invention is, therefore, not considered limited to the devices chosen used for purposes of disclosure. Rather the invention contemplates any and all suitable diffraction mechanisms. Hereinafter, the term diffraction mechanism is used to refer to any diffraction device suitable for use in practicing the instant invention.
[0039] A protective screen 112 is disposed intermediate a sound source 110 and a front face of diaphragm 102 . Screen 112 is isolated therefrom by a layer 136 , typically formed from silicon dioxide or the like. In the preferred embodiment, protective screen 112 consists of a micromachined silicon plate that contains a plurality of very small holes, slits, or other orifices 114 sized to exclude airborne particulate contamination (e.g., dust) from diaphragm 102 and other interior regions, not shown, of microphone 100 . The small holes 114 , however, allow the passage of sound pressure 110 .
[0040] A lower surface of protective screen 112 bears an electrically conductive (typically metallic) layer 118 used to apply a voltage dependent force (i.e., a mechanical bias) to diaphragm 102 as described in detail hereinbelow. The application of a voltage dependent force enables optimizing the position of diaphragm 102 to achieve maximum sensitivity of the optical sensing portion of microphone 100 . Conductive layer 118 , in addition to helping provide a voltage dependent force, also provides an optically reflective surface that enables the detection of interference fringes between the reflected light from the diffraction mechanism 120 (e.g., optical grating 120 a , etc.) incorporated on/into diaphragm 102 and screen 112 disposed forward of diaphragm 102 . Screen 112 must be as stiff as possible so that the reflective surface of conductive layer 118 is mechanically stable with respect to movements of diaphragm 102 . The reflective rear surface of conductive layer 118 forms a fixed mirror portion of the optical interferometer. Screen 112 is integrally attached to diaphragm 102 and manufactured as part of the micromachining process used to form forming microphone 100 . The micromachining process is described in detail hereinbelow.
[0041] A miniature vertical cavity surface emitting laser (VCSEL) 122 is disposed behind diaphragm 102 , typically on or in a bottom chip 140 . Bottom chip 140 is typically attached to the remainder of microphone 100 by a bonding layer 138 . Coherent light 132 from VCSEL 122 is directed toward diffraction mechanism 120 . A Model VCT-F85-A32 VCSEL supplied by Lasermate Corp. operating at a wavelength of approximately 0.85 μm with an aperture of approximately 9 μm has been found suitable for the application. It will be recognized, however, that other similar coherent light sources provided by other vendors may be suitable for the application. Consequently, the invention is not limited to a particular model or operating wavelength but includes any suitable coherent light source operating at any wavelength.
[0042] An array of photodetectors 124 is also disposed behind diaphragm 102 . In the embodiment chosen for purposes of disclosure, a linear array of three photodetectors 124 appropriately spaced to capture the zeroth and first orders of refracted light as described hereinbelow. In some embodiments, VCSEL 122 , can be tilted with respect to the plane of the photodetectors so that the reflected diffraction orders are efficiently captured by the array of photodetectors 124 .
[0043] In other embodiments, the miniature laser and the array of photodetectors can be formed on the same substrate, such as a gallium arsenide semiconductor material.
[0044] The components shown schematically in FIG. 1 implement a Michelson interferometer complete in a small volume. Such a compact arrangement including a low power laser and detection electronics is suitable for use in hearing aids and other miniature devices requiring a microphone.
[0045] The diffraction grating 120 a or other diffraction apparatus 120 on the microphone diaphragm 102 and the reflective surface of metallic coating 118 on the protective screen 112 together form a phase-sensitive diffraction grating. Such structures are used to detect displacements as small as 2×10−4 Å/√Hz in atomic force microscope (AFM), micromachined accelerometer, and acoustic transducer applications.
[0046] When the structure of FIG. 1 is illuminated from the back side using coherent light source 122 , light reflects both from the diffraction mechanism 120 (e.g., diffraction grating 120 a ) that is integrated into diaphragm 102 and from coating 118 of protective screen 112 , reference numbers 128 , 130 , respectively. While reflected light 128 , 130 is shown schematically as rays, it will be recognized that the reflected diffraction orders have a beam shape of finite effective size determined by the light distribution at the laser source, the shape and curvature of the diffraction mechanism 120 , and the distance traveled by the light 128 , 130 . In the ideal case of a linear grating with 50% fill factor, i.e. equal amount of light reflection from the diffraction mechanism and the coating of the protective screen the reflected light 128 , 130 has odd diffraction orders in addition to the normal specular reflection.
[0047] In an alternate embodiment of the inventive microphone, interdigitated fingers 120 b ( FIG. 2 b ) bearing reflective rear surfaces may be used to form both the fixed and movable mirrors necessary to form the optical interferometer. The use of the fixed interdigitated fingers as the stationary mirror allows the elimination of a reflective surface on screen 112 . Reflective rear surfaces on the movable fingers form the movable mirror. Interdigitated fingers are described in detail in copending U.S. patent application Ser. No. 11/198,370. Interdigitated fingers 120 b are typically disposed at the end of diaphragm 102 to maximize the relative motion of the fingers relative to associated fixed fingers. It will be recognized, however, that the interdigitated fingers may be disposed at other locations around the perimeter of diaphragm 102 . It will also be recognized that multiple, independent sets of interdigitated fingers, each associated with its own optical pickup system, may be used to differentially sense an electrical signal from diaphragm 102 of microphone 100 . It may be desirable under certain operating conditions to use such a differential arrangement to overcome outputs caused by in-phase motion of the diaphragm 102 .
[0048] In embodiments utilizing interdigitated fingers, fingers of approximately 100 μm length and 1 μm width having approximately 4 μm periodicity have been found suitable for the application. While the aforementioned dimensions have been determined by detailed finite element analysis, other interdigitated geometries, of course, may be used. Interdigitated fingers may be disposed at one or both ends of diaphragm 102 where deflection thereof is greatest. In alternate embodiments, one or more groups of interdigitated fingers may be disposed at any position on the perimeter of diaphragm 102 .
[0049] Referring now to FIGS. 3 a , 3 b , and 3 c , there are shown calculated reflected diffraction patterns for various gap values at the surface of the silicon wafer, which carries the photodetectors and associated CMOS electronics, not shown. FIGS. 3 a , 3 b , and 3 c represent gap spacing of λ/2, λ/4, and λ/8, respectively. These calculations are performed using scalar diffraction theory with 1 μm periodicity.
[0050] Optical output signals can be converted to electrical signals by placing three 100 μm by 100 μm silicon photodetectors at x=0, and x=±150 μm to capture the zero and first orders. The intensities, I 0 and I 1 can be expressed as a function of the gap thickness, d 0 128 ( FIG. 1 ), between the microphone diaphragm 102 and the protective screen 112 ( FIG. 1 ) and may be computed as:
[0000]
I
0
=
I
in
cos
(
2
Π
d
0
λ
0
)
I
1
=
4
I
in
Π
2
sin
2
(
2
Π
d
0
λ
0
)
(
4
a
,
4
b
)
[0051] As may be seen in FIG. 4 , the maximum displacement sensitivity is obtained when d o is biased to an odd multiple of λ 0 /8. It can be shown that for small displacements, Δx, around this bias value, the difference in the output currents of the photodetectors detecting these orders, i is given by the equation:
[0000]
i
=
R
∂
(
I
0
-
α
I
1
)
∂
d
0
Δ
x
=
RI
in
4
Π
λ
0
Δ
x
(
5
)
[0000] where I in is the incident laser intensity and R is the photodetector responsivity. It may be concluded, therefore, that the inventive structure provides the sensitivity of a Michelson interferometer for small displacements of the microphone diaphragm with the following advantages:
The bulky beam splitter typically required in a Michelson interferometer is eliminated enabling construction of a miniature interferometer. Both the reference reflector and moving reflector (grating) are on the same substrate, thereby minimizing spurious mechanical noise. The small distance between the grating 120 and the protective screen 112 (≈5 μm) enables the use of low power, low voltage VCSELs with short (i.e., 100-150 μm) coherence length as light sources for the interferometer. The novel interferometer construction enables integration of photodetectors and electronics in small volumes (i.e., ≈1 mm 3 ).
[0056] Since the curves in FIG. 4 are periodic, it will be recognized that the microphone diaphragm 102 ( FIG. 1 ) need only be moved λ 0 /4 to maximize the microphone sensitivity. In some embodiments where the grating period is comparable to the wavelength λ 0 , a more accurate calculation of the diffraction patterns should be performed taking the vectorial nature of the light propagation into account. As shown in the reference by W. Lee and F. L. Degertekin, “Rigorous Coupled-wave Analysis of Multilayered Grating Structures,” IEEE Journal of Lightwave Technology, 22, pp. 2359-63, 2004, the diffraction order intensity variation with the gap thickness, d 0 128 can be different than the simple relation in Equation 4. However, since the sensitivity variation has its maxima and minima with close to λ 0 /2 periodicity, to obtain maximum sensitivity the microphone diaphragm 102 needs only to be moved less than λ 0 /2 to maximize the microphone sensitivity. In the novel microphone design, a bias voltage in the range of approximately 1-2 V applied between the membrane (i.e., diaphragm 102 ) and the protective screen 112 is sufficient to accomplish displacements of this magnitude. The selective application of such a bias voltage, therefore, overcomes process variations. During microphone fabrication, applying bias voltages suitable for hearing aids or other intended applications results in a robust design.
[0057] The use of a miniature laser is important when implementing the optical sensing method of the invention. The recent availability of VCSELs, for example, is helpful in creating a practical differential microphone using optical sensing. These efficient micro-scale lasers have become available due to recent developments in opto-electronics and optical communications. VCSELs are ideal for low voltage, low power applications because they can be switched on and off, typically using 1-2V pulses with threshold currents in the 1 mA range to reduce average power. VCSELs having threshold currents below 400 pA are available. The noise performance of VCSELs has also been improving rapidly. This improvement helps make them suitable for sensor applications where high dynamic ranges (e.g., in the 120-130 dBs) are desirable. Furthermore, using the differential detection scheme (between I 1 and I ±1 , in Equation (5)), the intensity noise is reduced to negligible levels.
[0058] One important concern with optical detection methods is power consumption. Given the mechanical sensitivity of the microphone diaphragm 102 in m/Pa, the minimum detectable displacement (MDD) determines the power consumption. As an example, for a typical differential microphone diaphragm suitable for use in the optical sensing microphone of the invention, having a mechanical sensitivity of 10 nm/Pa, an input sound pressure referred noise floor of 15 dBA SPL requires an MDD of 1×10 −4 Å/√Hz. To predict the power consumption required for this MDD, a noise analysis of the photodetector-amplifier system has been performed based on an 850 nm VCSEL as the light source and responsivity of the photodetector, R=0.5 A/W.
[0059] A transimpedance configuration formed using a commercially available micro power amplifier (Analog Devices OP193, 1.7V, 25 , uW, e n =65 nV/VHz, in =0.05 pA/√Hz) was analyzed. Transimpedance amplifier topologies are known to those of skill in the art and are not further disclosed herein. FIG. 5 shows the MDD as a function of the average laser power with a 1 MO feedback resistor. Due to the high electrical sensitivity of the optical sensing technique, the displacement noise is dominated by the shot noise. Hence, custom designed CMOS amplifiers with a 1V supply voltage and 5 pW power consumption may be used without affecting the photodiode-dominated noise floor. Then, the power consumption of the microphone can be estimated from the laser power required for a given displacement noise from the shot noise relation:
[0000]
2
q
I
peak
2
R
=
4
Π
2
λ
4
Π
I
peak
R
x
n
λ
⇒
x
n
=
2
q
I
peak
R
(
6
)
[0060] The results show that the average laser power required for 1×10 −4 Å/√Hz, is an MDD of approximately 20 pW. Similar values (e.g., 5.5×10 −4 Å/√Hz with 3 pW optical power) have already been achieved in some AFM applications. This average power may be achieved using the VCSEL in the pulsed mode as described in copending U.S. patent application Ser. No. 11/297,097
[0061] filed by Degertekin et al. on Dec. 8, 2005 for “Displacement Sensor”. Assuming 30% wall plug efficiency for the VCSEL, 20 pW optical power can be obtained with about 80 pW input power including optical losses. See http://www.ulm-photonics.de. Therefore, it is possible to achieve a 15 dBA noise floor using an optical sensing technique with total power consumption of less than 100 pW, including associated electronics, which is comparable to the power consumption of a directional hearing aid with two electret microphones (for example, a Knowles electronics model EM series). Furthermore, the development of more efficient VCSELs in the pulse-modulation mode is expected to help reduce both the power consumption and to improve of low-frequency amplifier noise.
[0062] Implementation of the photodetectors 124 with integrated amplifiers in CMOS technology is facilitated by the fact that the proposed optical sensing scheme does not impose strict design requirements with the exception of the low power consumption.
[0063] Referring now to FIGS. 6 a - 6 d , there is shown the fabrication process flow for the microphone diaphragm 102 . Many ways may be found to fabricate the microphone of the present invention. The following exemplary method has been successfully utilized to fabricate the diaphragm 102 membrane and diffraction mechanism 120 . The micromachining fabrication technique uses deep-trench etching and sidewall deposition to create very lightweight, very stiff membranes with stiffening ribs at optimal locations.
[0064] As shown in FIG. 6 a , the fabrication starts with a deep reactive ion trench etch into the 4-inch test grade silicon wafer 150 forming trenches 152 that act as the molds for the polysilicon stiffeners 104 ( FIGS. 1 a , 1 b ).
[0065] The etching process is followed by a wet oxidation at approximately 1100° C. to grow an approximately one-micron thick thermal oxide layer 154 on the wafer 150 surface and in the trenches 152 as shown in FIG. 6 b.
[0066] As seen in FIG. 6 b , oxide layer 154 acts as an etch stop for a subsequent back side cavity etching step that removes the bulk of the silicon wafer 150 from the region 156 behind what will be the diaphragm. A film of polysilicon 158 is next deposited and planerized to form a flat diaphragm surface 102 having stiffeners 104 formed on a rear surface thereof. Typically phosphorus-doped polysilicon is deposited at approximately 580° C. and subsequently annealed at 1100° C. in argon gas for approximately 60 minutes. The annealing step reduces intrinsic stress in the film 158 .
[0067] The back cavity region 156 is then etched using a deep reactive ion etch and the thermal oxide layer 154 is removed in buffered oxide etch (BOE). The final step is to etch the polysilicon 158 to define the interdigitated fingers 162 and slits 164 that separate the diaphragm 102 from the substrate 150 .
[0068] Referring now also to FIGS. 7 a and 7 b , there are shown front-side optical and back side schematic views, respectively, of the microphone diaphragm and interdigitated fingers formed in accordance with the forgoing fabrication process. FIG. 7 a shows the front surface 160 . The interdigitated fingers and slits 162 , 164 on each end of the diaphragm 102 extend into the polysilicon layer connected to the silicon substrate 150 .
[0069] The microphone diaphragm 102 is separated from the substrate with an approximately 2 μm gap around the edge and the center hinges for acoustical damping and electrical isolation.
[0070] The details of the interdigitated fingers can be seen in FIG. 7 c that also shows the stiffeners 104 on the diaphragm 102 as dark lines on the left, whereas the stationary fingers 162 extend from the polysilicon layer attached to the substrate on the right.
[0071] It will be recognized that other fabrication processes and/or materials may be used to form structures similar to that described herein. The invention, therefore, is not limited to the fabrication steps and/or material chosen for purposes of disclosure. Rather, the invention contemplates any and all fabrication processes and materials suitable for forming a microphone as described herein.
REFERENCES
[0072] Hall N. and Degertekin F. L., An Integrated Optical Detection Method for Capacitive Micromachined Ultrasonic Transducers , Proceedings of 2000 IEEE Ultrasonics Symposium, pp. 951-954, 2000.
[0073] Hall N. A. and Degertekin F. L., An Integrated Optical Interferometric Detection Method for Micromachined Capacitive Acoustic Transducers , Appl. Phys. Lett., 80, pp. 3859-61 2002.
[0074] W. Lee and F. L. Degertekin, Rigorous Coupled - wave Analysis of Multilayered Grating Structures , IEEE Journal of Lightwave Technology, 22, pp. 2359-63, 2004
[0075] W. Cui, B. Bicen, N. Hall, S. A. Jones, F. L. Degertekin, and R. N. Miles Proceedings of 19 th IEEE International Conference on Micro Electro Mechanical Systems (MEMS 2006 ) , Jan. 22-26, 2006, Istanbul, Turkey. Optical sensing in a directional MEMS microphone inspired by the ears of the parasitoid fly, Ormia ochracea
[0076] Since other modifications and changes varied to fit particular operating requirements and environments will be apparent to those skilled in the art, this invention is not considered limited to the example chosen for purposes of this disclosure, and covers all changes and modifications which does not constitute departures from the true spirit and scope of this invention.
[0077] Having thus described the invention, what is desired to be protected by Letters Patent is presented in the subsequently appended claims.
|
A microphone having an optical component for converting the sound-induced motion of the diaphragm into an electronic signal using a diffraction grating. The microphone with inter-digitated fingers is fabricated on a silicon substrate using a combination of surface and bulk micromachining techniques. A 1 mm×2 mm microphone diaphragm, made of polysilicon, has stiffeners and hinge supports to ensure that it responds like a rigid body on flexible hinges. The diaphragm is designed to respond to pressure gradients, giving it a first order directional response to incident sound. This mechanical structure is integrated with a compact optoelectronic readout system that displays results based on optical interferometry.
| 7
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a joined structure of different metals which has improved corrosion resistances at the joined interface. The present invention also relates to a friction welding method that is desirably used for manufacturing the above-mentioned joined structure of different metals.
[0003] 2. Description of the Related Art
[0004] With respect to joints formed by joining members of different metals through a metallurgical method such as a friction welding method, conventionally, a joint which has a flange that is caused by a material melted or discharged during the joining process and bent toward the side of the base material of the flange with respect to the joined interface, or a joint on which the flange is ground to provide a smooth circumference of the joined interface, has been used.
[0005] However, the respective metals (pure metals or alloys) have natural electric potentials that are inherent to the components, and when different metals are placed very close to each other or in a joined state and an electrolytic solution is supplied between the different metals, a phenomenon similar to that in a battery takes place due to the difference between the natural electric potentials, causing corrosion to progress between the different metals. For this reason, in the case of the conventional joints in which the circumference of the joined interface is continually exposed to the external atmosphere, when the surface is not coated with paint, etc., or when the coated paint, etc., has separated therefrom, an electrolytic solution, which is a main source of corrosion, is easily supplied to the joined interface, resulting in failure to prevent the progress of corrosion.
SUMMARY OF THE INVENTION
[0006] The present invention has been devised so as to solve the above-mentioned problems, and objects thereof are to provide a joined structure of different metals which can improve the corrosion resistance at the joined interface by utilizing a flange that is generated during a joining process and which is usable even in severely corrosive environments such as the use in a location susceptible to salt damage.
[0007] The joined structure of different metals of the present invention, which is a joined structure formed by joining members of different metals, is characterized in that a flange is allowed to extend in a direction from the circumferential side of one of the members along the circumference of the other member. In the present invention, a flange refers to an area stretching outside from a line connecting the end portion of the original joining member at the time of joining is performed.
[0008] As shown in FIG. 1 , in accordance with the joined structure of different metals of the present invention, a structure in which this flange 1 covers the circumferential portion of the joined interface forms is formed by allowing a flange 1 to extend in a direction from the circumferential side of one of members (first member) 2 along the circumference of the other member (second member) 3 . In this structure, it is possible to prevent an electrolytic solution such as salt water from reaching the joined interface by the existence of the flange. Moreover, even in the case when the electrolytic solution enters the inside of the flange 1 , the flange 1 or one portion of the second member 3 in the vicinity of the joined interface is subject to corrosion by this electrolytic solution to generate an oxide product 4 , and this oxide product 4 accumulates in a gap between the flange 1 and the second member 3 so that a further supply of the electrolytic solution to the vicinity of the joined interface is blocked, thereby inhibiting corrosion at the joined interface. Therefore, the joined structure of different metals of the present invention has an effect for delaying the progression of corrosion at the joined interface as described above, thereby achieving improvement of corrosion resistances.
[0009] In another aspect of the joined structure of different metals of the present invention, by taking the natural electric potential difference between the different metals into consideration, the flange that is extended in a direction from the circumferential side of one of the members along the circumference of the other member is made of a metal that is relatively low in natural electric potential between the different metals. In other words, as shown in FIG. 2 , in a joined structure having members of different metals being joined to each other, a flange 1 , which is made of a metal member that is relatively low in natural electric potential, is formed so as to extend in a direction from the circumferential side of a metal member 5 having a lower natural electric potential along the circumference of a metal member 6 having a higher natural electric potential so that the metal member 5 having a lower natural electric potential is arranged so as to cover the circumferential portion of the joined interface.
[0010] In this aspect, when an electrolytic solution is supplied between the flange 1 made of a metal member having a lower natural electric potential and the metal member 6 having a higher natural electric potential, the area of the flange 1 is subjected to corrosion. The corrosion of this flange area serves as a sacrifice corrosion for the corrosion at the joined interface. In other words, the electrolytic solution that will cause corrosion at the joined interface actually uses for causing corrosion between the flange 1 and the metal member 6 having a higher natural electric potential so as to decrease in the corrosion at the joined interface. Therefore, in this more preferable embodiment of the joined structure of different metals of the present invention, in addition to the above-mentioned effect of the flange for preventing the electrolytic solution from reaching the joined interface and the effect of the oxide product for blocking corrosion, the sacrifice corrosion effect of the flange is exerted so that it becomes possible to further improve the corrosion resistance of the joined structure of different metals.
[0011] The joined structure of different metals having such a joined interface is formed by, for example, a friction welding process that is one type of solid-phase joining method. In the friction process, the surfaces of the joined members are mechanically cleaned, and in the succeeding upset process, a reaction product generated at the joined interface is externally discharged, and the press-welding process between the two joined members is completed. Here, the member, which has been discharged together with the reaction product, forms a flange.
[0012] The friction welding method of members of different metals of the present invention is characterized in that a friction pressure is not more than the proof stress of the member having a lower melting point at the frictional interface temperature, and an upset pressure is not less than the proof stress of the member having a lower melting point at normal temperature. With this friction welding method, in a joined structure having members of different metals joined to each other, it becomes possible to allow a flange to desirably extend in a direction from the circumferential side of one of the members along the circumference of the other member.
[0013] In the friction process in the friction welding method of the present invention, the friction pressure must be set to not more than the proof stress of the member having a lower melting point in the friction interface temperature in order to store heat in an axis portion without continuously discharging the flange. This friction pressure is determined by the composition of the member having a lower melting point, and more specifically, the proof stress in a joined structure between a steel product and an aluminum alloy at an interface temperature of 450° C. is set to be 17 MPa in the case of an aluminum alloy (JIS A5052-H34), and 22 MPa in the case of another aluminum alloy (JIS A5454). Moreover, in the upset process, it is necessary to set the upset pressure to be not less than the proof stress of the member having a lower melting point at normal temperature in order to bend the axis so as to allow the flange to cover the joined interface. In the same manner as the friction pressure, this upset pressure is also determined by the composition of the member having a lower melting point, and more specifically, the proof stress at a normal temperature of 25° C. in a joined structure between a steel product and an aluminum alloy is set to be 215 MPa in the case of an aluminum alloy (JIS A5052-H34), and 240 MPa in the case of another aluminum alloy (JIS A5454).
[0014] Moreover, in the friction welding method of the present invention, when a friction time in the friction process is insufficient, the joined face is not sufficiently cleaned, that is, stains and residual oxides are excessively left at the joined face, causing a failure in obtaining a better welding state in the subsequent upset process. In contrast, when the friction time is too long, although the joined face is sufficiently cleaned, the input quantity of heat to be supplied to the joining members becomes too great, resulting in an excessive growth of the reaction product layer in the upset process and the subsequent serious degradation in the joining strength. For this reason, in the present invention, it is preferable to set the friction time appropriately by taking the above-mentioned friction pressure and upset pressure into consideration. Moreover, with respect to the upset time, any period of time may be set as long as it provides a sufficient press-welding process of the joining members.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a cross-sectional view schematically showing a joined structure of different metals in accordance with one embodiment of the present invention.
[0016] FIG. 2 is a cross-sectional view schematically showing a joined structure of different metals in accordance with another embodiment of the present invention.
[0017] FIG. 3A is a cross-sectional photograph showing a joined structure of different metals in accordance with Example 1 of the present invention after a corrosive environment test; and FIG. 3B is a cross-sectional view schematically showing FIG. 3A .
[0018] FIG. 4A is a cross-sectional photograph showing a joined structure of different metals in accordance with Comparative Example 1 after a corrosion environment test; and FIG. 4B is a cross-sectional view schematically showing FIG. 4A .
[0019] FIG. 5A is a cross-sectional photograph showing a joined structure of different metals in accordance with Comparative Example 2 after a corrosion environment test; and FIG. 5B is a cross-sectional view schematically showing FIG. 5A .
DETAILED DESCRIPTION OF THE INVENTION
[0020] In the following, the present invention will be explained in detail by referring to Examples.
EXAMPLE 1
[0021] A steel product (JIS S10C) was used as a metal member having a higher natural electric potential, and an aluminum alloy member (JIS A5052-H34) was used as a metal member having a lower natural electric potential, and these were formed into a cylindrical steel rod having an outer diameter of 16 mm and a predetermined length and a cylindrical aluminum alloy rod having an outer diameter of 16 mm and a predetermined length to prepare test pieces. The cylindrical steel rod was set to a fixed side and the cylindrical aluminum alloy rod was set to a rotating side. As shown in Table 1, after the faces to be joined of the two members had been defatted by using acetone, the cylindrical aluminum alloy rod was rotated at 1200 rpm and was made to frictionally weld with the cylindrical steel rod at a friction pressure of 10 MPa for a friction time of 3 seconds; thereafter, these were made to press-weld with each other with an upset pressure of 250 MPa for an upset time of 6 seconds to prepare a joined structure of the steel product and the aluminum alloy of Example 1. Here, the friction welding process of the cylindrical steel rod and the cylindrical aluminum alloy rod was carried out by a brake method that is a conventional method.
TABLE 1 Joining conditions Material Friction Number of Friction Upset Upset Steel Aluminum pressure revolutions time T1 pressure time T2 product alloy P1 (MPa) N (rpm) (sec.) P2 (MPa) (sec.) Example 1 S10C A5052-H34 10 1200 3 250 6 Comparative S10C A5052-H34 10 1200 3 250 6 Example 1 Comparative S35C A5454 62.5 1200 1 150 6 Example 2
[0022] The thus-obtained joined structure of a steel product and an aluminum alloy of Example 1 was greatly deformed on the cylindrical aluminum alloy rod side having a lower strength in the cross-section of the joined portions, and the deformed portion was discharged to form a flange that extends in a direction from the circumferential side of the cylindrical aluminum alloy rod along the circumference of the cylindrical steel rod in a manner so as to cover the circumferential portion of the joined interface.
COMPARATIVE EXAMPLE 1
[0023] With respect to the joined structure of a steel product and an aluminum alloy of Example 1, the flange was cut, and the circumferential portion of the joined structure was ground to a smooth face, thereby obtaining a joined structure of a steel product and an aluminum alloy of Comparative Example 1.
COMPARATIVE EXAMPLE 2
[0024] A steel product (JIS S35C) was used as a metal member having a higher natural electric potential, and an aluminum alloy member (JIS A5454) was used as a metal member having a lower natural electric potential, and these were formed into a cylindrical steel rod having an outer diameter of 16 mm and a predetermined length and a cylindrical aluminum alloy rod having an outer diameter of 16 mm and a predetermined length to prepare test pieces. Next, the cylindrical steel rod was set to a fixed side and the cylindrical aluminum alloy rod was set to a rotating side. As shown in Table 1, after the joining faces of the two members had been defatted by using acetone, the cylindrical aluminum alloy rod was rotated at 1200 rpm and was made to frictionally weld with the cylindrical steel rod at a friction pressure of 62.5 MPa for a friction time of 1 second; thereafter, these were made to press-weld with each other with an upset pressure of 150 MPa for an upset time of 6 seconds to prepare a joined structure of the steel product and the aluminum alloy of Example 1. Here, the above-mentioned friction welding process was carried out in the same manner as in Example 1.
[0025] The thus-obtained joined structure of a steel product and an aluminum alloy of Comparative Example 2 was greatly deformed on the cylindrical aluminum alloy rod side having a lower strength in the cross-section of the joined portions, and the deformed portion was discharged to form a flange that was bent from the joined interface toward the cylindrical aluminum alloy rod side.
[0026] Corrosive Environment Test
[0027] Corrosive environment tests including a cycle shown in Table 2 in which salt-water spraying, drying, and wet environments were combined with high and low temperatures were carried out on the joined structures of steel products and aluminum alloys of Example 1 and Comparative Examples 1 and 2, obtained as described above, and corrosion states in the vicinity of the joined interface were observed. The results of these tests show in FIGS. 3 to 5 . Therein, figures labeled A are each a cross-sectional photograph showing the joined interface, and figures labeled B are each a cross-sectional drawing schematically showing figures labeled A.
TABLE 2 Mode Condition Time (hr) Step 1 Wet 40° C., 95% RH 2 Step 2 Salt-water spray 35° C., 5% NaCl 2 Step 3 Dry 60° C. 1 Step 4 Wet 50° C., 95% RH 6 Step 5 Dry 60° C. 2 Step 6 Wet 50° C., 95% RH 6 Step 7 Dry 60° C. 2 Step 8 Low temperature −20° C. 3
[0028] As a result of the above-mentioned corrosive environment tests, with respect to the joined structure of Example 1 in which a flange is allowed to extend in a direction from the circumferential side of the cylindrical aluminum alloy rod along the circumference of the cylindrical steel product rod in a manner so as to cover the circumferential portion of the joined interface, as shown in FIG. 3 , even after tests of 90 cycles, there was only slight corrosion at the joined interface, although the top portion of the flange was subjected to sacrifice corrosion. In contrast, in the case of the joined structure of Comparative Example 1 in which the flange had been cut off and the circumference of the joined structure had been ground to form a smooth surface, as shown in FIG. 4 , the corrosion progressed along the joined interface and it was damaged after tests of 40 cycles. Moreover, in the case of the joined structure of Comparative Example 2 in which the flange was bent from the joined interface toward the cylindrical aluminum alloy rod side, as shown in FIG. 5 , although there was a delay in corrosion due to the sacrifice corrosion effect of the flange, it was not possible to block the supply of salt water, and after tests of 90 cycles, the corrosion at the joined interface progressed at the same speed as the corrosion of the flange, failing to provide sufficient corrosion resistances.
[0029] Therefore, with respect to the joined structure of a steel product and an aluminum alloy, by providing the arrangement in which a flange is allowed to extend in a direction from the circumferential side of a cylindrical aluminum alloy rod along the circumference of a cylindrical steel product rod in a manner so as to cover the circumferential portion of the joined interface, it becomes possible to suppress the progress of corrosion at the joined interface, and it is therefore possible to provide a joined structure between a steel product and an aluminum alloy which has improved corrosion resistances.
|
A joined structure of different metals is usable even in a severely corrosive environments such locations susceptible to salt damage. In a joined structure of different metals, members of different metals are joined to each other in such a manner that a flange is allowed to extend in a direction from the circumferential side of one of the members along the circumference of the other member.
| 1
|
TECHNICAL FIELD
[0001] This disclosure relates to water harvesting systems integrated in a vehicle, and more specifically to purification of the harvested water and harvesting of the water when the vehicle is keyed-off.
BACKGROUND
[0002] Clean drinking water is not readily available in arid locations, especially for travelers. The cost of infrastructure to provide clean drinking water in arid locations by traditional underground piping may be prohibitive. One solution has been to use stationary water harvesting stations, such as a water-making billboard, to condense water from the air and make it available for drinking.
[0003] The concept of harvesting water from vehicle air-conditioning systems has been disclosed in prior art references, however no automotive manufacturer has provided such a system on a vehicle to date. The prior art discloses the harvesting of water from air-conditioning systems when the vehicle is being driven and the air-conditioning is being used to cool the passenger compartment. There exists a need for a water purification system that may provide clean drinking water in a simple cost effective design. In addition, there exists a need for a vehicle based system that may harvest water while the vehicle is not being driven.
SUMMARY
[0004] One aspect of this disclosure is directed to a system for harvesting clean drinking water in a vehicle. The system includes a heat-exchanger, a reservoir fluidly connected with the heat-exchanger and configured to collect water from the heat-exchanger, and a heating element configured to heat water within the reservoir. This system includes a controller coupled with the heating element and programmed to boil the water in the reservoir.
[0005] The system may include a water level sensor disposed within the reservoir. The controller may be further programmed to boil the water in response to the water in the reservoir reaching a predetermined level. The system may also include a valve fluidly disposed between the heat-exchanger and the reservoir. The controller may be coupled with the valve and further programmed to, in response to the water in the reservoir reaching the predetermined level, actuate the valve to inhibit water flow from the heat-exchanger to the reservoir.
[0006] The system may have a temperature sensor disposed in the reservoir. The controller may be coupled with the temperature sensor and further programmed to, in response to the water having a temperature indicative of boiling, maintain the temperature of the water for a predetermined period of time. The predetermined time period may be at least one minute. The controller may also be programmed to purge the water in the reservoir after a second predetermined period of time elapsing from the water having a temperature indicative of boiling. The second predetermined period of time may be at least 12 hours.
[0007] The system may have a display. The controller may be programmed to send information relating to the purging of the water in the reservoir to the display. The system may have an air duct proximate the reservoir to facilitate cooling of the water after being boiled. The system may also have a temperature sensor in the reservoir. The controller may be further programmed to, in response to the water reaching a predetermined temperature below a temperature indicative of boiling, indicate that the water is ready to drink.
[0008] The system may include a dispensing line and a water bottle compartment capable of holding at least one water bottle. The controller may be programmed to fill at least one water bottle. The heat-exchanger may be a condenser.
[0009] The system may be part of a vehicle that has a battery capable of being recharged by plugging it in to an external electric source. The heat-exchanger may be part of an air-conditioning system of such a vehicle capable of being operated by the battery. The controller may be coupled with the battery and the air-conditioning system and further programmed, in response to the battery being recharged by the external electric source, operate the air-conditioning system to generate water from the heat-exchanger.
[0010] Another aspect of this disclosure is directed toward a method of providing clean drinking water in a vehicle. The method includes a step of operating an air-conditioning system during a key-off time period. The method also includes the step of collecting the condensed water from a condenser in the air-conditioning system, and then boiling the condensed water.
[0011] The step of collecting condensed water may include collecting a predetermined amount of condensed water, and isolating the collected amount of condensed water from additional waters that may condense off of the condenser. The method may include filtering the condensed water. The method may include purging the boiled water after a predetermined time period. Alternatively, the method may include re-boiling the boiled water after the predetermined time period. The time period may be at least 12 hours.
[0012] The step of operating an air-conditioning system during a key-off period may include providing an external power source to the vehicle.
[0013] The above aspects of this disclosure and other aspects will be explained in greater detail below with reference to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a diagrammatic illustration of a vehicular water harvesting and purification system.
[0015] FIG. 2 is a flowchart illustrating an example of automatic water harvesting.
[0016] FIG. 3 is a flowchart illustrating an example of automatic water purification.
DETAILED DESCRIPTION
[0017] The illustrated embodiments are disclosed with reference to the drawings. However, it is to be understood that the disclosed embodiments are intended to be merely examples that may be embodied in various and alternative forms. The figures are not necessarily to scale and some features may be exaggerated or minimized to show details of particular components. The specific structural and functional details disclosed are not to be interpreted as limiting, but as a representative basis for teaching one skilled in the art how to practice the disclosed concepts.
[0018] FIG. 1 shows a vehicle 10 having a passenger compartment 12 . Vehicle 10 may be a vehicle with an engine 14 , an electric machine 16 , or both cooperating as a prime mover of the vehicle. The Engine 14 and electric machine 16 represent any machine designed to convert energy into useful mechanical motion. The engine 14 may be a gasoline engine, a diesel engine or any form of an internal combustion engine that burns fuel. The electric machine 16 may be an electric motor. As such, the vehicle may be a traditional engine only vehicle, a battery-only electric vehicle (BEV), or may be a hybrid electric vehicle (HEV).
[0019] The vehicle 10 may have a battery 18 . The battery 18 may be a high voltage traction battery that coupled with the electric machine 16 may provide the energy for the electric machine to provide motion. The vehicle 10 may have a plug-in cable 20 . The plug-in cable 20 is configured to connect the battery 18 to an external power source (not shown). Thus battery 18 is capable of being recharged by plugging the plug-in cable 20 into an external power source.
[0020] Vehicle 10 has an air-conditioning system 26 . The air-conditioning system 26 has a heat-exchanger 28 disposed outside of the passenger compartment 12 , a compressor 30 , and a heat-exchanger 32 disposed within the passenger compartment 12 . The heat exchanger 28 located outside of the passenger compartment 12 may be referred to as a condenser 28 . The heat exchanger 32 located within the passenger compartment 12 may be referred to as an evaporator 32 . The compressor 30 may be driven by the engine 14 , such as by the use of an auxiliary drive belt off a crankshaft (not shown), or an auxiliary drive belt off the electric machine 16 , or by having a separate compressor motor (not shown). The compressor motor may be provided energy from the high voltage traction battery 18 or from a 12 volt battery (not shown).
[0021] Other components of an air-conditioning system 26 may be present in the system, such as a pressure regulator, an expansion valve, an accumulator, a receiver, a desiccant filter, or the like. The air-conditioning system 26 may also include an electronic control system (not shown) and a series of ducts 34 to route conditioned air from the evaporator 32 into the passenger compartment 12 . A fan 36 may be employed adjacent the heat-exchanger 28 to aid in improved airflow across heat-exchanger 28 . A second fan 38 , or a group of fans 38 , may be disposed within the series of ducts 34 to aid in airflow across the heat-exchanger 32 .
[0022] As a vehicle air-conditioning system 26 runs, water may condense on the heat exchangers 28 , 32 . Condensation is generally known as a change in the state of water vapor to liquid water when in contact with any surface. Generally when the air-conditioning system 26 is used to cool the passenger compartment, condensation may occur on the heat-exchanger 28 disposed outside of the passenger compartment 12 , although condensation may occur on the heat-exchanger 32 located within the passenger compartment as well. The heat-exchanger 28 located outside of the passenger compartment 12 is in fluid contact with the ambient environment (or an equivalent environment within an engine compartment adjacent the ambient environment. The water that condenses on heat-exchanger 28 is from water vapor formerly held within air surrounding the heat-exchanger 28 .
[0023] Vehicle 10 has a water harvesting and purification system 44 . A collector 46 is located near the heat-exchanger 28 and is configured to collect condensed water from the heat-exchanger 28 . The collector may be located below the heat-exchanger 28 and gravity may be used to collect the water. The collector 46 may be fluidly connected to a collection valve 48 via a collector line 50 . Collection valve 48 may be a three-way valve, or a series of T-shaped valves. Collection valve 48 may also be an electric actuated valve 48 . Collection valve 48 may be used to divert water from the collector 46 to a first fluid flow path 52 allowing water to flow from the heat-exchanger 28 to a reservoir 54 . Said another way, the collection valve 48 may be fluidly disposed between the heat-exchanger 28 and the reservoir 54 . Collection valve 48 may also be used to divert water from the collector 46 to a second fluid flow path 56 allowing water to flow from the heat-exchanger 28 to a drain 58 and outside of the vehicle 10 .
[0024] The first fluid flow path 52 may include a filter 60 . The filter 60 may be a mesh screen which is used for the separation of solids from fluids by interposing a medium through which the fluid can pass but not solids larger than the mesh sizing. The filter 60 may also be a chemical or ultraviolet filtration device which may be used to filter out undesirable bacteria, organic carbons, or the like. The filter 60 may be a number of filters 60 . The first fluid flow path 52 may also include a pump 62 . The filter 60 may be located before or after the pump 62 . The filter 60 may also be located before the collection valve 48 . Likewise, the pump 62 may also be located before the collection valve 48 . The system may also operate without a filter 60 or pump 62 , or provide more than one filter 60 or pump 62 at any location within the harvesting and purification system 44 to provide desired filtration, to move water, or to provide pressure where desired. Thus the filter 60 , if used, may be fluidly disposed between the heat-exchanger 28 and the reservoir 54 .
[0025] The reservoir 54 is fluidly connected with the heat-exchanger 28 such that the reservoir 54 is configured to collect water from the heat-exchanger 28 . The reservoir 54 may be located inside or outside of the passenger compartment 12 . The reservoir 54 may have a water level sensor 66 . The water level sensor 66 may be a float 66 disposed within the reservoir 54 which floats on accumulated water 68 within the reservoir 54 . The reservoir 54 may have a heating element 70 configured to heat the accumulated water 68 . The heating element 70 may be disposed within the water 68 , or may be disposed in a wall of the reservoir 54 . The accumulated water 68 may also be pre-heated by having the collector line 50 or first fluid flow path 52 warmed by other heat generating sources. For example, the collector line 50 may pass through or near the engine 14 .
[0026] The reservoir 54 has a temperature sensor 72 configured to provide a temperature of the accumulated water 68 . The temperature sensor 72 may be submerged in the water 68 , may be in a wall of the reservoir 54 , or may be part of the heating element 70 . The heating element 70 may be used to heat the accumulated water 68 . The heating element 70 may be used to boil the accumulated water 68 . The boiling of the water 68 may be done to remove additional impurities. The air-conditioning system 26 may be used to add heat to the water 68 . After heating of the water 68 , ducts 34 from the air-conditioning system 26 may be used to cool the water 68 . A duct 34 of the multiple ducts 34 may be located proximate the reservoir 54 configured to facilitate cooling of the water 68 . Additional cooling devices (not shown) may be used to cool the water 68 after being boiled.
[0027] The reservoir 54 may have an outlet valve 73 . The outlet valve 73 may be a three way valve similar to the collection valve 48 . The outlet valve 73 may be actuated to allow the water 68 to flow out of the reservoir 54 . A first dispensing line 74 may extend from the outlet valve 73 to a first spout 76 in the passenger compartment 12 . A second dispensing line 78 may extend from the outlet valve 73 to a second spout 80 outside of the passenger compartment 12 . The reservoir 54 may be disposed within or outside of the passenger compartment 12 . The first spout may be opened and closed by a first dispensing valve 82 . The second spout 80 may be opened and closed by a second dispensing valve 84 . The first and second valves 82 , 84 may be manual valves or electric actuated valves.
[0028] The first spout 76 may be configured to fill at least one water bottle 86 . The water bottle 86 may be located within a water bottle compartment 88 . The water bottle 86 may be a 12 ounce water bottle and the water bottle compartment 88 may be able to hold six water bottles 86 . The water bottle compartment 88 may be sized to fit six water bottles 86 , three wide and two deep. The first spout 76 may be moveable via a first spout motor (not shown) to fill each water bottle 86 . Alternatively, the water bottles 86 may be on a rotatable tray or conveyor tray and each moveable to the first spout 76 . The water bottle compartment 88 may be cooled by a duct 34 from the number of ducts 34 of the air-conditioning system 26 . The water bottle compartment 88 may also be heated by a duct 34 from the number of ducts 34 of the air-conditioning system 26 . The water bottle compartment 88 may be cooled by a separate refrigeration unit (not shown). The water bottle compartment 88 may be disposed in a dash panel or instrument panel adjacent, or in place of, a glove compartment. The system 44 provides a removable bottle 86 with purified water within reach of a driver of the vehicle 10 .
[0029] The water harvesting and purification system 44 may also have a display 94 for relating information about the water harvesting and purification system 44 to a user. Information may include such data as amount or temperature of the accumulated water 68 in the reservoir 54 , whether the accumulated water 68 has been purified, time elapsed since the accumulated water 68 has been purified, or the like. The display 94 may be located in a location visible to a user in the passenger compartment 12 . The display 94 may be an existing display in an infotainment system (not shown). The display 94 may be located in a location visible to a user outside of the passenger compartment 12 . An exterior display 94 may be within the passenger compartment 12 visible through a window, may be a projector that projects the data onto a window, or may be a series of lights in the exterior surface of the vehicle 10 .
[0030] An ignition 96 may be connected to the vehicle 10 . The ignition 96 may be controlled by a user to key-on and start the vehicle 10 . When the vehicle 10 is key-on and started, either the engine 14 , motor 16 , or both may be used to propel the vehicle 10 . As well, in the key-on state, the air-conditioning system 26 may be used to cool the vehicle and provide condensed water for the water harvesting and purification system 44 . The user may also use the ignition 96 to key-off and stop the vehicle 10 . The engine 14 and motor 16 may not propel the vehicle in a key-off state. A traditional key 98 is shown that may be inserted into the ignition 96 and used to key-on and key-off the vehicle 10 , however the ignition may not need an inserted key 98 , as it may be a button or have a proximity key, or the like.
[0031] The water harvesting and purification system 44 may operate the air-conditioning system 26 to generate condensed water even when the vehicle 10 is in a key-off state. The water harvesting and purification system 44 may operate the air-conditioning system 26 to generate condensed water even when the vehicle 10 has the plug-in cable 20 plugged into an external power source to recharge the battery 18 . The water harvesting and purification system 44 may utilize the external power source to provide the energy necessary to operate the air-conditioning system 26 while the vehicle 10 is key-off.
[0032] A controller 100 may automate the water harvesting and purification system 44 . The controller 100 may be coupled with the engine 14 , if one is in the vehicle 10 , as indicated by communication line 114 . The controller 100 may be coupled with the motor 16 , if one is in the vehicle 10 , as indicated by communication line 116 . The communication lines 114 , 116 may communicate data to the controller 100 such as current use of the engine and/or motor 14 , 16 , among others.
[0033] The controller 100 may be coupled with the battery 18 , as indicated by communication line 118 . The communication line 118 may communicate data such as current state of charge, battery charge level, or whether the battery 18 is being recharged by an external power source (via plug-in cable 20 ), among others. The controller 100 may be coupled with the compressor 30 , as indicated by communication line 130 . Communication line 130 may include data about the operation of the air-conditioning system 26 , as well as provide a conduit for the controller 100 to control the operation of the compressor 30 . The communication line 130 may also convey electrical current from the battery 18 to operate the compressor 30 when the engine 14 or motor 16 are not in use. The controller 100 may be coupled with the air-conditioning system 26 , via the compressor 30 , and programmed to, in response to the battery 18 being charged by an external electric source, operate the air-conditioning system 26 to generate water from the heat-exchanger 28 .
[0034] The controller 100 may be coupled with the collection valve 48 , as indicated by communication line 148 . The controller 100 may be programmed to actuate the control valve 48 to switch from the first fluid flow path 52 to the reservoir 54 or the second fluid flow path 56 to the drain 58 . The controller 100 may be programmed to, in response to the water 68 in the reservoir 54 reaching a predetermined level, actuate the control valve 48 to inhibit water flow from the heat-exchanger 28 to the reservoir 54 . The controller 100 may be programmed to, in response to the water 68 in the reservoir 54 reaching a predetermined level, switch the collection valve 48 from the first fluid flow path 52 to the second fluid flow path 56 . The controller 100 may be programmed to, in response to the water 68 in the reservoir 54 reaching a predetermined level, turn off the air-conditioning system 26 if being run during key-off/plug-in state.
[0035] The controller 100 may be coupled with the water level sensor 66 , as indicated by communication line 166 . The communication line 166 may convey data relating to the level of water 68 in the reservoir 54 . The communication line 166 may convey the water 68 in the reservoir 54 reaching a predetermined level. The predetermined level may be different for each programmed operation. The predetermined level may be at least 12 ounces. The predetermined level may be greater than 72 ounces (enough to fill six 12 ounce bottles). The controller 100 may be coupled with the pump 62 via communication line 162 . The controller 100 may be programmed to actuate pump 62 to move water or provide pressure within the water harvesting and purification system 44 . The controller 100 may utilize the pump 62 to provide the pressure needed for the water 68 to reach the predetermined level.
[0036] The controller 100 may be coupled with the heating element 70 via communication line 170 . The controller 100 may utilize the heating element 70 to heat the water 68 . The controller 100 may utilize the heating element 70 to boil the water 68 . The controller 100 may be programmed to, in response to the water 68 in the reservoir 54 reaching a predetermined level, boil the water 68 . The controller 100 may be coupled with a temperature sensor 72 via communication line 172 . The controller 100 may be programmed to, in response to the water 68 having a temperature indicative of boiling, maintain the temperature of the water for a predetermined period of time. The predetermined time period may be at least one minute. The controller 100 may be further programmed to, in response to the water reaching a predetermined temperature below a temperature indicative of boiling, indicate that the water 68 is ready to drink.
[0037] The controller 100 may be coupled with the outlet valve 73 via communication line 173 . The controller 100 may actuate the outlet valve 73 to provide water to the first or second fluid flow paths 74 , 78 , or to maintain water 68 in the reservoir 54 until purified or until at a desired temperature. The controller 100 may be coupled with the first dispensing valve 82 via communication line 182 . the controller 100 may be programmed to open the first dispensing valve 82 to automatically fill a water bottle 86 . Alternatively, a user may initiate the opening and closing of the first dispensing valve 82 by a touch sensitive button, or the like (not shown).
[0038] The controller 100 may be coupled with the second dispensing valve 84 via communication line 184 . the controller 100 may be programmed to open the second dispensing valve 84 to automatically purge water from the reservoir. Alternatively, a user may initiate the opening and closing of the second dispensing valve 84 by a touch sensitive button, or the like (not shown). The second dispensing valve 84 in conjunction with the second spout 80 provide an option of filling up any container outside of the vehicle 10 .
[0039] The controller 100 may be further programmed to purge the water 68 in the reservoir after a second predetermined period of time elapsing from the water having a temperature indicative of boiling. The second predetermined period of time may be at least 12 hours. The controller may be coupled with the display 94 via communication line 194 . The controller 100 may be programmed to display information on the display 94 . The display 94 may display information relating to the purging of the water 68 , such as a countdown until the next purge. The display 94 may also show information relating the amount or temperature of the accumulated water 68 in the reservoir 54 , whether the accumulated water 68 has been purified, time elapsed since the accumulated water 68 has been purified, number of water bottles 86 filled, different operating parameters of the system, or the like.
[0040] FIG. 2 shows an example of control logic, utilizing the above disclosed components, for the harvesting of water. Decision diamond 200 determines whether a water harvest mode has been selected by a user. If no water harvest mode has been selected, the logic flow moves to end block 202 . Decision diamond 200 allows the automatic harvesting of water to be turned off. If the water harvest mode has been selected, the flow moves to decision diamond 204 .
[0041] Decision diamond 204 determines whether water in a reservoir has reached a predetermined level. The predetermined level may be a full line. If the reservoir is full, the logic flow moves to action block 206 , then to action block 208 , and then to end block 202 . Action block 206 actuates a collection valve to send any water condensed off a heat-exchanger to a drain. Action block 208 discontinues the water harvest mode. Action block 208 will turn off any and all other action blocks in this strategy flow diagram. If the reservoir is not full, the logic flow moves to action block 210 .
[0042] Action block 210 actuates the collection valve to direct water from the heat-exchanger to the reservoir. The logic flow then moves to decision diamond 212 where it is determined whether an air-conditioning system is operating. If an air-conditioning system is operating, then the flow returns to decision diamond 200 . This allows for a do-loop until the reservoir is filled or the water harvest mode is turned off by a user. If the air-conditioning system is not operating, the logic flow moves to decision diamond 214 .
[0043] Decision diamond 214 determines whether the vehicle is running. If the vehicle is key-on and running, then the logic flow moves to action block 216 . Action block 216 turns on the air-conditioning system and the flow returns to decision diamond 200 . This allows for a do-loop in the logic flow until the reservoir is filled, the harvest mode turned off, or the vehicle turned off. If the vehicle is key-off, then the logic flow moves to decision diamond 218 .
[0044] Decision diamond 218 determines whether the vehicle is plugged in to an external power source. If the vehicle is plugged in, then the logic flow moves to action block 220 and turns on the air-conditioning system to harvest water from the ambient air. The external power source provides the energy needed to run the air-conditioning system without draining a battery or gas tank. After action block 220 , the logic flow returns to decision diamond 200 . This allows for a do-loop in the logic flow until the reservoir is filled, the harvest mode turned off, the vehicle is unplugged, or the vehicle is keyed back on. If the vehicle is not plugged in, then the logic flow returns to decision diamond 200 . This allows for a do-loop in the logic flow until the reservoir is filled, the harvest mode turned off, the vehicle is keyed back on, or the vehicle is plugged in.
[0045] FIG. 3 shows an example of control logic, utilizing the above disclosed components, for the purification of water. Decision diamond 300 determines whether water in a reservoir has reached a predetermined level. The predetermined level may be a full line. If the reservoir is not yet full, the logic flow moves to action block 302 . Action block 302 actuates a collection valve to send any water condensed off a heat-exchanger to the reservoir and then returns the logic flow to decision diamond 300 . This provides a do-loop in the logic flow until the reservoir fills. If the reservoir is full, the logic flow moves to action blocks 304 , 306 , 308 .
[0046] Action block 302 activates the collection valve to send water condensing off an evaporator to the drain and not to the reservoir. This allows for the water accumulated in the reservoir to be isolated. Action block 306 provides for the water in the reservoir to be brought to a boil. This allows for the water to be purified by the heat. Action block 306 may have a duration of at least one minute. Action block 308 starts a purge counter on the boiled water. after action blocks 304 , 306 , 308 , the logic flow moves to decision diamond 310 .
[0047] Decision diamond 310 determines whether the water in the reservoir has been emptied. If the water has been emptied, then the logic flow moves to action block 302 and back to decision diamond 300 . This provides for a do-loop in the logic flow to allow the system to automatically fill itself and purify the accumulated water and refill itself and re-purify newly accumulated water so long as the older purified water has been discarded or used. If the reservoir still has some water remaining in it, then the logic flow moves to decision diamond 312 .
[0048] Decision diamond 312 determines whether the purge counter has reached a predetermined time. In other words, it determines how much time has elapsed since the water was purified. The predetermined time may be at least 12 hours. If the predetermined time has not elapsed, then the logic flow returns to decision diamond 310 . This allows for a do-loop in the logic flow until all of the water in the reservoir is discarded or used, or until the purge counter has reached its limit. If the purge counter has reached its limit, then the logic flow moves to action block 314 . Action block 314 purges all of the water from the reservoir. This provides for the discarding of unused water and the prevention of the water in the reservoir from becoming un-purified. After action block 314 , the logic flow returns to action block 302 and decision diamond 300 . this allows for a do-loop in the logic flow to refill the reservoir and re-purify the water.
[0049] This logic flow chart may also include an action block of filtering the water (not shown) before or after action block 306 of boiling the water. The filtering of the water may include a mesh screen or other filtering techniques such as ultraviolet light or the like.
[0050] While exemplary embodiments are described above, it is not intended that these embodiments describe all possible forms of the disclosed apparatus and method. Rather, the words used in the specification are words of description rather than limitation, and it is understood that various changes may be made without departing from the spirit and scope of the disclosure as claimed. The features of various implementing embodiments may be combined to form further embodiments of the disclosed concepts.
|
A water harvesting and purifying system and method for an automobile. The system automatically collects condensed water from a heat-exchanger in an air-conditioning system. the system filters the condensed water and isolates it in a reservoir. the system boils the isolated water to further purify. The water is then useful for drinking for a predetermined time period, after which the water is purged and the process restarted.
| 8
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus for receiving and dispensing bills, in particular to an apparatus for receiving and dispensing bills which can efficiently receive the paper money (i.e., bills).
2. Description of the Related Art
A conventional bill receiving and dispensing machine is known which discriminates whether received bills are acceptable or not and the denominations of the bills, and in which the paper monies (hereinafter referred to as bills) are stored in a temporary storing box and then the bills are stored in bill storing boxes by bill denomination. In the conventional bill receiving and dispensing machine, after a teller or a customer confirms the amount of the bills received and inputs a bill deposit instruction signal, the bills are fed from the bill temporary storing box to the bill storing boxes.
However, in the conventional machine, the next bills can not be received until all of the bills in the temporary storing box have been fed to the bill storing boxes. Therefore, the conventional machine can not efficiently receive the bills.
Further, when the number of the one denomination of bill in the bill storing box exceeds a predetermined value, the bill storing box can not store any more bills. Therefore, the teller or the customer has to stop the machine and remove the bills. Then the customer has to deposit the bills again. Thus, the machine can not efficiently receive the bills.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide an apparatus for receiving and dispensing bills which can efficiently receive the bills
This and other objects are achieved according to the present invention by providing an apparatus for receiving and dispensing bills comprising, a bill receiving opening in which the bills are deposited, at least two bill temporary storing boxes adapted to temporary store the bills which are deposited in the bill receiving opening and to take out the stored bills, a plurality of bill storing boxes adapted to store the bills taken out from the bill temporary storing boxes and to take out the stored bills, the bill storing boxes being provided for respective denominations, a first transport passage for connecting the bill receiving opening with the bill temporary storing boxes such that the bills are fed between the bill receiving opening and the bill temporary storing boxes, and a second transport passage for connecting the bill temporary storing boxes with the bill storing boxes such that the bills are fed between the bill temporary storing boxes and the bill storing boxes, the second transport passage being disposed independently from the first transport passage.
In the present invention, at least two bill temporary storing boxes are adapted to temporary store the bills which are deposited in the bill receiving opening and to take out the stored bills, the first transport passage for connecting the bill receiving opening with the bill temporary storing boxes and the second transport passage for connecting the bill temporary storing boxes with the bill storing boxes are disposed independently. Therefore, while the bills stored in one of the two bill temporary storing boxes are fed to the plurality of the bill storing boxes, the bills deposited in the bill receiving opening can be efficiently stored in the other of the two bill temporary storing boxes.
According to a preferred embodiment of the present invention, the apparatus further comprises a transport passage branching off from the second transport passage and connecting with the first transport passage. In this embodiment, even if the number of the bills in one of the plurality of the bill storing boxes becomes too large and therefore the bill storing box can not store the bills any more, the bills to be stored in the one of the bill storing boxes are fed to one of the two bill temporary storing boxes which is empty through the passage branching off the second transport passage and connecting with the first transport passage. Therefore, the bills can continue to be received and the machine can efficiently receive the bills.
According to another preferred embodiment of the present invention, the second transport passage connects with a bill dispensing opening.
According to another preferred embodiment of the present invention, the first transport passage and the second transport passage respectively include bill discrimination means for discriminating the bills.
The above and other objects and features of the present invention will be apparent from the following description by taking reference with accompanying drawings employed for preferred embodiments of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings:
FIG. 1 is a schematic side view showing a bill receiving and dispensing machine in accordance with a preferred embodiment of the present invention; and
FIG. 2 is a block diagram showing a sensing section, a driving section, an input section, a display section and a control section of the bill receiving and dispensing machine in accordance with the preferred embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will now be explained with reference to preferred embodiments and the drawings.
FIG. 1 is a schematic side view showing a bill receiving and dispensing machine in accordance with a preferred embodiment of the present invention.
As shown in FIG. 1, the bill receiving and dispensing machine 1 comprises a bill receiving opening 2 for receiving bills, a bill dispensing opening 3 for dispensing bills, and a bill returning opening 4 for returning bills which are discriminated to be unacceptable. All of the openings 2, 3 and 4 are disposed at the front side of the machine 1. The bill receiving and dispensing machine 1 further comprises a bill discrimination section 5 for discriminating the bills one by one which are received by the bill receiving opening 2 and then taken out from the bill receiving opening 2 by a known taking out means (not shown). The bill discrimination section 5 is adapted to discriminate whether or not the bills are acceptable. The bill discrimination section 5 is further adapted to discriminate the denominations of bills, the front and rear surfaces of the bills, whether or not two or more bills are completely or partially overlapped (hereinafter called "double feed") and whether or not the bills are obliquely fed (hereinafter called "oblique travel") and further to count the number of bills which are acceptable, when the bill are discriminated to be acceptable. The bills discriminated by the bill discrimination section 5 to be unacceptable, double fed or traveling obliquely are fed to the returning opening 4 and returned to the teller or customer. A first transport passage 6 is disposed to connect the bill receiving opening 2 and the bill discrimination section 5 with the bill returning opening 4.
A first bill temporary storing box 10 and a second bill temporary storing box 11 are provided detachably on the lower portion of the front side of the machine 1. The first bill temporary storing box 10 is connected to the first transport passage 6 through both a transport passage 12 and a transport passage 13 branching off from the passage 12, and the second bill temporary storing box 11 is connected to the first transport passage 6 through both a transport passage 14 and a transport passage 15 branching off from the passage 14. The transport passages 13 and 15 turn the bills over and feed them into the first and second temporary storing boxes 10 and 11. The first and second temporary storing boxes 10 and 11 have the same structure and are respectively provided therein with bill placement plates 16 and 17 which move up and down and on which the fed bills are placed. The first temporary storing box 10 is provided with a bill receiving and taking out mechanism 20 which receives the bills from the transport passages 12 and 13 in the first box 10 and takes out the bills stored in the first box 10 and feed them to a transport passage 18. Similarly, the second temporary storing box 11 is provided with a bill receiving and taking out mechanism 21 which receives the bills in the second box 11 from the transport passages 14 and 15 and takes out the bills stored in the second box 11 and feeds them to a transport passage 19. The transport passages 12, 13, 14 and 15 and the bill receiving and taking out mechanisms 20 and 21 are disclosed in U.S. Pat. No. 5,553,840. The transport passages 18 and 19 are connected to a second transport passage 22 for dispensing the bills to the bill dispensing opening 3.
Three bill storing boxes 30, 31 and 32, each for storing bills of one denomination after the bills have been classified into the respective denominations, are provided detachably on the lower portion of the rear side of the machine 1, and an unacceptable bill receiving box 33 is provided behind the box 30.
The second transport passage 22 is connected to the bill dispensing opening 3 through a bill discrimination section 35 which discriminates the denominations of bills, the double feed of bills and the oblique travel of the bills and counts the number of bills. The bill discrimination section 35, the unacceptable bill receiving box 33 and the bill storing boxes 30, 31 and 32 are connected by a loop passage 22a.
The bill storing boxes 30, 31 and 32 are respectively connected to the loop passage 22a of the second transport passage 22 through transport passages 40 and 41, transport passages 42 and 43 and transport passages 44 and 45. The bill storing boxes 30, 31 and 32 are respectively provided therein with bill placement plates 46, 47 and 48 which move up and down and on which the fed bills are placed. The bill storing boxes 30, 31 and 32 are respectively provided with bill receiving and taking out mechanisms 50, 51 and 52 which receive and take out the bills. The bill placement plates 46, 47 and 48 and driving mechanisms thereof have the same structures as those of the bill placement plates 16 and 17 of the first and second boxes 10 and 11 and their driving mechanisms. The structures of the bill receiving and taking out mechanisms 50, 51 and 52 are well known.
A transport passage 55 branches off from the loop passage 22a of the second transport passage 22 and is connected to the unacceptable bill receiving box 33, and a transport passage 56 branches off from the downstream portion of the second transport passage 22 and connects with the first transport passage 6.
The bill receiving and dispensing machine 1 is further provided with a pair of supporting units (not shown) which are slidable. The first and second bill temporary storing boxes 10 and 11 are supported by one of the supporting units, and the bill storing boxes 30, 31 and 32 are supported by the other of the supporting units. Accordingly, the first and second bill temporary storing boxes 10 and 11 can be picked up by the one of the supporting units being drawn out, and the bill storing boxes 30, 31 and 32 can be picked up by the other of the supporting units being drawn out.
FIG. 2 is a block diagram showing a sensing section, a driving section, an input section, a display section and a control section of the bill receiving and dispensing machine in accordance with the preferred embodiment.
The sensing section of the bill receiving and dispensing machine 1 includes the bill discrimination sections 5 and 35 and bill sensors 60, 61 and 62. The bill sensors 60, 61 and 62 respectively sense whether or not numbers of the bills stored in the bill storing boxes 30, 31 and 32 have reached respective predetermined values, by detecting the locations or heights of the bill placement plates 46, 47 and 48.
The driving section of the machine 1 includes a driving means 65 having driving rollers (not shown) disposed in the first and second transport passages 6 and 22, and a plurality of motors (not shown) disposed so as to drive the bill receiving and taking out mechanisms 20, 21, 50, 51 and 52 and the like.
The input section of the machine 1 includes a keyboard 70 which tellers and customers operate and through which various instruction signals are input. The display section of the machine 1 includes a display 75 which displays the results of counted numbers of the bill and the like.
The control section of the machine 1 includes a CPU 80, a ROM 81 storing a program for controlling the machine 1 and the like, and a RAM 82 for storing various data. The bill discrimination signals generated by the bill discrimination sections 5 and 35 and the detection signals generated by the bill sensors 60, 61 and 62 are input to the CPU 80. The CPU 80 controls the machine 1 based on these input signals and the instruction signals input through the keyboard 70, by using the control program stored in the ROM 81.
How the bills are received and dispensed in the bill receiving and dispensing machine 1 in accordance with the embodiment explained above will be explained below.
When the machine 1 is put in service, the first and second boxes 10 and 11 and the unacceptable bill receiving box 33 are all empty, and the bill storing boxes 30, 31 and 32 store predetermined numbers of the respective bills. The bills can be stored in the boxes 30, 31 and 32 after they are drawn out by the supporting unit of the boxes 30, 31 and 32. Alternatively the bills may be stored in the boxes by the bills being fed to the boxes 30, 31 and 32 through the bill receiving opening 2, the first transport passage 6, the first or second bill box 10 or 11 and the second transport passage 22, which will be explained below.
When a bill receiving signal is input through the keyboard 70 and the bills are deposited in the bill receiving opening 2 by a teller or a customer, the CPU 80 outputs a driving signal to the driving means 65.
As a result, the bills are taken out to the first transport passage 6, and the bill discrimination section 5 discriminates whether or not the bills are acceptable. When the bills are discriminated to be acceptable, the bill discrimination section 5 further discriminates the denominations of the bills, front surfaces and rear surfaces of the bills, double feed and oblique travel of the bills, and counts the amounts of the bills in the respective denominations.
The amounts of the bills in the respective denominations counted by the bill discrimination section 5 are output to the CPU 80 and are stored in the RAM 82.
The bills which are discriminated to be acceptable by the bill discrimination section 5 are received in one of the first box 10 or the second box 11 which is empty. Since both of the first and second boxes 10 and 11 are empty when the machine 1 is put in service, the case where the acceptable bills are received in the first box 10 will be explained below.
The bills which are discriminated to be acceptable and to have the front surfaces thereof facing upward by the bill discrimination section 5 are fed to the first temporary storing box 10 through the first transport passage 6 and the transport passage 12. On the other hand, the bill which are discriminated to be acceptable and to have the front surfaces thereof facing downward by the bill discrimination section 5, are fed to the first temporary storing box 10 through the first transport passage 6 and the transport passage 13, in which the bills are turned over so that the front surfaces thereof face upward. The bills fed to the first box 10 are placed on the bill placement plate 16, which is located at the upper portion by a motor (not shown), with the front surfaces of the bills facing upward. As is well known, the bill placement plate 16 is moved downward by the motor as the bills are placed on the plate 16.
On the contrary, the bills which are discriminated by the bill discrimination section 5 to be double fed or traveling obliquely are returned through the first transport passage 6 to the bill returning opening 4 and finally returned to the teller or the customer.
When all of the bills deposited in the bill receiving opening 2 have been stored in the first box 10, the CPU 80 operates the display 75 to display the total amount of the bills counted by the bill discrimination section 5 and stored in the RAM 82. Thus, since all of the bills which are discriminated to be unacceptable, double fed or traveling obliquely are returned to the bill returning opening 4 and finally returned to the teller or the customer, and all of the bills stored in the first box 10 are counted by the bill discrimination section 5, the correct total amount of the bills is stored in the RAM 82 and displayed on the display 75.
Next, when the teller or the customer confirms the amount of the bills displayed on the display 75 and inputs a deposit instruction through the keyboard 70, the CPU 80 outputs a driving signal to the driving means 65 and the driving means 65 drives the bill receiving and taking out mechanisms 20 so that the bills stored in the first box 10 are taken out one by one to the second transport passage 22 through the transport passage 18, unless where some bills are present in the second transport passage 22.
The denomination, the double feed and the oblique travel of the bills taken out to the second transport passage 22 are discriminated and the amount of the bills are counted in the respective denominations by the bill discrimination section 35. The amounts of the bills in the respective denominations counted by the bill discrimination section 35 are output to the CPU 80 and are stored in the RAM 82.
The bills which are discriminated to be double fed or traveling obliquely by the bill discrimination section 35 are received in the unacceptable bill receiving box 33 through the transport passage 55.
On the other hand, the bills which are discriminated to be normal and being fed with no trouble, are sent to the loop passage 22a of the second transport passage 22 and then received and stored in one of the bill storing boxes 30, 31 and 32 based on denomination discriminated by the bill discrimination section 35. Thus, since all of the bills stored in the boxes 30, 31 and 32 are counted by the bill discrimination section 35, the correct amounts of the bills are stored in the RAM 82.
The CPU 80 further calculates the amount of the bills stored in the box 33 by subtracting the total amounts of the bills stored in the boxes 30, 31 and 32 counted by the bill discrimination section 35 from the amount of the bills stored in the first box 10, and stores the amount of the bills in the box 33 in the RAM 82. Thus, the amount of the bills in the unacceptable bill receiving box 33 stored in the RAM are also correct.
According to the preferred embodiment explained above, the feeding of the bills from the first box 10 to the boxes 30, 31 and 32 does not require feeding of the bills onto the first transport passage 6. Therefore, even when the bills have not yet been taken out from the first box 10, the bills deposited in the bill receiving opening 2 can be efficiently stored in the second box 11 by feeding then onto the first transport passage 6. Thus, the deposited bills are efficiently received by the machine 1.
On the other hand, when the teller or the customer does not accept the displayed amount of the bills and inputs a no deposit signal through the keyboard 70 based on the amount of the bills, the CPU 80 outputs a drive signal to the driving means 65. In response, the bill taking out mechanism 20 takes out the bills one by one stored in the first box 10 to the second transport passage 22 through the passage 18. The bills taken out to the passage 22 are fed to the bill dispensing opening 3 through the bill discrimination section 35, and finally are received by the teller or the customer. Thereafter, the CPU 80 clears the amount counted by the section 5 and stored in the RAM 82.
Next, when the teller or the customer inputs a dispense signal through the keyboard 70, the CPU 70 calculates the numbers of the respective denominations of the bills to be dispensed from the boxes 30, 31 and 32 and outputs a drive signal to the driving means 65 based on the input amount. In response, the bill taking out mechanisms 50, 51 and 52 successively take out the calculated numbers of the respective denominations of the bills from the boxes 30, 31 and 32 to the loop passage 22a of the second transport passage 22.
The bills taken out to the loop passage 22a are fed the bill discrimination section 35 in which the denomination, the double feed and oblique travel of the bills are discriminated.
The bills discriminated as being double fed or traveling obliquely are fed to the passage 55 and stored in the unacceptable bill receiving box 33. The CPU 80 calculates the amount of the bills discriminated as being double fed which of the boxes 30, 31 and 32 the bills are taken out from. At this time, the CPU 80 calculates the amount of the double fed bills stored in the box 33 as double the amount of a bill of the denomination concerned. The CPU 80 further calculates the amount of the bills discriminated as traveling obliquely based on which of the boxes 30, 31 and 32 the bills were taken from. These calculated amounts for the double fed and obliquely traveling bills are respectively stored in the RAM 82. When double feed and/or oblique travel are discriminated by the section 35, the CPU 80 operates the driving means 65 so that one bill of the denomination corresponding that of the bill discriminated as being double fed and/or traveling obliquely is taken out from the corresponding box 30, 31 or 32 to the loop passage 22a of the second transport passage 22. At the same time, the CPU 80 calculates the amount of the bills which pass through the section 35 and reach to the bill dispensing opening 3, calculates the total of this amount and the amount of the bills stored in the box 337 obtains the amount of the bills stored in the boxes 30, 31 and 32 by subtracting the sum from the amount of the bills in the boxes 30, 31 and 32 stored in the RAM 82, and finally updates the data stored in the RAM 82. Even if bills discriminated as being double fed and fed into the box 33 are actually three or more bills, the amount of such bills is counted as a double amount as explained above. Thus, the amount of the bills stored in the box 33 is not always the real amount but an estimated amount. Therefore, when double feed is discriminated by the section 35, the amounts of the bills stored in the boxes 30, 31 and 32 are also estimated amounts.
The bills passing through the section 35 with no double feed or oblique travel are fed to the dispensing opening 3 and dispensed to the teller or the customer.
According to the preferred embodiment, bills are dispensed by feeding them from the boxes 30, 31 to the bill dispensing opening 3 through the second transport passage 22. Therefore, when the bills are dispensed, when the bills are received by the bill receiving opening 2 while the bills are being dispensed, the section 5 discriminates and counts the bills and stores the bills in the box 10. Thus, the received bills can be efficiently processed by the machine 1.
Further, the bill receiving and dispensing machine 1 in accordance with the preferred embodiment can continue to receive the bills even when one of the boxes 30, 31 and 30 can not store any more bills because the height of the bills placed on the plate 46, 47 or 48 in the box 31, 32 or 33 becomes greater than a predetermined value.
Namely, when the bill number counting sensor 60, 61 or 62 outputs a detection signal indicating that the height of the bills placed on the plate 46, 47 or 48 in the box 30, 31 or 32 has reached a predetermined value when the bills stored in box 10 are to be fed or are being fed to the box 30, 31 or 32 through the transport passage 18 and the second transport passage 22, the CPU 80 outputs a driving signal to the driving means 65 to cause the bills that were to be stored in the box 30, 31 or 32 associated with the sensor 60, 61 or 62 that output the signal to be fed to the second box 11 through the section 35, unless a bill is present in the first transport passage 6.
The denominations, double feed and oblique travel of the bills are discriminated by the bill discrimination section 35, and the amount of the bills is counted in the respective denominations by the section 35. The bills discriminated as being double fed or traveling obliquely are fed to the box 33 through the passage 55.
The bills not double fed or traveling obliquely are fed to the second box 11 through the passages 22, 56, 6 and 14. The CPU 80 stores in the RAM 82 the amount of the bills counted by the section 35 and stored in the second box 11. Since the section 35 accurately counts the amount of the bills to be stored in the second box 11, the accurate amount is stored in the RAM 82.
The bills other than the bills to be thus stored in the second box 11 are, as explained above, fed to the section 35 in which the numbers of the bills in the respective denominations are counted, and are fed to the corresponding box 30, 31 or 32 based on their denominations. The
The CPU 80 calculates the amount of the bills stored in the box 33 by subtracting the amount of the bills counted by the section 35 and stored in the boxes 30, 31, 32 and 11 from the amount of the bills which were previously stored in the box 10, and the RAM 82 stores the amount of the bills in the box 33. The calculated amount of the bills in the box 33 is accurate since such amount is obtained based on the amounts which were actually counted by the sections 5 and 35.
When the CPU 80 has determined, based on the data in the RAM 82 regarding the bills in the boxes 30, 31 and 32 stored in the RAM 82, that no bills received through the bill receiving opening 2 are present in the first box 10 or the second box 11 and the number of the bills in one of the boxes 30, 31 and 32 has fallen below a predetermined value, the boxes 30, 31 or 32 is replenished with the bills of the corresponding denomination.
Namely, supplementary bills are supplied into the first or second box 10 or 11, whichever is empty, after the supporting unit of the first and second boxes 10 and 11 has been drawn out. Both the first and second boxes 10 and 11 are empty unless bills to be stored in the boxes 30, 31 and 32 were stored in one of them because the number of the bills in one of the boxes 30, 31 and 32 reached to the predetermined value. The supplementary bills can therefore be supplied into either the first or second box 10 or 11.
When replenishing the bills, the teller inputs the amounts of the supplementary bills in the respective denominations through the keyboard 70, and the CPU 80 stores the amounts in the RAM 82.
After the supplementary bills have been supplied into the one of the first and second boxes 10 and 11, the supporting unit is set to the machine 1. Thereafter, the bills are taken out and stored in the one of the boxes 30, 31 and 32 in the same manner as in the case that the bills received in the bill receiving opening 2 and stored in the box 10 are taken out and stored in the boxes 30, 31 and 32.
Namely, the bills discriminated as being double fed or traveling obliquely by the section 35 are stored in the box 33 through the passage 55. The CPU 80 calculates the amount of the bills stored in the one of the boxes 30, 31 and 32 based on the discrimination signal from the section 35, and the RAM 82 stores the amount of the bills. After all of the bills stored in either of the boxes 10 or 11 have been taken out, the CPU 80 calculates the amount of the bills stored in the box 33 by subtracting the amount of the bills stored in the one of the boxes 30, 31 and 32 from the amount of the supplementary bills previously input through the keyboard 70, and the calculated amount is stored in the RAM 82. The calculated amount of the bills in the box 33 is accurate since the section 35 actually counts the amount of the bills stored in the one of the boxes 30, 31 and 32.
The bill receiving and dispensing machine 1 in accordance with the preferred embodiment can calculate the amounts of the bills remaining in the respective boxes 30, 31 and 32 and display such amounts on the display 75 when the machine 1 is taken out of service at the end of the day.
Namely, after the machine 1 has been taken out of service at the end of the day, the teller inputs a remaining bill calculation signal through the keyboard 70. In response, the CPU 80 outputs a drive signal to the driving means 65 for feeding the bills stored in one of the boxes 30, 31 and 32 through the loop passage 22a of the second transport passage 22 and the passages 22, 56 and 6 to the one of the boxes 10 and 11 which is empty. At this time, the section 35 discriminates only double feed and oblique travel. When double feed and/or oblique travel are discriminated, the CPU 80 operates the driving means 65 to feed such discriminated bills to the box 33 through the passage 55, but does not count the amount of the bills. As explained above, one of the boxes 10 and 11 is necessarily empty when the service is over, although other of the boxes 10 and 11 may store the bills fed from one of the boxes 30, 31 and 32 in which bills can not be stored. Since the CPU 80 can recognize which one of the boxes 10 and 11 is empty, all of the bills stored in one of the boxes 30, 31 and 32 can be stored in one or the other of the boxes 10 and 11. When both of the boxes 10 and 11 are empty, the CPU 80 selects one of them and stores the bills fed from one of the boxes 30, 31 and 32 therein. Storing of the bills in the first box 10 will be explained below.
The CPU 80 then outputs a drive signal instructing the driving means 65 to feed the bills stored in the first box 10 to the bill discrimination section 35 through the passages 18 and 22. The section 35 discriminates double feed and oblique travel of the bills and counts the bills. When double feed and/or oblique travel are discriminated, the bills discriminated as being double fed and/or traveling obliquely are fed to the box 33 through the passage 55 based on the detection signal from the section 35. The bills not double feed or traveling obliquely are fed from the section 35 through the loop passage 22a to the one of the boxes 30, 31 and 32 in which the bills were previously stored. The CPU 80 stores in the RAM 82 the amount of the bills stored in the one of the boxes 30, 31 and 32 and displays the amount of the bills on the display 75 based on the data input from the section 35. Thus, the amount of the bills displayed on the display 75 is accurate since the section 35 counts the amount of the bills actually passing through the section 35 and stored in the box 30, 31 or 32. When the teller inputs an instruction signal through the keyboard 70 requesting display of the amount of the bills stored in the box 30, 31 or 32 which was previously stored in the RAM 82, the CPU 80 operates the display 75 to display the previously stored amount of the bills in the box 30, 31 and 32. As a result, the teller can compare the newly counted amount of the bills with the previously stored amount of the bills.
In a similar manner, the CPU 80 successively operates the machine 1 so that the bills stored in another of the boxes 30, 31 and 32 are fed to the first box 10, the discrimination section 35 counts the amount of the bills, the bills are returned to the box 30, 31 or 32, and finally the display 75 displays the amount of the bills stored in the one of the boxes 30, 31 and 32.
In the preferred embodiment, as explained above, the bills are stored in the first box 10 or the second box 11 when the height of the bills in one of the boxes 30, 31 and 32 has reached the predetermined value so that the box can not store any more bills. Therefore, when the machine 1 is taken out of service, bills may remain in one of the first box 10 and the second box 11. When the bills remain in one of the first and second boxes 10 and 11 at the end of the service day, therefore, the machine 1 in accordance with the preferred embodiment calculates the amount of the bills remaining in the one of the first and second boxes 10 and 11 and displays this amount on the display 75. This will be explained for the case in which the bills remain in the second box 11.
The CPU 80 outputs a drive signal to the driving means 65 instructing it to feed he bills stored in the second box 11 to the bill discrimination section 35 through the passages 19 and 22. The section 35 discriminates the denomination, double feed and oblique travel of the bills and counts the bills. When double feed and/or oblique travel are discriminated, the bills discriminated as being double fed and/or traveling obliquely are fed to the box 33 through the passage 55. The bills without such double feed nor oblique travel are fed from the section 35 through the second transport passage 22, the first transport passage 6 and the passage 12 to the first box 10.
The CPU 80 stores in the RAM 82 the amount of the bills stored in the first box 10 and displays this amount of the bills on the display 75 based on the data input from the section 35. Thus, the amount of the bills displayed on the display 75 is accurate since the section 35 counts the amount of the bills actually passing through the section 35 and stored in the first box 10.
Thereafter, the teller draws out the supporting unit from the machine 1, collects the bills remaining in the first box 10 and the unacceptable bill receiving box 33, and counts the amount of the bills. Then, when the teller inputs an instruction signal through the keyboard 70, the CPU 80 operates the display 75 to display the amounts of the bills in the boxes 10 and 33 previously stored in the RAM 82. As a result, the teller can compare the newly counted amount of the bills with the previously stored amount of the bills.
Thus, the teller can confirm the amount of the bills remaining in the boxes 30, 31 and 32 of the machine 1 at the end of the service day and make preparations for next day's service.
Further, in accordance with the preferred embodiment, the bill receiving and dispensing machine 1 can leave predetermined numbers of the bills in the respective boxes 30, 31 and 32 at the end of the service day. In this case, when the teller inputs an instruction signal through keyboard 70, the CPU 80 outputs a drive signal instructing the driving means 65 to feed the bills stored in one of the boxes 30, 31 and 32 to the one of the boxes 10 and 11 which is empty through the loop passage 22a of the second transport passage 22 and the passages 22, 56 and 6. At this time, the section 35 discriminates only double feed and oblique travel. When double feed and/or oblique travel are discriminated, the CPU 80 operates the driving means 65 so that such discriminated bills are fed to the box 33 through the passage 55, but does not count the amount of the bills. Storing of the bills in the first box 10 will be explained below.
The CPU 80 then outputs a drive signal instructing the driving means 65 to feed the bills stored in the first box 10 to the bill discrimination section 35 through the passages 18 and 22. The section 35 discriminates double feed and oblique travel of the bills and counts the bills. When double feed and/or oblique travel are discriminated, the bills discriminated as being double fed and/or traveling obliquely are fed to the box 33 through the passage 55 based on the detection signal from the section 35. The bills without such double feed nor oblique travel are fed from the section 35 through the loop passage 22a to the one of the boxes 30, 31 and 32 in which the bills were previously stored. When the number of the bills stored in the one of the boxes 30, 31 and 32 has reached the predetermined value, the CPU 80 operates the driving means 65 based on the data input from the section 35 so that the bills passing through the section 35 are fed to the second box 11 through the passages 22, 56, 6 and 14. At this time, the amount of the bills stored in the second box 11 is counted by the section 35, and the CPU 80 stores this amount of the bills in the RAM 82.
In a similar manner, the CPU 80 successively operates the machine 1 so that the bills stored in another one of the boxes 30, 31 and 32 are fed to the first box 10, and only the predetermined number of the bills are returned to the boxes 30, 31 or 32. Thus, the machine 1 can leave the predetermined numbers of the bills in the respective boxes 30, 31 and 32 at the end of the service day.
In this case, if the numbers of the bills left in the respective boxes 30, 31 and 32 are less than the predetermined numbers to be left at the end of the service day, the teller makes up for the shortage of the respective denominations of the bills, and operates the keyboard 70. The replenishment of the bills can be carried out as explained above.
Thus, the amounts of the bills stored in the boxes 30, 31 and 32 and the first and second boxes 10 and 11 are accurately calculated and stored in the RAM 82 at the end of the service day. Further, the amounts of the bills stored in the boxes 30, 31 and 32 of the machine 1 at the start of the service day are known. Therefore, by subtracting the amount of the bills received and dispensed by the machine 1 after the start of service and the amount of the bills remaining in the boxes 30, 31 and 32 and the boxes 10 and 11 at the end of service, which amounts are stored in the RAM 82, from the amount of the bills stored in the machine 1 at the start of service, the amount of the bills left in the unacceptable bill receiving box 33 can be accurately calculated. As a result, at the end of the service, the teller can compare the actual amount of the bills collected from the box 33 with the calculated amount of the bills.
According to the embodiment of the present invention, the bill receiving and dispensing machine 1 includes the first bill temporary storing box 10 and the second bill temporary storing box 11, and the bills received in the bill receiving opening 2 are fed to the first and second boxes 10 and 11 through the first transport passage 6. Further, the bills stored in the first box 10 or the second box 11 are fed to the bill storing boxes 30, 31 and 32 through the second transport passage 22. Since the first transport passage 6 is disposed independently from the second transport passage 22, the first box 10 or the second box 11 can newly accept the bills which are later deposited in the receiving opening 2, even before all of the bills stored in the box 10 or 11 have been fed to the bill storing boxes 30, 31 and 32. Therefore, the machine 1 can efficiently receive the bills.
Further, according to the embodiment of the present invention, the first transport passage 6 through which the bills received in the bill receiving opening 2 are fed to the first box 10 or the second box 11 is disposed independently from the second transport passage 22 through which the bills in the boxes 30, 31 and are fed to the bill dispensing opening 3. Therefore, the machine 1 can store the bills received in the bill receiving opening 2 in the first box 10 or the second box 11 while the machine 1 is dispensing the bills in the boxes 30, 31 and 32. As a result, the machine 1 can efficiently receive and dispense the bills.
Moreover, according to the embodiment of the present invention, when the number of the bills stored in one of the boxes 30, 31 and 30 becomes too large and therefore the one of the boxes 30, 31 and 32 can not store any more bills, the bills to be stored in the box 30, 31 or 32 can be stored in the first box 10 or the second box 11. Therefore, even if the number of the bills stored in one of the boxes 30, 31 and 30 becomes too large, the machine 1 does not need to stop the bill receiving operation, and therefore the machine 1 can efficiently receive the bills.
Further, according to the embodiment of the present invention, even if the number of the bills stored in one of the boxes 30, 31 and 32 becomes too large and then the bills to be stored in the box 30, 31 or 31 are stored in one of the first box 10 and the second box 11, the machine 1 can accurately confirm the amounts of the bills left in the respective boxes 30, 31 and 32 by using the other of the first box 10 and the second box 11 at the end of the service day.
Still further, according the embodiment of the present invention, at the end of the service day, the bills left in the boxes 30, 31 and 32 are once stored in one of the first box 10 and the second box 11, and thereafter only the predetermined numbers of the bills are returned to the boxes 30, 31 and 32 and the numbers of the bills exceeding the predetermined numbers are stored in the other one of the first box 10 and the second box 11. As a result, the machine 1 can leave only the predetermined numbers of the bills in the boxes 30, 31 and 32.
In the above mentioned embodiment, when the supplementary bills are supplied into the machine 1, the supporting unit is drawn out from the machine 1 and then the bills are supplied into the first box 10 and the second box 11. However, according to another embodiment of the present invention, when the supplementary bills are supplied into the machine 1, the bills to be supplied can be deposited into the bill receiving opening 2 and fed to the first box 10 or the second box 11 and further fed to the boxes 30, 31 and 32. In this embodiment, since the bills are counted by the bill discrimination section 5, the replenishment amount of the bills does not need to be input through the keyboard 70.
In the above mentioned embodiment, based on the data stored in the RAM 82, it is determined whether or not the bills in the boxes 30, 31 and 32 need to be replenished. However, according to still another embodiment of the present invention, sensors are disposed in the boxes 30, 31 and 32, and whether or not the bills in the boxes 30, 31 and 32 need to be replenished is determined by using the detection values of the sensors.
In the above mentioned embodiment, the bill number sensors 60, 61 and 62 detect the condition that the respective boxes 30, 31 and 32 can not store any more bills. However, according to still another embodiment of the present invention, the condition that the respective boxes 30, 31 and 32 can not store any more bills can be determined by using the data stored in the RAM 82.
In the above mentioned embodiment, when double feed and/or oblique travel of the bills are discriminated during the replenishment of the bills, the bills discriminated as being double fed and/or traveling obliquely are fed into the unacceptable bill receiving box 33. However, according to still another embodiment of the present invention, such bills are returned to the dispensing opening 3.
While the present invention has been illustrated by means of several preferred embodiments, one of ordinary skill in the art will recognize that modifications and improvements can be made while remaining within the spirit and scope of the invention. The scope of the invention is determined solely by the appended claims.
|
A paper currency (hereinafter "bill") receiving and dispensing machine includes a bill receiving opening in which the bills are deposited, temporary storing boxes for the bills each of which is adapted to temporarily store plural denominations of bills which are deposited in the bill receiving opening and to discharge the stored bills therefrom, and a plurality of bill storing boxes adapted to store the bills discharged from the temporary storing boxes, and to discharge the stored bills therefrom. The bill storing boxes are provided in respective denominations. The machine further includes a first transport passage for communicating the bill receiving opening with the temporary storing boxes such that the bills are moved between the bill receiving opening and the temporary storing boxes, and a second transport passage for communicating the temporary storing boxes with the bill storing boxes such that the bills are moved between the temporary storing boxes and the bill storing boxes. The second transport passage is independently disposed from the first transport passage.
| 6
|
CROSS-REFERENCE TO RELATED APPLICATIONS
A concurrently filed application entitled "Solid State Microwave Power Source For Use In An Electrodeless Light Source" bears Ser. No. 705,324, is assigned to the same assignee herein, and is filed in the name of Robert J. Regan, Paul O. Haugsjaa and William H. McNeill. Also, a concurrently filed application entitled "Continuous Automatic Starting Assist Circuit For A Microwave Powered Electrodeless Lamp" bears Ser. No. 705,328, is assigned to the same assignee herein, and is filed in the name of Robert J. Regan, Paul O. Haugsjaa and William H. McNeill.
BACKGROUND OF THE INVENTION
The present invention relates to microwave excited electrodeless light sources and, more specifically, to an automatic starting control circuit for an electrodeless lamp powered by a solid state microwave source.
There has recently been developed a light source in which an electrodeless lamp is disposed at the ends of inner and outer conductors of a fixture in which the lamp forms a termination load for microwave power supplied at the other end of the conductors. There have also been developed various types of starting assist devices for this type of light source. The need for a starting assist is due to the high impedance mismatch between the lamp in the off state and the output impedance of the power source which results in a low percentage of the forward directed power being absorbed by the lamp. In one starting scheme, the fixture is made to be in a condition of resonance at starting to increase the power absorbed by the lamp. In another scheme, a UV light source is used to supply a flux of UV photons to the lamp. Both schemes have functioned satisfactorily in providing a starting assist. In both starting assist devices, the operator must manually disconnect the devices after the lamp is started. There exists a need for automatic connecting and decoupling of these devices if the electrodeless light source is to have enhanced versatility. It has also been found that a solid state microwave power source can not tolerate running into large impedance mismatches such as occur when the source is coupled to a lamp in the off state.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a reliable starting control circuit for a microwave powered electrodeless lamp in which a starting assist device is automatically coupled into and decoupled out of the light source while also automatically protecting the power source from damage due to large impedance mismatches.
According to the invention, there is provided a control circuit for use in an electrodeless light source having a source of power at a microwave frequency, an electrodeless lamp having an envelope made of a light-transmitting material and a volatile fill material emitting light upon breakdown and excitation and a termination fixture having an inner conductor and an outer conductor disposed around the inner conductor, the conductors having first ends associated with the lamp and second ends coupled to the source so that microwave power terminates at the lamp to cause breakdown and excitation of the fill material. Accordingly, the source includes a dc power source and a microwave power source receiving the dc power for providing microwave power in an amount related to the amount of dc power received by the dc power source, the output of the microwave power source being coupled to the inner and outer conductors. A switch device is provided for controlling the application of dc power to the microwave power source. A UV producing light source is disposed near the lamp and coupled in series between the the dc power source and the microwave power source to emit UV light upon activation of the switch device to assist in starting the lamp. The UV source upon emission of light decreases the amount of dc power coupled to the microwave power source to reduce the output as the lamp is started. A device responsive to a preselected amount of heat from the UV source provides a shunt path for the dc power to bypass the UV source and thereby to provide maximum dc power to the microwave power source. In another aspect, a capacitive impedance device is adapted to be coupled across the conductors at the second end of the fixture to create a resonant condition in the fixture as microwave power is first applied to the lamp. The heat responsive device decouples the capacitive impedance means after the lamp is started. Preferably, the heat responsive device includes a switch having a bimetallic element electrically coupled at a first end to a first side of the UV source, and a first contact electrically coupled to a second side of the UV source. A second end of the bimetallic element moves into contact with the first contact in response to heat to form a shunt path for the dc current through the bimetallic element around the UV source.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing:
The sole FIGURE is a diagram illustrating the principle components according to the present invention.
DESCRIPTION OF PREFERRED EMBODIMENT
In an exemplary embodiment of the present invention, as shown in the FIGURE, there is provided an electrodeless light source represented generally by the reference numeral 10. The source 10 has a source of power represented generally by the reference numeral 12 at a microwave frequency. As used herein, the term "microwave frequency" is intended to include frequencies within the range of 10 MHz to 300 GHz. An electrodeless lamp 14 is provided and has an envelope made of a light-transmitting material, such as quartz, and a volatile fill material emitting light upon breakdown and excitation. A termination fixture represented by the reference numeral 16 has an inner conductor 18 and an outer conductor 20 disposed around the inner conductor 18. The conductors 18 and 20 have first ends 22 and 24, respectively, at which the lamp 14 is disposed and second ends 26 and 28, respectively, which are coupled to the source 12 of microwave power. A transparent dome 23 encloses the second end 24 of the outer conductor. This dome includes a metallic mesh which acts as a shield. Accordingly, the microwave power is absorbed by the lamp 14 to cause breakdown and excitation of the fill material.
According to the invention, a starting control circuit is provided for assisting in the starting of the lamp 14. The source 12 includes a dc power source, which in the embodiment includes an ac source 30, such as a source of power at 60 Hz, and an ac to dc converter 32 for converting the ac power into a dc voltage across output terminals 34 and 36 of the converter 32. The dc power is coupled to a microwave power source 38 via a switch 40. The microwave power source 38 provides an amount of microwave power which is related to the amount of dc power received by the dc power source. The source 38 preferably includes a solid microwave oscillator and a solid state microwave amplifier. Additional details of one suitable power source may be found in the previously mentioned patent application entitled "Solid State Microwave Power Source For Use In An Electrodeless Light Source." The source described in this application includes an oscillator in which a transistor is the active element of a class "C" modified Colpitts type of common base oscillator, a transistorized class "C" power amplifier and an impedance matching circuit utilizing microstrip elements coupled between the output of the amplifier and the first ends 26 and 28 of the fixture 16 for providing an acceptable impedance transformation from the fixture to the collector of the power transistor and for providing a sufficient amount of power to the lamp during the starting mode. The output of the microwave power source 38 is coupled via a transmission line 42, such as a microstrip, to the inner and outer conductors 18 and 20. A UV light source 44 is disposed near the lamp 14 and is coupled in series between the dc power source 32 and the microwave power source 38 to assist in starting the lamp 14. The UV source upon the emission of light decreases the amount of dc power coupled to the microwave power source to reduce the power output as the lamp is started. In the FIGURE the UV source is shown as being displaced from the lamp 14 only for simplification of illustrating the features of the invention. In actual practice, the UV source is located either within the fixture near the first ends 22 and 24 of the conductors or outside the fixture and adjacent the transparent dome 23. A device represented generally by the reference numeral 46 is responsive to heat from the UV source and provides a shunt path for the dc power to bypass the UV source after the lamp is started. This causes maximum power from the converter 32 to be applied to the microwave power source 38.
A reactive impedance device, such as the capacitor 50, is adapted to be coupled across the conductors 18 and 20 near the second ends 26 and 28 to create a resonant condition in the fixture 16 as microwave power is first applied to the lamp. Given the impedance of the lamp at starting, one skilled in the art may determine the required length measured along the conductor 18 separating the lamp 14 and the capacitor 50 and the required reactive impedance of the capacitor to achieve a condition of resonance. According to the invention, the heat responsive device 46 includes the capability for decoupling the capacitor 50 after the lamp is started.
The heat responsive device 46 includes a switch having a bimetallic element 52 electrically coupled at a first end 55 to a first side 56 of the UV source 44 and a first contact 58 electrically coupled to a second side 60 of the UV source 44. The second end 62 of the bimetallic element 52 moves into contact with the first contact 58 in response to heat to form the shunt path for the dc current through the bimetallic element 52 and around the UV source 44. The capacitive impedance is coupled at one side 64 to the outer conductor 20 and at the other side 66 to the side 55 of the bimetallic element 52. A second contact 68 is electrically coupled to the inner conductor 18. The bimetallic element 52 is positioned such that the second end 62 of the bimetallic element 52 is in contact with the second contact 68 prior to movement of the bimetallic element due to heat. This permits the capacitor 50 to be coupled across the conductors 18 and 20 for starting. In operation, the second end 62 of the element 52 moves away from the second contact 68 in response to heat to decouple the capacitor 50 after the lamp is started. In the embodiment, the bimetallic element 52 has a first strip of conductive material made out of a nickel alloy having a low temperature coefficient and a second strip of conductive material made out of a nickel-chrome steel alloy having a higher temperature coefficient.
In operation, the UV source in series with the microwave power source 38 reduces the voltage on the source 38 so that its power output is less than the full voltage value. This reduced power is fed via the transmission line 42 to the fixture 16. With the combination of the UV and the resonant condition brought about by the starting capacitor, this low power level is sufficient to start the lamp. With the low applied dc voltage, the microwave power source can withstand the mismatches occurring during the lamp warm-up. Some predetermined length of time after the microwave lamp is started, the heat generated by the UV source together with the heat generated in the bimetallic element itself due to absorption of microwave power, cause the bimetallic element 52 to bend downwardly thereby closing the lower contacts. This shunts out the UV source and applies full dc voltage to the source, causing it to produce full power. It can safely do this at this point because the microwave lamp is fully warmed-up and presents a matched load to the source. With the lower contacts closed, the bimetallic element carries the dc current. This heats the bimetallic element, helping to keep the lower contacts closed. Heat from the microwave lamp also tends to heat the bimetallic element. When the on-off switch 40 is open, the bimetallic element relaxes as it cools so that the upper contacts are closed and the system is in the ready-to-start mode. Thus, the major advantages according to the present invention are that there is provided a UV source for the lamp, a build-up of the microwave fields in the termination fixture by way of resonance, impedance matching the fixture to the source in the lamp-off condition and switching of the microwave power source from low power at starting to higher power after breakdown occurs in the lamp. These functions are accomplished automatically since once the on-off switch 40 is turned on, the system operates entirely by itself.
The embodiment of the present invention is intended to be merely exemplary and those skilled in the art shall be able to make numerous variations and modifications of it without departing from the spirit and scope of the present invention. All such variations and modifications are intended to be within the scope of the present invention as defined by the appended claims.
|
A starting assist control circuit for an electrodeless light source in which a UV source for assisting in starting an electrodeless lamp is coupled in series with the dc supply for a microwave power source for the lamp so that a reduced dc voltage is supplied to the microwave power source at lamp starting. At staring, a capacitive impedance element is coupled across the inner and outer conductors of the fixture to provide an additional starting assist by creating a condition of resonance in the fixture. A heat responsive bimetallic switch element associated with both the capacitor and the UV source automatically shorts out the UV source and decouples the capacitor after the lamp has started thereby permitting full dc power to the microwave power source during the operating condition of the lamp.
| 7
|
[0001] This application is a Continuation patent application of copending U.S. application Ser. No. 12/736,814, filed 12 Nov. 2010.
RELATIONSHIP TO OTHER APPLICATIONS
[0002] This application claims priority to and benefits of the following: U.S. Provisional Patent Application No. 60/127,588, filed 13 May 2008, entitled “Fluorescence Detection And Deactivation Of Poison Oak Oil”, International Patent Application number PCT/US2009/002958, filed 13 May 2009, entitled “Fluorescence Detection And Deactivation Of Poison Oak Oil”, and U.S. National Phase patent application Ser. No. 12/736,814, filed 12 Nov. 2010, entitled “Fluorescence Detection And Deactivation Of Poison Oak Oil”, each of which is herein incorporated by reference in its entirety for all purposes.
[0003] This invention was made partly using funds from United States National Science Foundation (NSF) research grant No. CHE-0453126. The Federal Government has certain rights to this invention.
FIELD OF THE INVENTION
[0004] The invention provides compositions, kits, and methods of using the compositions and kits for detecting, deactivating, degrading, immunogenic compounds from poison oak and poison ivy.
BACKGROUND
[0005] Urushiol-induced allergic contact dermatitis in the United States most commonly results from unexpected exposure to oils from plants in the sumac Family Anacardiaceae. Approximately 10 to 50 million Americans suffer from rashes resulting from exposure every year. In particular, the genus Toxicodendron species (which include Western and Eastern poison oak T. diversilobum , poison ivy T. radicans , and poison sumac or dogwood T. vernix ) are distributed widely across North America. Other sources of urushiol include poison wood (in Florida and the Bahamas), and the sap (kiurushi) of the Asian lacquer tree ( Toxicodendron vemiciflua ) used as a varnish in Japanese lacquer ware, and cashew nut shells. (See, for example, Tucker and Swan (1998) NEJM, 339(4): 235.)
[0006] Reaction to urushiol is an immunological response to the bio-oxidized form of urushiol (the ortho-quinone). Approximately 50-70% of the U.S. population is either allergic to urushiol, or will become allergic to it upon sensitization by repeated exposure. Symptoms of allergic contact dermatitis from urushiol exposure (often referred to as Rhus dermatitis) vary from a mild annoyance to weeks of irritation and pain. Occasionally, exposure can lead to nephropathy and even to fatal systemic anaphylaxis. The monetary cost due to worker disability from urushiol-induced injuries is substantive: in the states of California, Washington and Oregon, it has been estimated that up to one third of forestry workers are temporarily disabled by poison oak dermatitis each year. In California, the medical costs associated with poison oak injuries accounts for up to 1% of the annual workers' compensation budget. It has been estimated that Toxicodendron dermatitis is responsible for 10% of the total U.S. Forest Services lost-time injuries. In 1988, NIOSH estimated that 1.07-1.65 million occupational skin injuries occurred yearly, with an estimated annual rate of 1.4 to 2.2 cases per 100 workers (8) the costs attributable to lost productivity, medical payments, and disability payments are very high. (See U.S. Centers for Disease Control; Leading work-related diseases and injuries—United States. MMWR, 1986 335:561-563).
[0007] Chemically, urushiol is a name given to a collection of related compounds that are 3-substituted catechols (1,2-benenediols), in which the long hydrophobic chain is a linear C 15 or C 17 alkyl chain containing 0-4 degrees of cis unsaturation ( FIG. 1 ). The catechols with two, three, and four carbon-carbon double bonds (2-4 degrees of unsaturation) seem to be the most virulent in eliciting an allergic response. Each of the different members of the Toxicodendron species contain mixtures of the C 15 or C 17 alkyl chains, with various degrees of unsaturation.
[0008] They all share the catechol functionality in common, and a long, greasy alkyl chain that facilitates migration into the skin. In addition to direct contact with the toxic plants, exposure commonly occurs by transfer from animal fur, contaminated clothing, garden tools, fire-fighting equipment, forestry and sports equipment. There are a few commercially available products that can be applied prophylactically to protect the skin by creating a physical barrier using organoclays (for example, a lotion containing quaternium-18 bentonite is commercially available as IVYBLOCK from Enviroderm Pharmaceuticals, Inc.). However, the success of this strategy requires advanced planning By far the majority of allergic contact dermatitis cases from urushiol result from unexpected exposure.
[0009] A number of methods to treat poison ivy or poison oak have been investigated, including hyposensitization, but this process is involved and can have unfavorable side effects. Studies towards an immunological approach to desensitization have been pursued, but have not yet reached a level of practical application. The best treatment to date is to avoid contact with urushiol. As most patients are unaware that they have had contact with urushiol, a low cost, quick and inexpensive method of detection is warranted. There are many recommended methods to remove urushiol after recent contact, including water, soapy water, organic solvents, and a variety of commercially available solubilizing mixtures including TECHNU, IVYCLEANSE, ALL-STOP, ZANFEL (comprising fatty acid, alcohol, and the surfactant sodium lauroyl sarcosinate), and even DIAL ultra dishwashing soap. Thus the ability to detect urushiol before it transverses the skin will be extremely valuable in mitigating the suffering caused by contact with the various Toxicodendron species. In addition, continued re-exposure (chronic exposure) from repeated introduction of the oil to the patient (from door handles, shoelaces, etc.) is a considerable problem. As little as 0.001 mg of urushiol is enough to cause allergic contact dermatitis.
[0010] Treatment of the contact dermatitis usually involves a course of topical and/or enteric treatments with hydrocortisones, β-methasone, and other similar corticosteroids. Repeated exposure to either the original allergen or to a similar allergen can result in a severe hypersensitive immunoreaction, that is often extremely painful and, occasionally, fatal. There is therefore a particular need in the art for compounds and methods of treatment that can remove the allergen(s) prior to induction of an immune and/or allergic response, that can prevent the binding of the allergen(s) to an immunoglobulin or a cell-surface receptor, and/or that can be used to rapidly detect the presence of such allergen(s) so that other precautions may be used to remove the allergen(s) from the area of contact.
[0011] There is therefore a need in the art to provide for compositions and methods for detecting the presence of urushiol, inactivating urushiol, and removing urushiol from substrates (including, for example, skin and clothing).
BRIEF DESCRIPTION OF THE INVENTION
[0012] The invention is drawn to novel methods, kits, sprays (including aerosol sprays) and compositions for detecting active compounds present in oils that are found in poison oak, poison ivy, poison sumac, cashew nut, and related plants. The methods disclosed herein may also be used to detect other catechols, both synthetic and those found in nature. The invention also is drawn to compositions that may be used to detect said active compounds using fluorescence. In one embodiment the methods of the invention may be used to detect catechols and alkyl-substituted catechols, such as, for example, urushiol, catechin, epicatechin, gallocatechin, epigallocatechin, epigallocatechin-3-gallate, and the like; and chatecholamines, such as, for example, epinephrine, norepinephrine, dopamine, dihydroxyphenylalanine (DOPA), and the like.
[0013] The invention provides methods for detecting, treating, and deactivating the antigenic and/or allergenic compounds that induce urushiol-induced contact dermatitis. In one embodiment the method may be used for treating, deactivating, and/or detecting alk(en)yl catechols, and/or alk(en)yl resorcinols.
[0014] The invention may be used by clinicians, nursing staff, paramedics, emergency rescue team members, the military, firefighters, forestry personnel, lumberworkers, hunters, mountaineers, hikers, anglers, and the like. In one embodiment, the invention is a kit comprising the elements disclosed herein and a set of instructions of how to use the kit, wherein the kit is used for detecting, treating, and/or deactivating a catechol. The kit can be used, for example, in the home, in the field, in a camp, in a clinic, in a hospital, in an emergency room, and the like.
[0015] The invention provides a kit for detecting a catechol, the kit comprising a vessel, the vessel shaped and adapted for confining a composition, the composition further comprising a boron composition, a first nitroxide, and a second nitoxide, and an applicator. In one embodiment the boron composition comprises a hydrophobic alkyl group. In another embodiment the second nitroxide is a profluorescent nitroxide. In a preferred embodiment the applicator is a spray applicator. In a most preferred embodiment the catechol is urushiol. In one alternative embodiment, the kit can also comprise an aerosol propellant. In another embodiment the kit comprises a lamp.
[0016] In a preferred embodiment, the invention provides a method for detecting a catechol in a sample, the method comprising the steps of (i) contacting a boron composition and a nitroxide with the sample (ii) allowing the boron composition to react with the catechol in the sample thereby creating a catecholborane; (iii) allowing a first nitroxide to react with the catecholborane thereby generating an alkyl radical and a nitroxide-catecholborane complex; (iv) allowing the alkyl radical to react with a second nitroxide thereby creating an alkoxyamine; (v) measuring the amount of alkoxyamine, nitroxide-catecholborane complex, or an alkoxyamine hydrolysis product so created; the method resulting in detecting the catechol in the sample. In one embodiment the boron composition comprises a hydrophobic alkyl group. In a preferred embodiment, the catecholborane is a B-alkyl catecholborane. In another preferred embodiment the alkyl group is selected from the group consisting of a hydrophobic alkyl group and a hydrophilic alkyl group. In a yet alternative embodiment the nitroxide is a profluorescent nitroxide. More preferably, the nitroxide is tetramethylpiperidinyloxy (TEMPO). In a more preferred embodiment the profluorescent nitroxide is dansyl amino-TEMPO. In another preferred embodiment the sample is selected from the group consisting of an area of a subject's skin, clothing, boots, pets, camping gear, tools, and other outdoor equipment. In another preferred embodiment the sample is selected from the group consisting of a plant tissue, a plant extract, a plant tissue extract, an animal tissue, an animal extract, an animal tissue extract, and an animal fluid. In a more preferred embodiment the plant tissue is from a plant selected from the group consisting of poison oak, poison ivy, poison sumac, mango, cashew nut, and lac tree.
[0017] The invention further provides the methods as disclosed herein wherein the nitroxide further comprises a fluorescent compound, the fluorescent compound selected from the group consisting of a hydrophobic fluorescent organic molecule, a hydrophilic fluorescent organic molecule, and a fluorescent quantum-dot nanoparticle.
[0018] In one embodiment the method comprises the measuring the amount of alkoxyamine so created using a photon source that results in fluorescence of the alkoxyamine and the nitroxide-catecholborane complex, wherein the fluorescence is visible to the naked eye. In a preferred embodiment the measuring of the amount of alkoxyamine so created is performed using a photon source that induces fluorescence of the alkoxyamine and the nitroxide-catecholborane complex, wherein the fluorescence is detected by a photometer. In a more preferred embodiment the fluorescence comprises photons having a wavelength of between about 250 and 600 nm. In one embodiment the photon source is a lamp. In a preferred embodiment the lamp is a hand-held lamp. In an alternative embodiment the photon source is the sun. The method may also further comprise measuring hydroxylamine complexed with boron or free hydroxylamine created by hydrolysis.
[0019] In a preferred embodiment of the invention the catechol is selected from the group consisting of urushiol, catechin, epicatechin, gallocatechin, epigallocatechin, epigallocatechin-3-gallate, and catecholamines epinephrine, norepinephrine, dopamine, and dihydroxyphenylalanine (DOPA). In a more preferred embodiment the catechol is urushiol.
[0020] The method may further comprise the step of reacting the alkyl radical with a profluorescent nitroxide having a fluorescent tag, wherein the fluorescent tag is selected from the group consisting of an organic fluorophore and Cd—Se nanoparticle. In another embodiment the method may further comprise the step of measuring the amount of the nitroxide-catecholborane complex. In another embodiment the method further comprises the step of measuring the amount of hydroxylamine hydrolysis product. In a yet other embodiment the method further comprises the step of measuring the amount of alkoxyamine product.
[0021] The invention also provides for a method for deactivating a catechol in a sample, the method comprising the steps of (i) contacting a boron composition and an oxygen-containing molecule with the sample (ii) allowing the boron composition to react with the catechol in the sample thereby creating a catecholborane; the method resulting in deactivating the catechol in the sample. In one embodiment the boron composition comprises a hydrophobic alkyl group. In a preferred embodiment, the catecholborane is a B-alkyl catecholborane. In another preferred embodiment the alkyl group is selected from the group consisting of a hydrophobic alkyl group and a hydrophilic alkyl group. In a yet alternative embodiment the nitroxide is a profluorescent nitroxide. More preferably, the nitroxide is tetramethylpiperidinyloxy (TEMPO). In a more preferred embodiment the profluorescent nitroxide is dansyl amino-TEMPO. In another preferred embodiment the sample is selected from the group consisting of an area of a subject's skin, clothing, boots, pets, camping gear, tools, and other outdoor equipment. In another preferred embodiment the sample is selected from the group consisting of a plant tissue, a plant extract, a plant tissue extract, an animal tissue, an animal extract, an animal tissue extract, and an animal fluid. In a more preferred embodiment the plant tissue is from a plant selected from the group consisting of poison oak, poison ivy, poison sumac, mango, cashew nut, and lac tree.
[0022] In one preferred embodiment the oxygen-containing molecule comprises a nitroxide. The invention further provides the methods as disclosed herein wherein the nitroxide further optionally comprises a fluorescent compound, the fluorescent compound selected from the group consisting of a hydrophobic fluorescent organic molecule, a hydrophilic fluorescent organic molecule, and a fluorescent quantum-dot nanoparticle.
[0023] In one embodiment the method comprises the measuring the amount of alkoxyamine so created using a photon source that results in fluorescence of the alkoxyamine and the nitroxide-catecholborane complex, wherein the fluorescence is visible to the naked eye. In a preferred embodiment the measuring of the amount of alkoxyamine so created is performed using a photon source that induces fluorescence of the alkoxyamine and the nitroxide-catecholborane complex, wherein the fluorescence is detected by a photometer. In a more preferred embodiment the fluorescence comprises photons having a wavelength of between about 250 and 600 nm.
[0024] The method may also further comprise measuring hydroxylamine complexed with boron or free hydroxylamine created by hydrolysis.
[0025] In a preferred embodiment of the invention the catechol is selected from the group consisting of urushiol, catechin, epicatechin, gallocatechin, epigallocatechin, epigallocatechin-3-gallate, and catecholamines epinephrine, norepinephrine, dopamine, and dihydroxyphenylalanine (DOPA). In a more preferred embodiment the catechol is urushiol.
[0026] The invention also provides for a boron composition, the boron composition comprising a reactive moiety that reacts with a catechol with a rate constant, k, of at least 0.2 M −1 s −1 and wherein the reaction produces a stable chatecholborane.
[0027] The invention provides for a pharmaceutical composition, the pharmaceutical composition comprising a boron composition, wherein the boron composition comprises a hydrophobic alkyl group. In one embodiment the alkyl group is selected from the group consisting of a hydrophobic alkyl group and a hydrophilic alkyl group. In another embodiment the pharmaceutical composition comprises a boron composition in an effective amount for the treatment of poison oak oil-induced contact dermatitis. In a preferred embodiment the poison oak oil comprises a catechol. In a more preferred embodiment the catechol is urushiol.
[0028] The invention provide a topical composition, the topical composition comprising an effective amount of a boron composition and a suitable excipient, carrier, or combination thereof, the boron composition comprising an alkylboronic acid having the general formula R—B(OH) 2 . In one alternative embodiment the boron composition optionally comprises at least one B-alkyl boronic acid derivative. In another embodiment the topical composition optionally containing xanthan gum or gellan gum. In a more preferred embodiment the boron composition is present in an amount selected from the group consisting of from about 99.5% to about 0.001%, from about 95% to about 0.1%, and from about 90% to about 0.5%, by weight, based on the total combined weight of the boron composition thereof, not including other excipient, carrier, or combination thereof. In a most preferred embodiment the topical composition comprises a boron composition in an effective amount for the detection of a catechol in poison oak oil.
[0029] The invention further provides a topical medicament, the topical medicament comprising a boron composition, the boron composition comprising an alkylboronic acid having the general formula R—B(OH) 2 , a nitroxide, and a suitable excipient, carrier, or combination thereof, and where R is selected from the group consisting of a hydrophobic alkyl group and a hydrophilic alkyl group. In an alternative embodiment the boron composition optionally comprises at least one B-alkyl boronic acid derivative. In a more preferred embodiment the nitroxide is a profluorescent nitroxide. In a more preferred embodiment the topical medicament comprises a boron composition in an effective amount for the detection of a catechol in poison oak oil to avoid induced contact dermatitis. In another more preferred embodiment the topical medicament comprises a boron composition in an effective amount for the treatment of poison oak oil-induced contact dermatitis.
[0030] In one embodiment, the invention provides a method for detecting, treating, and deactivating alk(en)yl catechols, and/or alk(en)yl resorcinols using a boron compound bearing a hydrophobic alkyl group and an at least one equivalent of profluorescent nitroxide are that are mixed in solution or on a substrate. In one preferred embodiment, the profluorescent nitroxide is a nitroxide with a short tether to a fluorescent dye, wherein the dye is quenched in the presence of the free nitroxide. In an alternative embodiment the boron compound further comprises an alkyl boronic acid or alkyl boronic acid derivative. In another alternative embodiment the boron compound further comprises at least one leaving group. In yet another alternative embodiment, the boron compound further comprises two leaving groups.
[0031] In one embodiment the invention provides a method for detecting, treating, and deactivating alk(en)yl catechols, and/or alk(en)yl resorcinols, wherein the method results in producing a fluorescent compound that fluoresces when illuminated and wherein the fluorescence is induced by photons having a wavelength of between about 250 and 600 nm. In one embodiment the fluorescence can be, for example, between 250 and 300 nm, between 300 and 350 nm, between 350 and 400 nm, between 450 and 500 nm, between 500 and 550 nm, and between 550 and 600 nm. In the alternative, the method results in producing a fluorescent compound that fluoresces when illuminated with light in the visible spectrum and wherein the fluorescence is induced by photons having a wavelength of between about 600 and 750 nm. In one embodiment the fluorescence can be, for example, between 600 and 650 nm, between 650 and 700 nm, and between 700 and 750 nm.
[0032] In another alternative embodiment, the nitroxide can comprise a fluorescent tag such as, for example, a fluorescent organic compound, such as dansyl, 3-hydroxy-2-methyl-4-quinolinecarboxylic ester, a coumarin, a xanthene, a cyanine, a pyrene, a borapolyazaindacene, an oxazine, bimane, 4-acetamido-4′-isothiocyanatostilbene-2,2′-disulfonic acid (SITS) and related stilbene derivatives, and the isothiocyanate of pyrenetrisulfonic acid, fluorescein, acryoldan, rhodamine, dipyrrometheneboron difluoride (BODIPY), acridine orange, eosin, acridine orange, 1-(3-(succinimidyloxycarbonyl)benzyl)-4-(5-(4-methoxyphenyl)oxazol-2-yl)pyridinium bromide (PyMPO), alexa fluor 488, alexa fluor 532, alexa fluor 546, alexa fluor 568, alexa fluor 594, alexa fluor 555, alexa fluor 633, alexa fluor 647, alexa fluor 660 and alexa fluor 680, or the like, or a quantum-dot nanoparticle. In the present invention, a non-limited list of quantum dot nanoparticles includes cadmium sulfide (CdS), cadmium selenide (CdSe), zinc sulfide (ZnS), zinc oxide (ZnO), lead sulfide (PbS), zinc selenide (ZnSe), GaAS, and InP. (Lakowicz et al., Anal. Biochem., 2000, 280: 128-136.
[0033] The invention further provides use of a composition comprising a boron composition for the manufacture of a composition for detecting a catechol. In one embodiment the boron composition comprises an alkylboronic acid having the general formula R—B(OH) 2 , a nitroxide, and a suitable excipient, carrier, or combination thereof, and where R is selected from the group consisting of a hydrophobic alkyl group and a hydrophilic alkyl group. In one alternative embodiment the boron composition optionally comprises at least one B-alkyl boronic acid derivative. In a preferred embodiment the nitroxide is a profluorescent nitroxide. In another preferred embodiment the composition comprises a boron composition in an effective amount for the detection of a catechol in poison oak oil.
[0034] The invention can be used in a variety of embodiments, for example, for use as chemical sensors and molecular specific deactivating agents. The invention can be used in phototherapy for treatment of an inflammatory response and other disorders. The invention can also be used as a sensor that detects molecules. The invention is of particular use in the fields of clinical diagnosis, clinical therapy, clinical treatment, and clinical evaluation of various diseases and disorders, in the field of consumer goods, for example, over-the-counter medications, balms, ointments, etc., and diagnostic kits, manufacture of compositions for use in the treatment of various diseases and disorders, for use in molecular biology, structural biology, cell biology, molecular switches, molecular circuits, and molecular computational devices, and the manufacture thereof.
[0035] In one embodiment, the composition comprises a surface stabilizer. In another alternative embodiment the composition comprises at least two surface stabilizers. In a preferred embodiment, the surface stabilizer is selected from the group consisting of an anionic surface stabilizer, a cationic surface stabilizer, a zwitterionic surface stabilizer, and an ionic surface stabilizer.
[0036] In another preferred embodiment, the surface stabilizer is selected from the group consisting of cetyl pyridinium chloride, gelatin, casein, phosphatides, dextran, glycerol, gum acacia, cholesterol, tragacanth, stearic acid, benzalkonium chloride, calcium stearate, glycerol monostearate, cetostearyl alcohol, cetomacrogol emulsifying wax, sorbitan esters, polyoxyethylene alkyl ethers, polyoxyethylene castor oil derivatives, polyoxyethylene sorbitan fatty acid esters, polyethylene glycols, dodecyl trimethyl ammonium bromide, polyoxyethylene stearates, colloidal silicon dioxide, phosphates, sodium dodecylsulfate, carboxymethylcellulose calcium, hydroxypropyl celluloses, hypromellose, carboxymethylcellulose sodium, methylcellulose, hydroxyethylcellulose, hypromellose phthalate, noncrystalline cellulose, magnesium aluminum silicate, triethanolamine, polyvinyl alcohol, polyvinylpyrrolidone, 4-(1,1,3,3-tetramethylbutyl)-phenol polymer with ethylene oxide and formaldehyde, poloxamines, a charged phospholipid, dioctylsulfosuccinate, dialkylesters of sodium sulfosuccinic acid, sodium lauryl sulfate, alkyl aryl polyether sulfonates, mixtures of sucrose stearate and sucrose distearate, p-isononylphenoxypoly-(glycidol), decanoyl-N-methylglucamide; n-decyl β-D-glucopyranoside; n-decyl β-D-maltopyranoside; n-dodecyl β-D-glucopyranoside; n-dodecyl β-D-maltoside; heptanoyl-N-methylglucamide; n-heptyl-β-D-glucopyranoside; n-heptyl β-D-thioglucoside; n-hexyl β-D-glucopyranoside; nonanoyl-N-methylglucamide; n-noyl β-D-glucopyranoside; octanoyl-N-methylglucamide; n-octyl-β-D-glucopyranoside; octyl β-D-thioglucopyranoside; lysozyme, PEG-phospholipid, PEG-cholesterol, PEG-cholesterol derivative, and PEG-vitamin A.
[0037] In another alternative embodiment, the cationic surface stabilizer is selected from the group consisting of a polymer, a biopolymer, a polysaccharide, a cellulosic, an alginate, a nonpolymeric compound, and a phospholipid.
[0038] In another alternative embodiment, the surface stabilizer is selected from the group consisting of cationic lipids, polymethylmethacrylate trimethylammonium bromide, sulfonium compounds, polyvinylpyrrolidone-2-dimethylaminoethyl methacrylate dimethyl sulfate, hexadecyltrimethyl ammonium bromide, phosphonium compounds, quarternary ammonium compounds, benzyl-di(2-chloroethyl)ethylammonium bromide, coconut trimethyl ammonium chloride, coconut trimethyl ammonium bromide, coconut methyl dihydroxyethyl ammonium chloride, coconut methyl dihydroxyethyl ammonium bromide, decyl triethyl ammonium chloride, decyl dimethyl hydroxyethyl ammonium chloride, decyl dimethyl hydroxyethyl ammonium chloride bromide, C 12-15 dimethyl hydroxyethyl ammonium chloride, C 12-15 -dimethyl hydroxyethyl ammonium chloride bromide, coconut dimethyl hydroxyethyl ammonium chloride, coconut dimethyl hydroxyethyl ammonium bromide, myristyl trimethyl ammonium methyl sulphate, lauryl dimethyl benzyl ammonium chloride, lauryl dimethyl benzyl ammonium bromide, lauryl dimethyl (ethenoxy)4 ammonium chloride, lauryl dimethyl (ethenoxy)4 ammonium bromide, N-alkyl (C 12-18 )dimethylbenzyl ammonium chloride, N-alkyl (C 14-18 )dimethyl-benzyl ammonium chloride, N-tetradecylidmethylbenzy-1 ammonium chloride monohydrate, dimethyl didecyl ammonium chloride, N-alkyl and (C 12-14 ) dimethyl 1-napthylmethyl ammonium chloride, trimethylammonium halide, alkyl-trimethylammonium salts, dialkyl-dimethylammonium salts, lauryl trimethyl ammonium chloride, ethoxylated alkyamidoalkyldialkylammonium salt, an ethoxylated trialkyl ammonium salt, dialkylbenzene dialkylammonium chloride, N-didecyldimethyl ammonium chloride, N-tetradecyldimethylbenzyl ammonium, chloride monohydrate, N-alkyl(C 12-14 ) dimethyl 1-naphthylmethyl ammonium chloride, dodecyldimethylbenzyl ammonium chloride, dialkyl benzenealkyl ammoniumchloride, lauryl trimethyl ammonium chloride, alkylbenzyl methyl ammonium chloride, alkyl benzyl dimethyl ammonium bromide, C 12 trimethyl ammonium bromides, C 15 trimethyl ammonium bromides, C 17 trimethyl ammonium bromides, dodecylbenzyl triethyl ammonium chloride, poly-diallyldimethylammonium chloride (DADMAC), dimethyl ammonium chlorides, alkyldimethylammonium halogenides, tricetyl methyl ammonium chloride, decyltrimethylammonium bromide, dodecyltriethylammonium bromide, tetradecyltrimethylammonium bromide, methyl trioctylammonium chloride, polyquaternium 10, tetrabutylammonium bromide, benzyl trimethylammonium bromide, choline esters, benzalkonium chloride, stearalkonium chloride compounds, cetyl pyridinium bromide, cetyl pyridinium chloride, halide salts of quaternized polyoxyethylalkylamines, quaternized ammonium salt polymers, alkyl pyridinium salts; amines, amine salts, amine oxides, imide azolinium salts, protonated quaternary acrylamides, methylated quaternary polymers, and cationic guar.
[0039] The invention also provides for a chemical spray that can be used in the field to allow the detection of urushiol in conjunction with the use of a fluorescent lamp. In one embodiment the amount of urushiol detected is in the range of between about 0.1-100 μg. In a preferred embodiment, the amount of urushiol detected is in the range of between about 1-10 μg.
BRIEF DESCRIPTION OF THE DRAWINGS
[0040] FIG. 1 illustrates the chemical formulae of chatechol and exemplary urushiols.
[0041] FIG. 2 illustrates how B-alkyl catechol borane species react with oxygen radicals to expel alkyl radicals (adapted from Darency and Renaud, 2006, Top. Curr. Chem., 263: 71-106; Cadot et al. 2002, JOC, 67: 7193-7202; Baban et al. 1986, J. Chem. Soc., Perkin Trans. 2: 157).
[0042] FIG. 3 illustrates a modified Brown and Negishi reaction that may comprise chain transfers with PTOC-OMe for radical acceptors (Brown and Negishi, 1971, J. Am. Chem. Soc. 93: 3777; Suzuki et al. 1969, J. Chem. Soc., Chem. Commun, 17: 1009; Forster 1999, PhD Thesis, University de Fribourg, Switzerland, Diss Nr. 1242; Ollivier and Renaud 1999, Chem. Eur. J., 5: 1468; Kumli and Renaud, 2006, Org. Lett. 8: 5861; Olivier and Renaud, 2000, Angew. Chem. Int. Ed. 39: 925).
[0043] FIG. 4 illustrates novel methods for detecting poison oak oil (including poison ivy, sumac oil, and lac tree extracts) that are present upon a substrate by chemical generation of fluorescence.
[0044] FIG. 5 illustrates an exemplary reaction between a nitroxide (for example, TEMPO) and a catechol that results in a nitroxide-catecholborane.
[0045] FIG. 6 illustrates an exemplary reaction between a profluorescent nitroxide and a catechol that results in a fluorescent nitroxide-catecholborane.
[0046] FIG. 7A illustrates details of another exemplary reaction between either a borane compound (top), a catecholborane (middle and bottom), and a nitroxide or profluorescent nitroxide that results in no reaction (top), production of a nitroxide-catecholborane (middle), or production of a fluorescent nitroxide-catecholborane (bottom). FIG. 7B illustrates details of how a reaction between a profluorescent nitroxide in the presence of phenylhydrazine results in production of a fluorescent compound.
[0047] FIG. 8 illustrates that addition of an oxygen radical to an alkylcatecholborane forms a perboryl radical 5, visible by ESR
[0048] FIG. 9 illustrates that addition of nitroxide to an alkylcatecholborane forms a perboryl radical 6, which fragments to generate an alkyl radical. A second equivalent of nitroxide reacts with the alkyl radical to form alkoxyamine 8.
[0049] FIG. 10 shows exemplary profluorescent nitroxides: the free nitroxide quenches fluorescence of a closely tethered fluorophore; fluorescence is restored upon reaction to from the alkoxyamine or hydroxylamine.
[0050] FIG. 11 illustrates a reaction sequence that may detect catechol using profluorescent nitroxide addition to alkylcatecholborane 13.
[0051] FIG. 12 illustrates use of profluorescent Dansyl amino-TEMPO: preparation, reduction, and formation of radical trapping product 17.
[0052] FIG. 13 shows an exemplary reaction of a model alkyl-catecholborane 19 with two equivalents of nitroxide: both alkoxyamine and hydroxylamine 21 were isolated from the reaction mixture.
[0053] FIG. 14 illustrates reaction of profluorescent Dansyl amino-TEMPO 16 with n-butylcatecholborane 19 in toluene to give fluorescent n-butylalkoxyamine 22 (A): paper towel spot test shows fluorescence of alkoxyamine 22 (B).
[0054] FIG. 15 shows the in situ formation of n-butylcatecholborane 19 and subsequent reaction to form fluorescent 22 (A) in one pot (B).
[0055] FIG. 16 illustrates common classes of readily synthesized stable nitroxides.
[0056] FIG. 17 illustrates a general synthesis pioneered by Hideg and Keana for the preparation of proxyl nitroxides 42.
[0057] FIG. 18 shows the synthesis of the pyrene proxyl profluorescent nitroxide 44.
[0058] FIG. 19 illustrates a few representative known profluorescent nitroxides.
[0059] FIG. 20 illustrates the excitation and emission spectra of profluorescent nitroxide 12 and fluorescent N-alkoxyamine 28 in DMSO.
[0060] FIG. 21 shows a hydroboration route to prepare n-alkylboronic acids 25
[0061] FIG. 22 illustrates representative pyrogallols and catechols commonly found in foods such as red wine, tea, and chocolate: note that compounds 48 and 49 are polyols, and are thus aqueous rather than organic soluble.
[0062] FIG. 23 illustrates a slow reduction of nitroxide by catechol; rapid reoxidation of the hydroxylamine to the nitroxide with PbO 2 .
[0063] FIG. 24 illustrates fluorescence quenching and recovery upon addition of catechol to profluorescent nitroxide 12, with and without addition of PbO 2 as a reoxidant.
[0064] FIG. 25 illustrates how exemplary mild oxidants can rapidly oxidize hydroxylamine to nitroxide but that do not oxidize catechol to quinone.
[0065] FIG. 26 illustrates detection of urushiol on leaves of poison oak. A: Fresh Poison Oak triad of leaves; B: Print of the same leaves on a paper towel after treatment with Fl-NitO., nBuB(OH) 2 and catalytic PbO 2 in acetone.
DETAILED DESCRIPTION OF THE INVENTION
[0066] In order to develop a system to selectively detect catechols in the presence of other alcohols and diols (such as sugars), a reaction that takes place with catechols but not with other alcohols was required. In the field of organic free radical chemistry, alkylcatecholboranes have been used to selectively generate alkyl radicals upon reaction with oxygen radicals. The efficacy of this oxygen radical addition specifically to alkylcatecholboranes is due to de-localization of the unpaired electron of the perboryl species 5 into the aromatic ring ( FIG. 8 ). Direct ESR evidence for this delocalized perboryl radical 5 below 270 K was observed by Roberts (Baban et al., J. Chem. Soc. Perkin Transact. 1986, 2(1): 157-161). A number of very useful synthetic methodologies have been developed from this chemistry. Key to this proposal is the work by Renaud, in which addition of two equivalents of the oxygen radical TEMPO 7, a commercially available persistent nitroxide radical, results in formation of the carbon radical trapping product, alkoxyamine 8 ( FIG. 9 ).
[0067] In order to design a visual indicator of the reaction of nitroxides with alkylcatecholboranes, profluorescent nitroxides are used. Profluorescent nitroxides 10 (sometimes referred to as “pre-fluorescent nitroxides”) are nitroxides bearing a short covalent tether to a fluorophore. The free nitroxide quenches the fluorescence. Upon reaction of the nitroxide moiety to form an alkoxyamine 11 or a hydroxylamine (or any other non-nitroxide product), the fluorescence is no longer quenched, restoring fluorescence to the product ( FIG. 10 ). Profluorescent nitroxides have been utilized as sensors of nitric oxide, antioxidants, reactive oxygen species, carbon radicals, cationic metals, viscosity probes, as a chemical logic gate, and in the development of photomagnetic materials. (See Ivan, M. G.; Scaiano, J. C., Photochemistry and Photobiology 2003, 78, (4), 416-419; Hornig, F. S.; Korth, H. G.; Rauen, U.; de Groot, H.; Sustmann, R., Helvetica Chimica Acta 2006, 89, (10), 2281-2296; Lozinsky, E. M.; Martina, L. V.; Shames, A. I.; Uzlaner, N.; Masarwa, A.; Likhtenshtein, G. I.; Meyerstein, D.; Martin, V. V.; Priel, Z., Analytical Biochemistry 2004, 326, (2), 139-145; Meineke, P.; Rauen, U.; de Groot, H.; Korth, H. G.; Sustmann, R., Chemistry-a European Journal 1999, 5, (6), 1738-1747; Meineke, P.; Rauen, U.; de Groot, H.; Korth, H. G.; Sustmann, R., Biological Chemistry 2000, 381, (7), 575-582; Blough, N. V.; Simpson, D. J., Journal of the American Chemical Society 1988, 110, (6), 1915-1917; Lozinsky, E.; Martin, V. V.; Berezina, T. A.; Shames, A. I.; Weis, A. L.; Likhtenshtein, G. I., Journal of Biochemical and Biophysical Methods 1999, 38, (1), 29-42; Tang, Y. L.; He, F.; Yu, M. H.; Wang, S.; Li, Y. L.; Zhu, D. B., Chemistry of Materials 2006, 18, (16), 3605-3610; Hideg, E.; Kalai, T.; Kos, P. B.; Asada, K.; Hideg, K., Photochemistry and Photobiology 2006, 82, (5), 1211-1218; Aspee, A.; Garcia, O.; Maretti, L.; Sastre, R.; Scaiano, J. C., Free radical reactions in poly(methyl methacrylate) films monitored using a prefluorescent quinoline-TEMPO sensor. Macromolecules 2003, 36, (10), 3550-3556; Aspee, A.; Maretti, L.; Scaiano, J. C., Photochemical & Photobiological Sciences 2003, 2, (11), 1125-1129; Ballesteros, O. G.; Maretti, L.; Sastre, R.; Scaiano, J. C., Macromolecules 2001, 34, (18), 6184-6187; Blinco, J. P.; McMurtrie, J. C.; Bottle, S. E., European Journal of Organic Chemistry 2007, 4638-4641; Coenjarts, C.; Garcia, O.; Llauger, L.; Palfreyman, J.; Vinette, A. L.; Scaiano, J. C., Journal of the American Chemical Society 2003, 125, (3), 620-621; Dang, Y. M.; Guo, X. Q., Applied Spectroscopy 2006, 60, (2), 203-207; Fairfull-Smith, K. E.; Blinco, J. P.; Keddie, D. J.; George, G. A.; Bottle, S. E., Macromolecules 2008, 41, 1577-1580; Gerlock, J. L.; Zacmanidis, P. J.; Bauer, D. R.; Simpson, D. J.; Blough, N. V.; Salmeen, I. T., Free Radical Research Communications 1990, 10, (1-2), 119-121; Johnson, C. G.; Caron, S.; Blough, N. V., Analytical Chemistry 1996, 68, (5), 867-872; Maurel, V.; Laferriere, M.; Billone, P.; Godin, R.; Scaiano, J. C., Journal of Physical Chemistry B 2006, 110, (33), 16353-16358; Micallef, A. S.; Blinco, J. P.; George, G. A.; Reid, D. A.; Rizzardo, E.; Thang, S. H.; Bottle, S. E., Polymer Degradation and Stability 2005, 89, (3), 427-435; Nagy, V. Y.; Bystryak, I. M.; Kotelnikov, A. I.; Likhtenshtein, G. I.; Petrukhin, O. M.; Zolotov, Y. A.; Volodarskii, L. B., Analyst 1990, 115, (6), 839-841; Arye, P. P.-B.; Strashnikova, N.; Likhtenshtein, G. I., Journal of Biochemical and Biophysical Methods 2002, 51, (1), 1-15; and Wang, H. M.; Zhang, D. Q.; Guo, X. F.; Zhu, L. Y.; Shuai, Z. G.; Zhu, D. B., Chemical Communications 2004, (6), 670-671.)
[0068] The use of a profluorescent nitroxide with an alkylboronic acid derivative 12 is envisioned to react with catechols (such as, but not limited to, for example, urushiol) to form alkylboronate 13: nitroxide addition, radical 14 generation, and nitroxide trapping will generate the fluorescent signal of alkoxyamine 15. Other alkylboronic acid derivatives will be apparent to those of skill in the art.
[0069] Catechols are a group of compounds well-known to those of skill in the art having diverse biological activities, whilst at the same time being structurally conservative. The invention contemplates that the compositions and methods disclosed herein may be used to detect, inactivate, or bind to any biologically-active catechol composition. In particular the invention contemplates a catechol selected from the group consisting of urushiol, catechin, epicatechin, gallocatechin, epigallocatechin, epigallocatechin-3-gallate, and catecholamines epinephrine, norepinephrine, dopamine, and dihydroxyphenylalanine (DOPA). One of skill in the art would consider that the structures of catechols are sufficiently similar that they are a well-known chemical class of compounds.
[0070] Profluorescent nitroxide is sometimes referred to as a pre-fluorescent nitroxide. In the presence of a catechol such as urushiol and an B-alkylboronic acid derivative, a B-alkyl catecholborionate is formed. Addition of the nitroxide to the catecholborane results in expulsion of an alkyl radical, which is trapped by a second nitroxide, forming two fluorescent species: an alkoxyamine with a fluorescent tag, and fluorescently tagged nitroxide-catecholborane complex. In addition, the nitroxide-catecholborane may degrade to hydroxylamine that is also a fluorescent compound. Use of a hand-held fluorescent lamp shows fluorescence when a catechol such as urushiol is present. This can be used as a method to detect the presence of urushiol. As a treatment, binding of the urushiol into a catecholborane complex will prevent transfer through the skin, preventing oxidation of the catechol and elicitation of an immune response, thus preventing contact dermatitis. For detecting aqueous soluble catechols such as dopamine, epinephrine, and norepinephrine, a water-soluble alkyl group is preferred on the initial boron compound rather than a hydrophobic alkyl group.
[0071] Examples of profluorescent nitroxides may be found in the following non-exhaustive list of publications: Blough, 1988, JACS, 110: 1915; Bottle, 2005, Polym. Degrad. & Stability, 89: 427-435; Sciano, 2001, Macromol. 34: 6184; Ibid., 2003, JACS, 125: 620; Ibid., 2003, Photochem. Photobiol. 78: 416; Turro, 2001, Macromol., 34: 8187; Koth, 2000, Biological Chem., 381(7): 575-582; Ibid., 1999, Chem. Eur. J. 5(6): 1738-1747; Ibid., 1997, Ang. IEE, 36: 1501-1503; Ibid., 2006, Hely. Chim Acta, 89: 2281-2296; Hideg 2006, Photochem. Photobiol. 82: 1211; Want, 2006, Chem. Mater., 18: 3605; and Dang and Guo, 2006, Appl. Spectrosc. 60: 203-207,
[0072] In the present invention, a non-limited list of quantum dot nanoparticles includes cadmium sulfide (CdS), cadmium selenide (CdSe), zinc sulfide (ZnS), zinc oxide (ZnO), lead sulfide (PbS), zinc selenide (ZnSe), GaAS, and InP. (Lakowicz et al. Analytical Biochemistry, 2000, 280: 128-136). Alternative suitable donor fluorophores will be apparent to those of ordinary skill without undue experimentation. For example, nitroxides tethered to such a quantum dot will quench any fluorescence; when the nitroxides react with a catechol boronate complex, the quenching effect is removed and fluorescence can occur under appropriate conditions.
Use of the Compositions for Detection of Urushiol
[0073] A composition prepared according to the present invention may be formulated as an aerosol spray, a topical cream, ointment, medicament, or a solution.
[0074] An aerosol containing approximately 0.005% to about 5.0% (w/w) each of the boron composition and nitroxide according to the present invention is prepared by dissolving the compositions in absolute alcohol. The resulting solution is then diluted in an organic solvent or purified water, depending upon the hydrophobicity of the compound. Routine experimentation by those having skill in the art can be used to determine an effective amount for detecting a catechol in a sample.
[0075] There are several biologically very important catechols: the catecholamines (including epinephrine, norepinephrine, and dopamine), in addition to epicatechin (common in tea). All of these are water-soluble. Because boron species undergo dynamic exchange of alcohol ligands via their anionic “-ate” species in water, it is likely that this methodology may be extrapolated to detect catechols in an aqueous environment. The key reaction sequence of nitroxide reacting with alkylcatecholborane is well established in non-polar organic solvents. Extension to aqueous conditions would provide a very powerful detection method for catecholamines: success would depend on the lifetimes of the tricoordinate borane species compared to the predominate tetracoordinate boronate species. Water-soluble nitroxides and fluorophores are widely known; nitroxides have been used extensively as an EPR probe in biology. The detection of biologically important catecholamines (including epinephrine, norepinephrine, and dopamine) in aqueous environments could lead to powerful new methods in biomedicine.
[0076] Contact dermatitis from exposure of skin to urushiol causes agony and suffering for tens of millions of Americans each year, making this an important human health issue in North America. Urushiol can be effectively removed from skin, clothes and equipment, but only if it is known where this invisible contamination is located. The invention comprises a fluorescence detection method: a spray containing a profluorescent nitroxide and an alkylboronate derivative in an organic solvent will react selectively with urushiol to form a fluorescent N-alkoxyamine. An inexpensive UV light can then be used to pinpoint the presence of urushiol, to prevent or mitigate exposure to skin. Preliminary results with catechol confirm that the key reaction works as expected, and that a highly fluorescent signal is generated. Optimization of the profluorescent nitroxide (both the fluorophore and nitroxide structures), solvent and fine-tuning of the alkyl group on the boronic acid are undertaken. The invention provides a clear benefit to society, including private outdoors enthusiasts, forestry workers, emergency rescue personnel, military personnel, and others who come in contact with poison oak, poison ivy, or sumac.
[0077] The invention also may be used to deactivate a chatechol, such as urushiol, using the methods disclosed herein. In certain case the product, such as B-alkyl catecholboronate or alkycatecholborane, may be chemically unstable and the composition may hydrolyse to the products, chatechol and the alkylboronate derivative, for example. It is contemplated that such hydrolysis may be impeded or decelerated in the presence of environmental modulators, such as a hydrophobic composition, a hydrophilic composition, a buffer composition, or the like. Such environmental modulators can be sugars, carbohydrates, proteins, peptides, glycopeptides, glycolipids, and glycophospholipids; organic compositions, such as organic acids, organic salts, organic bases, or the like, lipids, phospholipids, or fatty acids; chemical stabilizers, or the like, or any combination thereof. Such compositions may be used to formulate a topical medicament or topical composition that is used to reduce or eliminate the effects of poison oak oil-induced contact dermatitis.
[0078] In addition, the formulation or aerosol can comprise a solvent, the solvent comprising a polar organic solvent, a non-polar organic solvent, an aqueous solvent, or a non-aqueous solvent.
[0079] The invention will be more readily understood by reference to the following examples, which are included merely for purposes of illustration of certain aspects and embodiments of the present invention and not as limitations.
EXAMPLES
Example I
Preparation and Testing of Fluororescent Compounds
[0080] We have prepared the known profluorescent nitroxide Dansyl amino-TEMPO 16. As reported, the free nitroxide quenches fluorescence; the insert of FIG. 12 shows the reaction of the nitroxide to form either the hydroxylamine 17 (vial shown) or the n-butylalkoxyamine 18 (not shown) restores the fluorescence to the naked eye upon irradiation with a long wave-length UV lamp at 366 nm (A hand-held UV lamp typically used for viewing thin layer chromatography plates was utilized in these photographs).
[0081] As an initial model, B-n-butylcatecholborane 19 was pre-formed using Dean Stark conditions, and then allowed to react with two equivalents of TEMPO 7 ( FIG. 13 ). The expected N-n-butyloxyamine 20 was formed as a mixture with the hydroxylamine 21, confirming the chemistry developed by Renaud. Hydroxylamine 21 is presumably formed by hydrolysis of the nitroxide boronic ester complex.
[0082] This reaction was repeated with the profluorescent Dansyl amino-TEMPO 16 ( FIG. 14A ). The reaction mixture was strongly fluorescent in which a drop of solution was put on a paper towel; illumination with a thin layer chromatography (TLC) long-wavelength lamp clearly showed a strong fluorescent signal for the alkoxyamine 28 (see FIG. 14B ). Similar drops of solution containing the profluorescent nitroxide 16 and a control mixture of the profluorescent nitroxide mixed with n-butylboronic acid gave no detectible signal. Isolation and characterization of the fluorescent n-butylalkoxyamine 22 confirmed that the reaction had occurred as predicted.
Example II
Fluorescence Detection of Catechol
[0083] In order to form alkylcatecholborane 13 from free catechol under ambient conditions, we initially believed it would be necessary to convert the hydroxyl groups on an alkylboronic acid to better leaving groups. However, early work by Brown indicated that alkylboronic acids react reversibly with catechol in organic, nonpolar solvents to form the desired catecholboranes. It was determined that the reaction sequence shown in FIG. 15A worked: alkylcatecholborane 19 formed from free catechol and an alkylboroinic acid in situ, and reacted with profluorescent nitroxide 16 in one pot to form 22 with a strongly fluorescent signal ( FIG. 15B ). This was an unexpectedly superior result.
[0084] FIG. 26 shows a successful field test of this detection system. The composition was applied onto the surface of poison oak leaves. A paper towel was applied to the surface of the leaves and the paper towel was illuminated using a UV-lamp. As shown in FIG. 26 , the fluorescence was clearly visible to the naked eye.
[0085] It has also been observed that the reaction works well in a variety of polar and nonpolar solvents.
Example III
Synthesis and Development of the Components of the Fluorescence-Generation Method: Optimize the Structure of the Nitroxide, Fluorophore, Tether and Alkylboronic Acid
[0086] The chemical design of the profluorescent nitroxide is explored, entailing the choice of the optimum nitroxide, fluorescent tag, and tether to prepare a robust, soluble and effective component for this detection system. As fluorescence is a very sensitive method of detection, only very small amounts need react to give a signal visible to the naked eye using an inexpensive hand-held fluorescent lamp. The six-membered ring TEMPO is by far the most common nitroxide scaffold, however there are a number of other common stable nitroxide classes. Considerations in optimization of the nitroxide structure include ease and cost of synthesis, versatility in designing and optimizing the tether between the fluorophore and the nitroxide, stability and solubility. Common stable nitroxide classes include TEMPO (tetramethylpiperidinyl-1-oxyl), proxyl (pyrrolidine analogues), nitronyl, imino and doxyl nitroxides ( FIG. 16 ). The inventor and the inventor's research laboratory has been engaged in the synthesis and applications of nitroxides for over a decade, thus has extensive experience in the synthesis of new nitroxides. In addition, a large number of commercially nitroxides are available from Toronto Research Chemicals, Inc. (North York, Canada).
[0087] Recent work by Lozinsky et al. (2004) indicates that profluorescent nitronyl nitroxides quench fluorescence by a different mechanism involving nonbonding electrons of nitrogen and oxygen rather than to the unpaired electron. Thus the fluorescence does not increase upon reduction to the hydroxylamine (and also presumably from the formation of alkoxyamines), making them unsuitable for this study. Given the simple synthetic access ( FIG. 17 ) to proxyl nitroxides following the large body of work pioneered by Hideg, Keana, and many others, proxyl nitroxides 42 are particularly attractive.
[0088] The fluorophore can be easily introduced late in the synthetic sequence, encouraging synthetic diversity without having to start the sequence from the beginning. For an example, a Grignard reagent 43 prepared from 1-bromopyrene gives the proxyl nitroxide 44 with a very short tether between the fluorophore and the nitroxide ( FIG. 18 ).
Example IV
Use of Fluorescence Detection
[0089] With regard to the choice of fluorophore, preliminary data and results focused on Dansyl amino-TEMPO 12, a well-developed profluorescent nitroxide. One advantage of this compound is that sulfonamides are resistant to hydrolysis, thus minimizing the possibility of hydrolysis to give a free fluorophore and thus a false positive signal. Scaiano (Aliaga et al., Organic Lett., 2003, 5(22): 4145-4148) has developed 4-(3-hydroxy-2-methyl-4-quinolinoyloxy)-TEMPO 45, which shows significantly enhanced fluorescence upon reaction of the nitroxide compared to Dansyl amino-TEMPO 12 (but contains a more easily hydrolyzed ester linkage) ( FIG. 19 ). Bottle (Micallef et al., Polymer Degrad. Stabil., 2005, 89(3): 427-435) has developed the profluorescent nitroxide TMDBIO 46, containing a phenanthrene fluorophore covalently fused into the structure of the nitroxide, making hydrolysis an impossibility. Other fluorophores such as pyrene 47 and coumarins have been utilized, and many more are possible. The use of fluorophores observable in the visible range is also explored. The intensity, wavelength dependence, cost, stability and ease of synthesis will all be taken into consideration in selecting the best fluorophore.
[0090] Efficient quenching requires a short tether between the fluorophore and the nitroxide moiety; rotational freedom and flexibility also influence the quenching efficiency. Thus the 5-membered ring nitroxides may provide an advantage in holding the fluorophore in a closer geometry to the nitroxide as compared to the 6-membered ring framework of TEMPO.
Example V
Quenching of Fluorophore
[0091] Dansyl amino TEMPO 12 does show a small amount of residual fluorescence, as shown in FIG. 20 . Other profluorescent nitroxides may be even more effective at quenching the fluorescence in the free nitroxide state. The wavelength of excitation and emission can be tuned by selection of the fluorophore.
Example VI
Effect of Charge Upon Fluororescence Detection
[0092] Since urushiol is very hydrophobic, apolar organic solvents are investigated for the key reaction sequence, including toluene, hexanes, acetone, ethers, etc. The linear hydrophobic “tail” is optimized for both reactivity with catechol and solubility to match that of the hydrophobic urushiol. B-alkylpinacolboranes 24 are conveniently prepared by iridium-catalyzed hydroboration 78 of the corresponding terminal alkenes using commercially available pinacolborane 23 ( FIG. 21 ). Hydrolysis provides easy access to alkylboronic acids with a variety of chain lengths. Commercially available C 12 -C 17 linear terminal olefins are available, with the C 14 and C 16 being particularly inexpensive. Upon testing with actual urushiol, there may be an advantage to having an odd or even number of carbons in the sidechain, or the exact carbon count may prove to be inconsequential. The stability of the boronic acid is also a consideration. Tertiary alkyl boronic acids are prone to decomposition upon exposure with air. In our preliminary studies, we have used primary n-butyl boronic acid. The sample has remained stable for over a year without taking any precautions to avoid exposure to air. We have determined that aryl boronic acids (very stable, and commercially available) do not take part in the radical reaction sequence, presumably due to failure of the fragmentation step due to the instability of aryl radicals. Thus primary alkyl boronic acids seem to be ideal: they react in the desired radical reaction sequence, but are stable to storage.
Example VII
Optimizing the Detection System with Regard to Stoichiometry, Solvent, Concentration, Reaction Time, and Avoidance of False Positives
[0093] Calibration of the fluorescence signal as a function of the concentration of the catechol, boron reagent and nitroxide is carried out. As exposure to 0.001 mg of urushiol can elicit allergic contact dermatitis, very small amounts of urushiol should to be detectable to make this method effective. The optimal stoichiometry to obtain a short reaction time is studied. It is expected that two nitroxides are needed for every boron complex, although one equivalent may be sufficient if the nitroxide catecholboronate complex is hydrolytically unstable. If the fluorescent signal is extremely strong, it may be possible to economize by using a mixture of regular nitroxide mixed with some small percentage of profluorescent nitroxide.
[0094] The specificity of this system for catechols is explored. As controls, phenols, resorcinols (1,3-benenediols), alcohols and diols (for example, sugars) are not expected to participate in the key reaction sequence, as no delocalized perboryl radical intermediate similar to 6 will be formed. Reaction with these various alcohols are tested to ensure that this method is indeed selective for catechols. Pyrogallols (1,2,3-benenetriols, for example gallocatechins (ex. 48) and epigallocatechins ( FIG. 22 ) found in red wine, tea and chocolate) are expected to participate in the reaction, depending upon their solubility in the solvents. Likewise, the closely related catechins (ex. 49) and epicatechins (found in foods along with gallocatechins) are true catechols: reaction are again be limited by solubility.
[0095] Possible sources of false positives are examined. It is well known that nitroxides react rapidly with ascorbic acid to form hydroxylamines. Our research group has used ascorbate reduction of nitroxide to aid in chromatographic separation of alkoxyamine from unreacted nitroxide. Blough was the first to show profluorescent nitroxides react with ascorbic acid to generate a fluorescent signal. Lozinsky has utilized profluorescent nitroxides to assay the amount of vitamin C in fruit juices, and Wang has used a fluorescent conductive charged polymer nitroxide salt as a sensor for ascorbate and for trolox (a vitamin E mimic). Another side reaction that may interfere with the selective detection of urushiol by this boron catechol sequence is the simple reduction of nitroxides by phenols. Scaiano has studied the kinetics of hydrogen transfer from phenol to nitroxide using a profluorescent nitroxide. The rate constants are very slow: k=0.003 M −1 s −1 in protic solvent for gallic acid and BHT, and k=0.2 M −1 s −1 for TROLOX. Scaiano did not investigate reduction by catechol. In preliminary experiments ( FIG. 23 ), we have shown that addition of catechol to Dansyl amino-TEMPO 12 in toluene does produce a weak fluorescent signal, however this is suppressed by addition of a mild oxidant (PbO 2 ) to convert the tiny amount of hydroxylamine to nitroxide. This removes the false positive from phenol ( FIG. 24 ).
[0096] The use of other mild oxidants that will rapidly oxidize hydroxylamine to nitroxide in organic solvents, but not oxidize catechol to quinone, are investigated (See FIG. 25 ). Particularly attractive are Fe (III) salts as less toxic alternatives to lead. We have determined that OXONE is too strong of an oxidizing agent: the nitroxide is oxidized to the oxammonium salt. Interestingly, Bottle has shown that pyrrolidine nitroxides (cyclic 5-membered rings) have higher reduction potentials than piperidine (6-membered ring) nitroxides. Thus use of a pyrrolidine profluorescent nitroxide may inhibit the false positive signal arising from reduction by phenols.
REFERENCES
Addition of Nitroxides to Catecholboranes:
[0000]
Schaffner and Renaud (2004) Eur. J. Org. Chem. 2291-2298.
Darmency and Renaud, (2006) Top. Curr. Chem. 263: 71-106.
Cadot et al., (2002) J. Org. Chem., 67; 7193-7202.
Ollivert et al. (1999) Synlett. 6: 807-809.
Attempted Addition of Nitroxides to Trialkylboranes:
[0000]
Braslau and Anderson, in Radicals in Organic Synthesis , vol. 2 (Eds. P. Renaud, M. P. Sibi), Wiley-VCH, Weinheim, 2001, p. 129.
Addition of Oxygen Radicals to Catecholboranes:
[0000]
Baban et al. (1986) J. Chem. Soc., Perkin Trans 2: 157.
Suzuki et al. (1969) J. Chem. Soc., Chem. Commun 1009.
Brown and Negishi (1971) J. Am. Chem. Soc. 93: 3777.
Forster (1999) PhD Thesis, Universitéde Fribourg, Switzerland, Diss. Nr. 1242.
Ollivier and Renaud (1999) Chem. Eur. J. 5: 1468.
Kumli et al. (2006) Organic Lett. 8(25): 5861-5864.
Ollivier and Renaud (2000) Angew. Chem. Int. Ed. Eng. 39: 925.
Profluorescent Nitroxides:
[0000]
Blough (1988) J. Am. Chem. Soc. 110: 1915.
Blough (1990) Free Rad. Res. Comm 10: 119-121.
Blough (1996) Anal. Chem. 68: 867-872.
Micallef A S et al. (2005) Polym Degrad. & Stability 89: 427-435.
Foitzik et al. (2008) Macromolecules 41: 1577-1580.
Blinco et al. E. J. Org. Chem. 28: 4638-4641.
Sciano (2001) Macromol. 34: 6184.
Coenjarts et al. (2003) J. Am. Chem. Soc 125: 620-621.
Ivan et al. (2003) Photochem. Photobiol. 78: 416.
Aspee et al. (2007) Photochem. Photobiol. 83(3): 481-485.
Maurel et al. (2006) J. Phys. Chem. B, 110(33): 16353-16358.
Laferriere et al. (2006) Chem. Comm (3): 257-259.
Aspee et al. (2003) Photochem. Photobiol. Sci. 2(11): 1125-1129.
Aspee et al. (2003) Macromolecules, 36(10): 3550-3556.
Korth (2000) Biol. Chem. 381(7): 575-582; ibid (1999) Chem. Eur. J. 5(6): 1738-1747;
ibid (1997) Angew. Chem. Int. Ed. Eng. 36: 1501-1503; ibid (2006) Hely. Chim Acta 89: 2281-2296.
Zhang and Zhu (2004) Chem. Commun 670.
Hideg (2006) Photochem. Photobiol. 82: 1211.
Wang (2006) Chem. Mater. 18: 3605-3610.
Dang and Guo (2006) Appl. Spectrosc. 60: 203-207.
Likhtenstein et al. (2007) Photochem. Photobiol. 83: 871-881.
Lozinsky, et al. (2004) Anal. Biochem. 326: 139-145.
Likhtenstein (2002) Biochem. Biophys. Meth. 51: 1-15.
Likhtenstein (1990) Analyst 115: 839.
Likhtenstein (1999) Biochem. Biophys. Meth. 38: 29-42.
[0134] Those skilled in the art will appreciate that various adaptations and modifications of the just-described embodiments can be configured without departing from the scope and spirit of the invention. Other suitable techniques and methods known in the art can be applied in numerous specific modalities by one skilled in the art and in light of the description of the present invention described herein. Therefore, it is to be understood that the invention can be practiced other than as specifically described herein. The above description is intended to be illustrative, and not restrictive. Many other embodiments will be apparent to those of skill in the art upon reviewing the above description. The scope of the invention should, therefore, be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
|
The invention herein disclosed provides for compositions, methods for synthesizing said compositions, and methods for using said compositions, wherein the compositions and methods may be used to bind to and/or deactivate a poison oak oil, such as urushiol. The compositions and methods can be used to treat and/or reduce an inflammatory reaction and/or hypersensitivity to natural compounds found in poison oak, poison ivy, poison sumac, mango, lac tree, and cashew nut.
| 0
|
RELATED APPLICATIONS
[0001] This application claims the benefit under 35 U.S.C § 120 of prior co-pending U.S. patent application Ser. No. 10/377,642, Self-Healing Coating and Microcapsules to Make Same, by Sarangapani et al., filed Mar. 4, 2003, and incorporated herein by reference.
STATEMENT OF GOVERNMENT INTEREST
[0002] Under paragraph 1(a) of Executive Order 10096, the conditions under which this invention was made entitle the Government of the United States, as represented by the Secretary of the Army, to the entire right, title and interest therein of any patent granted thereon by the United States. This patent and related ones are available for licensing. Contact Bea Shahin at 217 373-7234 or Phillip Stewart at 601 634-4113.
FIELD OF THE INVENTION
[0003] The present invention relates generally to coatings, in particular coatings that have been modified to provide a self-healing characteristic.
BACKGROUND
[0004] Much effort and resources are expended in ongoing corrosion control, even when an item has been coated initially to protect it. Abrasion, saltwater, high humidity, ultraviolet light, temperature gradients, and other deleterious environmental factors contribute to this, alone or in combination. To conserve corrosion control resources, it would be beneficial to use not only a “tough” initial protective coating, but also a coating that, when compromised, “heals” itself.
[0005] There have been efforts to effect a self-repairing capability in various materials, notably shaped articles that may be made of materials with a weakness in one or more orientations, such as cementitious materials having inherently poor tensile strength. U.S. Pat. No. 5,575,841, Cementitious Materials, to Dry, Nov. 19, 1996, and U.S. Pat. Nos. 5,660,624 (Aug. 26, 1997), 5,989,334 (Nov. 23, 1999), and 6,261,360 B1 (Jul. 17, 2001), each entitled Self-Repairing Reinforced Matrix Materials, all to Dry, detail a method of incorporating hollow fibers in “pourable” material to effect a self-repairing function. These inventions employ selectively releasable compounds within the hollow fiber. Because of the size of the fibers, these patents are unsuitable for repair upon a smooth surface.
[0006] Microcapsules contain minute amounts of product for specialized delivery, often size, time or location critical. They may be obtained in diameters of less than 250 microns (μ) and have been used in a variety of applications, from the pharmaceutical industry (delivery of drugs) to the textile industry (providing protective wear for HAZMAT workers). One example is U.S. Pat. No. 6,060,152, Fabric with Microencapsulated Breach Indication Coating, to Murchie, May 9, 2000. The '152 patent describes a membrane incorporating a number of different microcapsules that alert to even the smallest compromise of the fabric comprising a protective suit such as may be worn by a HAZMAT worker or health professional.
[0007] Very recent work to improve coatings by the addition of additives involves only improving the application of the coating to a substrate, not the ability of the coating to “repair” itself upon its compromise. One such example is U.S. Pat. No. 6,746,522 B2, High Molecular Weight Polymer Additive for Coating and Protective Products, to Trippe et al., Jun. 8, 2004. The '522 patent details the advantages of adding small amounts of an ultrahigh molecular weight polymer, such as polyisobutylene, to enhance coating properties of a solvent. Once, a nick compromises the coating or abrasion, however, another separately applied application is required to protect the substrate.
[0008] Another concern in using microcapsules with solvents is the timing of delivery of the encapsulated compound. Prior patents have avoided this timing problem by mixing the microcapsules with dry powder coatings such as are used in “powder coating” applications involving elevated temperatures. U.S. Pat. No. 6,075,072, Latent Coating for Metal Surface Repair, to Guilbert et al., Jun. 13, 2000, details a self-repairing compound suitable for use in powder coating. By adding microcapsules of sufficiently small size, i.e., 10-40μ, to a dry powder form of protective coating, the resultant “self-repairing” coating is able to be powder coated upon metal substrates at suitable elevated temperatures that melt the coating to a homogenous continuous surface of approximately 200μ thickness. The microcapsules used with the '072 patent are mixed in the dry state to prevent short-term degradation of the shells by liquid solvents.
[0009] Unless appropriate materials are used to fabricate the microcapsule and its contents, it may “deploy” before the coating is applied or, upon application, spontaneously deploy improperly, i.e., without a physical compromise of the coating such as abrasion or nicking. Further, unless the microcapsule is compatible with both its contents (the encapsulated repair compound) and its surrounds (the solvent), the “application” life of the resultant mixed product may be less than desirable. These constraints have been addressed in the present invention.
SUMMARY
[0010] In a preferred embodiment of the present invention, urea formaldehyde microcapsules, approximately 60-150 microns (μ) in diameter and containing corrosion inhibitors and several types of film forming compounds, or “healants,” are mixed with commercially available coatings. When the applied modified coating is damaged, e.g., by abrasion through the coating to the substrate on which it is applied, the microcapsules burst, releasing the film forming and corrosion inhibiting compounds. This initiates a self-healing process, i.e., the damaged area of the substrate is covered and repaired, inhibiting corrosion. Steel substrates coated with these modified coatings, or “self-healing systems,” were scribed and laboratory tested according to ASTM D 5894, i.e., alternately exposing them to salt spray and ultraviolet (UV) light. ASTM D-5894, Standard Practice for Cyclic Salt Fog/UV Exposure of Painted Metal , ( Alternating Exposures in a Fog/Dry Cabinet and a UV Condensation Cabinet ), American Society for Testing Materials, West Conshohocken, Pa. The coated test specimens were evaluated with respect to undercutting at the scribe in accordance with ASTM D 1654. ASTM D 1654, Standard Practice for Cyclic Salt Fog/UV Exposure of Painted Metal , ( Alternating Exposures in a Fog/Dry Cabinet and a UV Condensation Cabinet ), American Society for Testing Materials, West Conshohocken, Pa. The undercutting was reduced from 2.12 mm to 0.46 mm at the scribe when employing microcapsules containing phenolic varnish, a long chain polyester diluent, a second carrier/diluent based on high molecular weight hydrocarbons and a corrosion inhibitor. Electrochemical impedance spectroscopy (EIS) tests showed that the incorporation of self-healing microcapsules resulted in significantly higher impedances for damaged “microcapsule coatings” than for the same coatings containing no microcapsules.
[0011] Thus, in general, a self-healing coating is provided that, after application and curing upon a substrate, self heals upon its physical compromise. It comprises one or more solvents, one or more solids and microcapsules containing a repair material that may comprise one or more substances. The shell of the microcapsule is resistant to degradation from within by the repair substances. Prior to application of the self-healing coating and after addition of the microcapsules to a solvent/solid mixture, the microcapsules are resistant to short term degradation of the exterior shell by either the solvents or the solids. The microcapsules burst upon physical compromise of the resultant applied and cured coating, releasing the repair substances to seal a volume (void) within the coating cause by the physical compromise. Spherical microcapsules produce a most efficient delivery volume and are preferred. However, other shapes, such as filaments, may be used also, with a concomitant loss of efficiency. In addition to traditional paints, the microcapsules may be used with or deliver greases, lubricants, varnishes, lacquers, shellacs, polyurethanes, waxes, polishes, fabric treatments, waterproofing compounds, liquid roofing coatings, oils, and similar compounds.
[0012] The combination of one or more solvents and one or more solids may comprise a protective coating that would serve the purpose of protecting a substrate but not have the self-healing properties of the present invention. This protective coating may be one of a number of commercially available products, to include primer paints, topcoat paints, “one coat” or “self-priming” paints, varnishes, lacquers, polyurethane finishes, shellacs, waxes, polishes, “one step” finishing preparations for wood, metal, or synthetic materials, and combinations thereof. The paint primers may be: polyurethanes, oil-based enamels, enamel undercoater, latex acrylics, acrylic formulations and epoxy formulations. Further, topcoat and self-priming paints may be: polyurethanes, oil-based enamels, enamels, latex acrylics, acrylic formulations and epoxy formulations.
[0013] Any of the coatings may serve as a corrosion inhibitor through the addition of suitable corrosion inhibitors or the coatings may be merely decorative.
[0014] The shell of the microcapsule may be a sphere with an outer diameter preferably within the approximate range of 50 to 200μ. More preferably, the shell may be a sphere with an outer diameter greater than approximately 63μ. Most preferably, the shell is a sphere with an outer diameter of approximately 150μ.
[0015] The shell of the microcapsule may comprise either gelatin or, more preferably, urea formaldehyde (UF).
[0016] The repair substances may be a combination of film-forming compounds and corrosion inhibiting compounds. The film-forming compounds may be any of: polybutenes, phenolics, phenolic varnishes, long chain polyester diluents, carrier diluents, and combinations thereof. The corrosion inhibiting compounds may be any of: camphor, alkylammonium salt in xylene, Ciba IRGACOR® 153 (hereafter also anti-corrosion agent A), polyamine fatty acid in salt in ethanol, Ciba IRGACOR® 287 (hereafter also anti-corrosion agent B), and combinations thereof.
[0017] The microcapsules are added prior to application as a pre-specified percentage of the dry weight of the solids in the base coating at a pre-specified time prior to application of the self-healing coating. Preferably, the pre-specified percentage lies in the approximate range of 10 to 40% and the microcapsules are added within fourteen (14) days of application. Most preferably, the pre-specified percentage is approximately 25% and the microcapsules are added when preparing the coating for application.
[0018] Also provided is the microcapsule suitable for adding to available protective coatings to facilitate self-healing thereof after application and curing. In general, this microcapsule comprises a repair substance and a shell enclosing a volume containing the repair substance. Upon application of the protective coating to a substrate and curing of the coating thereon, physical damage to the resultant coating ruptures the shell of the microcapsules in the vicinity of the rupture and deploys the repair substance into a volume (void) within the coating caused by the physical damage.
[0019] The shell of the microcapsule may be a sphere with an outer diameter preferably within the approximate range of 50 to 200μ. More preferably, the shell has an outer diameter greater than approximately 63μ. Most preferably, the shell has an outer diameter of approximately 150μ.
[0020] The shell of the microcapsule may be gelatin, or preferably urea formaldehyde (UF). The repair substance contained therein may comprise film-forming compounds and corrosion inhibiting compounds.
[0021] The film-forming compounds may be any of: polybutenes, phenolics, phenolic varnishes, and combinations thereof. The diluents may be any of: long chain polyester diluents, carrier diluents, and combinations thereof. The corrosion inhibiting compounds may be any of: camphor; alkylammonium salt in xylene, commercially available as Ciba IRGACOR® 153 (anti-corrosion agent A); polyamine fatty acid in salt in ethanol, commercially available as Ciba IRGACOR® 287 (anti-corrosion agent B); and combinations thereof.
[0022] Also provided is a method for making a self-healing coating. It comprises: (a) providing a non-self healing coating; (b) providing microcapsules filled with a repair substance compatible with the non-self healing coating; and (c) mixing the microcapsules into the non-self healing coating such that the microcapsules are fully wetted and interspersed evenly throughout the non-self healing coating.
[0023] Further provided is a method for producing a self-healing coating upon a substrate. It comprises: (a) providing a non-self healing coating; (b) providing microcapsules filled with a repair substance compatible with the non-self healing coating; (c) mixing the microcapsules into the non-self healing coating such that the microcapsules are fully wetted and interspersed evenly throughout the non-self healing coating; (d) applying the self-healing coating to the substrate by any of a number of means selected from the group consisting of: brushing, rolling, spraying, and combinations thereof; and (e) permitting the applied self-healing coating to cure prior to use of the substrate.
[0024] Advantages of preferred embodiments of the present invention include:
[0025] reduced need for maintenance and renewal of applied protective coatings;
[0026] reduced maintenance costs;
[0027] increased intervals between required inspections;
[0028] reduced life cycle costs;
[0029] improved appearance of the substrate over its design life;
[0030] increased service life of an item protected with the self-healing coating; and
[0031] increased mean time between failure (MTBF).
[0032] Further advantages of the present invention will be apparent from the description below with reference to the accompanying drawings, in which like numbers indicate like elements.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] FIG. 1A is a micrograph typical of small gelatin microcapsules (<63μ diameter) as collapsed when immersed in wet polyurethane when investigated for possible use in the present invention.
[0034] FIG. 1B is a micrograph typical of medium gelatin microcapsules (63-150μ diameter) after two (2) hours immersion in wet polyurethane when investigated for possible use in the present invention.
[0035] FIG. 2A is a micrograph typical of large urea-formaldehyde (UF) microcapsules (>150μ diameter) after two (2) weeks immersion in wet polyurethane when investigated for possible use in the present invention.
[0036] FIG. 2B is a micrograph typical of large urea-formaldehyde (UF) microcapsules (>150μ diameter) deteriorating after four (4) weeks immersion in wet polyurethane when investigated for possible use in the present invention.
[0037] FIG. 3 depicts a suggested mechanism for the collapse of microcapsules in wet coatings.
[0038] FIG. 4A is a micrograph showing the effect of burst UF microcapsules incorporated in applied coatings of the present invention in which a crack is induced in the coating.
[0039] FIG. 4B is a micrograph showing the effect of burst UF microcapsules incorporated in applied coatings of the present invention in which the coating has been scribed.
[0040] FIG. 5A depicts a cross section through a cube containing a single large microcapsule that may be used in a preferred embodiment of the present invention.
[0041] FIG. 5B depicts a cross section through the cube of FIG. 5A with a superimposed symmetric array of nine small microcapsules that fit in the same cube containing the large microcapsule of FIG. 5A .
[0042] FIG. 6 details the test results for the control and the three (3) self-healing coatings that may be employed as preferred embodiments of the present invention.
[0043] FIG. 7 depicts the relationship between impedance and frequency for both a control sample and a preferred embodiment of the present invention using data taken with Electrochemical Impedance Spectroscopy (EIS).
[0044] FIG. 8 depicts the relationship between phase angle and frequency for both a control sample and a preferred embodiment of the present invention using data taken with EIS.
DETAILED DESCRIPTION
[0045] A preferred embodiment of the present invention provides a “self-healing” coating system that may be used for corrosion protection, such as on outdoor steel cabinet enclosures for electrical equipment. Microcapsules in the form of microscopic spheres with a diameter of 50-200μ, and more preferably of 60-150μ diameter, are used to encapsulate “coating repairing” compounds as a means of effecting self-healing of the applied coating thus derived. These microcapsules are fabricated for optimum dispersal into various coating formulations, e.g., paint, enabling release of the coating repairing or “self-healing” compounds. These compounds may comprise, at least in part, corrosion-inhibiting constituents. Thus, when the applied coating is mechanically ruptured such as may occur upon damage by impact or abrasion, these compounds are “deployed.” Corrosion-inhibiting microcapsules may be used in coating systems to minimize damage caused by scratches or abrasions by releasing specially formulated chemicals that flow into the damaged areas forming thin films of corrosion protection.
[0046] For paint systems, self-healing coatings are fabricated by adding microcapsules containing at least one “self-healing” compound to commercially available paint primers. Paint primers may include those paints commercially termed “one coat” or “self-priming.” The microcapsules release the self-healing compound or compounds, most commonly as liquids, when the coating system is damaged. Urea formaldehyde (UF) microcapsules of 50-150μ in diameter have been added to primers with an applied thickness of 0.1 mm (0.004″) to increase the coating service life by “self-healing” damaged areas. Verification of performance was conducted by accelerated corrosion testing on conventional coating systems using ASTM D 5894 and Electrochemical Impedance Spectroscopy (EIS). M. Kendig and J. Scully, Basic Aspects of Electrochemical Impedance Applications for the Life Prediction of Organic Coatings on Metals, Corrosion , Vol. 46, No. 1, pp. 22-29, 1990. H. Hack and J. Scully, Defect Area Determination of Organic Coated Steels in Seawater Using the Breakpoint Frequency Method, J. Electrochem. Soc ., Vol. 138, No. 1, pp. 33-40, 1991.
[0047] One of the primary concerns in using microcapsules in coatings that contain solvents is the maintenance of structural integrity of the microcapsule until application of the coating and evaporation of the solvent or solvents. A laboratory study was undertaken to determine the stability of both urea formaldehyde (UF) and gelatin as shell materials as well as the propensity of the microcapsules to release the “self-healing” compounds only when the applied coating is physically damaged. The gelatin and UF capsules are filled with red dye as a tracer to facilitate evaluation.
[0048] Achieving timely and appropriate rupturing of microcapsules to be incorporated in applied coatings is crucial to developing and commercializing “self-healing” coatings. “Timely and appropriate rupturing” occurs, for example, when the applied coating is damaged physically or if cracks develop in the applied coating. Microcapsules may exhibit at least two major “improper rupturing” modes; viz., rupturing before the coating is applied to a surface and spontaneous rupturing on the surface of applied coatings prior to cracking or physical damage.
[0049] To determine the stability of the microcapsules in various coating formulations, samples of each are bottled. Samples are extracted from each bottle and placed on glass slides. Initial optical micrographs of each are taken. After initial sampling, each bottle is tightly sealed. Optical micrographs of each sample are taken weekly over a period of four (4) weeks, and deterioration (if any) as a function of time is noted. A listing of the types and quantities of tested microcapsules, designated as: small (<63μ), medium (63-150μ), and large (>150μ), is shown in Table 1.
[0000]
TABLE 1
Wet Coatings Investigated for Stability of Microcapsules
SIZE OF
SAMPLE
TYPE OF PAINT AND
CAPSULES AND
NUMBER
AMOUNT (grams)
AMOUNT (grams)
1
Polyurethane
35
Medium
0.6
2
Polyurethane
100
Medium
0.3
3
Polyurethane
100
Large
0.6
4
Polyurethane
100
Small
0.6
5
Oil-based enamel (flat white)
100
Medium
0.6
6
Acrylic primer (latex)
100
Medium
0.6
7
Interior enamel (latex acrylic)
100
Medium
0.6
8
Enamel under coater
100
Medium
0.6
9
Acrylic primer (latex)
50
Small
0.6
[0050] Refer to the micrographs of FIG. 1 . Small gelatin microcapsules 101 (diameters less than 63μ) failed to maintain structural integrity and self ruptured in polyurethane and other coatings in a few days. A micrograph typical of collapsed small gelatin microcapsules 101 is shown in FIG. 1A . As depicted in FIG. 1B after two hours immersion in polyurethane, medium (63-150μ) gelatin microcapsules 102 maintain integrity somewhat longer than a few days. As shown in the micrograph of FIG. 2A , large UF microcapsules 201 (diameter greater than 150μ) maintained integrity for at least two (2) weeks. However, as shown in the micrograph of FIG. 2B , even the large UF microcapsules 201 began to collapse 202 and lose core material after four (4) weeks immersion in wet polyurethane.
[0051] A suggested mechanism for the collapse of microcapsules immersed in wet coatings is illustrated in FIG. 3 . Upon initial introduction of microcapsules to the wet coating as shown at A, the pressure inside the microcapsule 201 from the compound or compounds contained therein counteracts the pressure from the wet coating (not shown separately) surrounding the microcapsule, thus maintaining microcapsule structural integrity. Diffusion of core material as at B (from inside the microcapsule 201 through its shell to the outside) creates empty space 301 in the cavity of the microcapsule 201 , disrupting the pressure balance aforementioned. After substantial compound (core material) diffuses from a microcapsule 201 , as at C the microcapsule collapses 202 inward.
[0052] Small gelatin microcapsules 101 are not appropriate for wet coatings if immersed therein more than two (2) weeks. The reason for this poor stability may be due to attack of the gelatin by the solvents either internal to the shell, i.e., the core material, external to the shell, i.e., the wet coating, or both. Further, even UF microcapsules 201 immersed in wet coatings have, a relatively short shelf life, thus, in a preferred embodiment of the present invention, microcapsules 201 should be mixed into the wet coating at the time of application.
[0053] For best results, UF microcapsules 201 greater than about 63μ in diameter should be employed for the containment and delivery of the self-healing compounds (core material). Larger microcapsules 201 contain and deliver more core material once ruptured than the smaller microcapsules 101 . Also, there is a higher probability of rupturing a small number of large microcapsules 201 than rupturing a large number of small microcapsules 101 to deliver the same volume of core material.
[0054] Refer to FIG. 5 . Consider, for example, a simple cube 500 , 520 of dimension, d, on a side with a distribution of one or more microcapsules therein. The volume of a sphere is 4/3 πr 3 , where r=d/2. Thus, volume in terms of d is 4/3π(d/2) 3 or ⅙πd 3 . If as shown by comparing the microcapsules (spheres) in FIG. 5A to those in FIG. 5B , the volume of the spheres of FIG. 5B , i.e., ⅓ the diameter of the large sphere of FIG. 5A , is given by ⅙π(d/3) 3 or ⅙πd 3 /27. Thus, assuming “perfect packing” of 27 small spheres of diameter d/3 in the same cube of dimension d, the same amount of core material is available within the cube. “Perfect packing” of the cube may be impossible to achieve but does serve to illustrate the point theoretically. As an example, for a large single microcapsule 501 just fitting the cube 510 of dimension d, its diameter d may be 150μ. A perpendicular cutting plane of 150×150μ will completely sever this single large microcapsule 501 , delivering a volume of 1.8×10 6 μ 3 . As depicted only in cross section 520 in FIG. 5B , the equivalent volume of the same cube 510 may be filled by 27 smaller microcapsules 521 , each of diameter, d s =50μ, where d s =d/3. However, a perpendicular cutting plane of the same area (150×150μ) as used in FIG. 5A will completely sever only nine (9) of the small microcapsules 521 . This yields a combined volume of 0.6×10 6 μ 3 of core material, only ⅓ of the single large microcapsule 501 of FIG. 5A . Thus, even under the assumption of optimal packing for the small microcapsules 521 , the larger microcapsules 501 will deliver microcapsule contents over an optimum area of compromise, thus assuring the opportunity of assuring a better seal along the perimeter of the compromise. Microcapsules much greater than 150 microns in diameter are too large for many coating applications, as conventional paint films (primers+topcoats) are only eight (8) mils (200μ) in thickness for both coats. Thus, microcapsules of 63-150 microns are recommended for typical applications of these types of coatings.
[0055] Microcapsules incorporated in coatings to be applied to steel substrates for corrosion testing preferably have core compositions with corrosion inhibiting “healants,” such as film-forming compounds containing polybutene or phenolics, and one or more pre-specified corrosion inhibiting compounds. As well, core material contains certain diluents that facilitate flow of the film-forming compounds upon rupture of the microcapsule. Primers and topcoats may be chosen from among acrylics and epoxy formulations. In all cases, the primers and topcoats and the core materials must be selected to not degrade the preferred UF shell material used in formulating the microcapsule.
[0056] Coatings used in testing preferred embodiments of the present invention include a paint primer, Dexter 1 OPW20-4 Water Reducible Epoxy Primer, Dexter-Hysol Company, and a paint topcoat, Sherwin-Williams Dura-Pox Water-based Epoxy Finish, Sherwin-Williams Paint Company. Samples were applied to steel panels (not shown separately except for partial representation in the micrographs of FIGS. 1 , 2 and 4 ) obtained from Q-Panel Laboratory Products, Cleveland, Ohio 44145. They are described as Type R39 and conform to ASTM Specification A366, D609-Type 1. The panels are 3″×9″×0.032″.
[0057] Microcapsules are added to the mixed primer at 25% weight based upon the dry solids contained in the primer. Microcapsules are added directly to the primer in small portions with slow mixing until all of the microcapsules appear to be wetted. The primer and topcoat are applied using a drawdown bar. The samples are dried for one to two days after the primer is applied and for two (2) weeks after the topcoat is applied.
[0058] Microcapsules selected for evaluation are UF shells of 63-150 micron diameter with core materials selected from the following candidates: phenolic varnish; a long chain polyester diluent; Iso decyl diphenyl phosphate, commercially available as SANTICIZÈR® 148, Solutia, Inc., St. Louis, Mo.; a second carrier/diluent, modified partially hydrogenated terphenol, commercially available as THERMINOL® 66, Solutia, Inc., St. Louis, Mo.; and either camphor or a corrosion inhibitor in either of two forms as alkylammonium salt in xylene, commercially available as Ciba IRGACOR® 153 or polyamine fatty acid in salt in ethanol, commercially available as Ciba IRGACOR® 287, Ciba Geigy Company. The only difference in the three microcapsule core materials that were tested is in the addition of one extra component in each. The extra component in the microcapsules designated “A” is “anti-corrosion agent A”; that designated “C” is “anti-corrosion agent B” and that designated “D” is camphor.
[0059] Four (4) sets of samples of three (3) panels each are tested. The edges and backs of all coated steel panel samples are sealed using a coal tar epoxy composition. The first set is the control, having no microcapsules in the coating. Three sets are formulated similarly to the control except for incorporating microcapsules in the primer at 25% of dry weight of solids in the primer. After allowing the samples to cure fully, two scribe marks are made on each sample panel per ASTM D 1654.
[0060] Accelerated corrosion testing for 2016 hours is accomplished under ASTM D 5894. ASTM D5894 testing combines the environmental effects of salt spray and UV light, simulating exposure to field conditions. In addition, electrochemical impedance spectroscopy (EIS) evaluations were performed on some samples subsequent to the ASTM D 5894 tests in order to determine the relative degree of coating degradation at the scribed area.
[0061] Representative self-healing “deployments” are shown in FIG. 4 . FIG. 4A depicts the rupture pattern 401 of UF microcapsules upon inducing a crack in the applied coating while FIG. 4B depicts the rupture “line” 402 of UF microcapsules upon scribing the applied coating.
[0062] Results for the “control” and the three (3) self-healing coatings, as formulated with microcapsules of three different compositions, are shown in FIG. 6 . The amount of undercutting for each panel is determined by taking the mean maximum of the coating loss extending between the top and bottom of each of two scribe marks, according to the procedure recommended by ASTM D 1654. These results are shown as a plot of mean undercutting (in mm) for all microcapsules in each sample set by microcapsule type for the four sample types (three microcapsule formulations A, C, D and a control or None). This clearly shows that addition of microcapsules with “self-healing” compounds and corrosion inhibitors significantly reduces undercutting at the scribe, compared to the control coatings containing no microcapsules. For example, the undercutting was reduced from a mean value of 2.12 mm for the control to a mean value of 0.39 mm for the coatings containing the “C” microcapsules.
[0063] Further, differences were noted among the undercutting results for the three separate microcapsule formulations. The coatings with the “C” microcapsules (mean undercutting of 0.39 mm) that contained Anti-Corrosion Agent “B”, performed only slightly better than the “D” microcapsules, containing the camphor (mean undercutting of 0.46 mm). However, coatings with either the “C” or “D” microcapsules performed significantly better than coatings with the “A” microcapsules, containing Anti-Corrosion Agent “A” (mean undercutting of 0.75 mm). Undercutting measurements taken in this way provide a measure of the relative ability of the coating system to adhere at the scribe where corrosion is taking place, and to resist underfilm corrosion.
[0064] Performance of epoxy-based primers is enhanced by the addition of appropriately fabricated microcapsules. Burst microcapsules counteract the effects of ultraviolet light and salt spray exposure, releasing “healing compounds” when damaged, e.g., by scribing. The core material in the microcapsules fulfilled expectations. The phenolic varnish acted as a film-former to seal the edges of the damaged coating. The diluents functioned as a low viscosity carrier/diluent for the other components. The camphor, and the two anti-corrosion agents, A and B, functioned as viable corrosion control agents to provide additional corrosion protection over at least part of the scribed region.
[0065] Refer to FIGS. 7 and 8 . Electrochemical impedance spectroscopy (EIS) is performed on the scribed area of one of the coating system samples containing the “C” microcapsules in the coating, and on the scribed area of one of the control samples after both were subjected to the ASTM D 5894 test. The EIS results are presented in FIG. 7 as Log Impedance Modulus (Ω) vs. Log Frequency (Hz), and in FIG. 8 , as Phase Angle (deg) vs. Log Frequency (Hz), respectively. Over a frequency range of 100 KHz to 0.1 Hz, the impedance moduli of the scribed areas of either the control coating or the “C” microcapsule coating did not change significantly. Note however, that the impedance modulus of the scribed area of the sample containing the “C” microcapsules is about 16 times greater than the impedance modulus of the scribed area of the coating with no microcapsules. This is an objective indicator of the “C” microcapsules having sealed the substrate, preventing further growth of the scribed area. The phase angles for both coatings display slightly negative values, with a suggestion of less on-going corrosion of the “C” microcapsule sample. The phase angles for coatings with the “C” microcapsules display a slightly more capacitive behavior, as would be expected for an uncompromised coating. Thus, the EIS results are consistent with the undercutting measurements previously described.
[0066] While the invention has been described in terms of its preferred embodiments, those skilled in the art will recognize that the invention may be practiced with modifications within the spirit and scope of the appended claims. For example, although the system is described in specific examples for paints, it is amenable for use with other coatings that one desires to prolong in an uncompromised state or to retain an original capacity for protection, regardless of outward appearance. These coatings may include merely decorative coatings as well as the aforementioned corrosion inhibiting coatings. Thus, it is intended that all matter contained in the foregoing description or shown in the accompanying drawings shall be interpreted as illustrative rather than limiting, and the invention should be defined only in accordance with the following claims and their equivalents.
|
A self-healing coating, incorporating medium-sized microcapsules filled with a liquid formulation, repairs itself upon physical compromise. In one embodiment, a commercial primer is mixed with these microcapsules and applied. After the coating has cured, any physical compromise of the cured coating results in the microcapsules bursting to release the liquid, in turn filling and sealing the compromised volume of the coating. In applications where a product is used to provide corrosion protection, the liquid contains anti-corrosion material as well as suitable diluents and film-forming compounds. In a preferred embodiment, the microcapsules are provided separately to be mixed with commercial products during preparation for application of the coating. For example, if a paint formulation is known a priori, tailored microcapsules packaged separately from the paint and designed for use with the paint formulation, are wet mixed into the paint during preparation for application.
| 2
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of Australian Provisional application no. 2013904861 filed on Dec. 13, 2013, the entire document of which is incorporated herein by reference.
TECHNICAL FIELD
[0002] The present invention relates to a network based referral system and method for recruitment.
BACKGROUND
[0003] Previously, there have been several well-known online recruitment systems for matching job seekers or candidates with employment or recruitment opportunities. For example, the websites such as: www.seek.com.au; www.monster.com; and www.naukri.com. These example websites typically allow candidates to upload their resumes and apply for jobs or employment using an online portal system.
[0004] However, these earlier systems generally fail to reward people who refer job opportunities onto appropriately qualified job seekers. Additionally, there is no incentive to refer job opportunities to other people who may be interested in the particular job opportunity.
[0005] Further, there have also been several inventions aimed at improving referral networks associated with online job portals. An example is PCT Published Applications No. WO2008019711 and WO2011140259, which describe network based referral systems for recruitment. However, in these disclosed systems, the candidate's profile and resume are in effect automatically garnered from social media websites (such as Facebook™). The disclosed systems then automatically refer people based on linkages from the social media sites and generally fail to compensate the referring party. Further, these systems rely on third party websites to generate contact lists and this type of system may be refer the best possible candidate for each job opportunity.
[0006] Many previous systems aim to improve the profiling of candidates but ignore the possible advantages of developing a referral tree or a network of referral contacts. For example, PCT Published Application No. WO1999017242, discloses an improved profiling system for job seeking and job matching websites but the disclosed systems generally fail to make efforts to improve the referral system to increase the number of appropriately skilled people viewing the job opportunity.
[0007] Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of common general knowledge in the field.
SUMMARY
Problems to be Solved
[0008] It is an aim and objective of the present invention to provide an improved network based referral system and method suitable for use in relation to the field of employment and recruitment, wherein users of the system or method may be able to refer other users to the system or method.
[0009] It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art, or to provide a useful alternative.
Means for Solving the Problem
[0010] A first aspect of the present invention may relate to a network based referral system for recruitment, comprising: a job profile corresponding to inputs by a first user of said system; an applicant description module which includes data from an applicant description profile corresponding to characteristics of an second user and an applicant referred to the system by the second user; and a database for storing a plurality of said job profiles and for receiving said applicant description profile over said network and for matching characteristics of said applicant description profile with corresponding characteristics of said job.
[0011] Preferably, the system is adapted to allow the second user to invite an applicant to be linked to the application description profile. The preferred system may be adapted to accept job applications from either second user or applicant.
[0012] The characteristics may include: contact details, a skills list, an expertise list, and a testing result profile; and the testing result profile may be derived from results of a standardised testing procedure relevant to a skillset as undertaken by the respective second user or applicant.
[0013] Preferably, the application description profile includes a referral tree that includes data on a plurality of applicants known to the second user and referred to the system by the second user.
[0014] The system may also include an authentication procedure to verify the relationship between the second user and applicant. Preferably, the applicant is a third party and not the second user.
[0015] The system may provide consideration to a second user wherein an applicant linked to the application description profile is employed by the first user. The preferred consideration payable to a second user is in the form selected from the following group: points, credits, currency or remuneration prizes.
[0016] The system may be adapted to allow the applicant to invite a second tier applicant to be linked to the application description profile, and further the system may be adapted to accept job applications from the second tier applicant. The preferred application description profile may also include a referral tree that includes data on a plurality of second tier applicants known to at least one applicant or the second user and referred to the system by the at least one applicant or the second user.
[0017] The preferred system may provide consideration to a second user and the applicant wherein the second tier applicant linked to the application description profile is employed by the first user. Further, the system may provide consideration to a second user and the applicant at a differentiation rate.
[0018] Preferably, the system may be adapted to allow the second tier applicant to invite a third tier applicant to be linked to the application description profile.
[0019] In the context of the present invention, the words “comprise”, “comprising” and the like are to be construed in their inclusive, as opposed to their exclusive, sense, that is in the sense of “including, but not limited to”.
[0020] The invention is to be interpreted with reference to the at least one of the technical problems described or affiliated with the background art. The present aims to solve or ameliorate at least one of the technical problems and this may result in one or more advantageous effects as defined by this specification and described in detail with reference to the preferred embodiments of the present invention.
BRIEF DESCRIPTION OF THE FIGURES
[0021] FIG. 1 depicts schematically part of a first embodiment of the present invention and demonstrates example components of a preferred system;
[0022] FIG. 2 depicts a candidate interface for use with the first embodiment;
[0023] FIG. 3 depicts a flowchart for use with the skill assessor interface as part of the first preferred embodiment;
[0024] FIG. 4 depicts a flowchart for use with a recruiter interface as part of the first preferred embodiment;
[0025] FIG. 5 depicts an administrator interface for use the first preferred embodiment;
[0026] FIG. 6 depicts a referral tree or candidate tree for use with the first preferred embodiment;
[0027] FIG. 7 depicts a skill assessment score calculator methodology for use with the first preferred embodiment;
[0028] FIG. 8 depicts a search methodology for use with the first preferred embodiment;
[0029] FIG. 9 depicts a candidate availability checking methodology for use with the first preferred embodiment;
[0030] FIG. 10 depicts an example of a flowchart that may be used to calculate an SAS score for use with the first preferred embodiment;
[0031] FIG. 11 depicts a consideration calculator interface for use with the first preferred embodiment; and
[0032] FIG. 12 depicts an improved interface to that shown in FIG. 11 .
DETAILED DESCRIPTION
[0033] Preferred embodiments of the invention will now be described with reference to the accompanying drawings and non-limiting examples.
[0034] In this specification, the terms “network tree”, “referral tree”, and “candidate tree” all refer to a network of people referred to the preferred system and entered as tiers of candidates or applicants, wherein each person has been invited into the system by the layer or tier above their location in the tree. Further, the terms “candidate” and “applicant” are synonymous. Further, the terms “employer” and “recruiter” both refer to person(s) who are likely to use the embodiments to list job openings for candidates.
[0035] According a first preferred embodiment of the present invention, a system or method is provided wherein the system or method comprises a network based and enabled system of linking candidates with employers or recruiters. The system provides an online web portal acting through an internet enabled web server to provide a means to link candidates with job openings posted by employers on the system.
[0036] Preferably, the system may include a referral tree within which candidates may refer other potential candidates to the system and encourage them to also apply for job openings or opportunities.
[0037] The system is generally adapted to operate on a server including a database of profiles of candidates and employers/recruiters. The database may also include selected data about these groups and people. The system is adapted to be engaged by users through a web browser interface.
[0038] Preferably, the first preferred embodiment may include a system with at least four distinct interfaces as defined by the following list: administration interface 4 , candidate interface 1 , recruiter interface 2 , and skill assessor interface 3 . Some of the basic system components of the distinct interfaces are shown or depicted in FIG. 1 . It is noted that preferably each one of the shown interfaces may be selectively connected to databases or tables recording data attributed to each interface. Each interface includes a plurality of data types to record information and data about regarding the relevant type of user.
[0039] The candidate interface is depicted in FIG. 2 , wherein this interface 21 is preferably used by the candidate to setup a profile. This profile may save the candidate's resumes for different skills and keywords, enter sales lead, look at his referral tree, redeem points and look at his point summary. The interface 21 may preferably include several regions or subtype interface screens available for the candidate or user to setup and engage. These regions include: My Profile area 22 , My Tree area 23 , Report A Need area 24 , My Jobs area 27 , My Reports area 26 , and My Offers 25 .
[0040] In respect of the My Profile area 22 , candidate may: setup or upload his or her skills to the system, upload his or her profile and setup keywords relating to his or her skills. He/she may also preferably be able to enter the job categories relative them and may also provide skill rating on a scale of 10. Candidate may also provide his personal details, address, email, social media contact details, country, bank details and tax file number (or social security number) or other relevant information or data about the candidate for completing his or her registration.
[0041] In respect of the My Tree area 23 , the candidate may view his or her referral tree which is described in greater detail in relation to FIG. 6 . This area may generally include further subtype areas labelled Treeview area (which allows the candidate to view their network or referral tree), Refer A Friend area (which allows the candidate to instruct the system to send email notifications or invites to friend or acquaintances of the candidate, if they accept they are joined to the aforementioned referral tree), statistics area (which allows the candidate to view various statistics about their own job applications or applications made by people in their referral tree).
[0042] In respect of the Report A Need area 24 , the candidate may be allow to report a sales need to system. Once a need is reported it is relayed (preferably by email) to the Administrator interface who allocate it to recruiter. Preferably, the candidate can keep a track of status of his or her needs that are reported to the system.
[0043] In respect of the My Jobs area 27 , this area may allow the candidate to view job opportunities referred by other people or search for job opportunities that significantly match the candidate's profile. This area may also allow the candidate to apply for job opportunities and send their contact details to recruiters or employers. Also in this area, the candidate may be able to view the progress and status of current job applications that they have been applied for. This subtype area is named “Jobsflash”.
[0044] In respect of the My Reports area 26 , the candidate is preferably allowed by the system to obtain several reports from the system using the web portal. These reports may include: My Tree report which may show a report on next tier candidates referred by the candidate to the system; MyPoint report which is a report based on the current or chosen financial year and preferably demonstrates points or credits gathered by candidate as part of the later described consideration scheme; and My Report A Need report which is a report that generates or shoes the status and summary of sales lead reported by candidate or referred by the candidate.
[0045] In respect of the My Offers area 25 , the candidate is allowed by the system to view offers made to them and/or to the next tier of referred candidates. Based on points or credits gathered by candidate he or she may be able to redeem the points or credits on either training services or cash voucher at predetermined time internals. The system may be integrated with other commercial training services provider whose vouchers they can redeem from within the system using the points or credits.
[0046] FIG. 3 depicts further information and detail regarding the Skill Assessor Interface 31 , which can be chosen from the Candidate's Interface 21 . Within the Skill Assessor Interface 31 , a process is shown wherein candidates may engage with the system to assess the candidate's skills in a particular chosen area or field 32 and then the system may generate a skill rating 33 based on the testing results of the candidate. The skill rating is converted to a SAS score (this is a standardised score from a predetermined maximum mark e.g. out of 100) and the SAS score is then relayed to the recruiter or employer.
[0047] Alternatively, an external skilled assessor may independently interview a candidate independently and update the skill assessor interface with rating of candidate on each of the skills. Preferably, this is skill assessment is conducted on a confidential basis available only to permitted users. This information will be used by recruiter and system to automatically calculate skill assessment score (SAS score) of relevant candidate based on needs. An example of how the SAS score may be calculated is described in further detail below and with reference to FIG. 7 .
[0048] Along with the candidate skill assessment feedback of existing candidate will also be updated in the system in form of rating and a quote. Candidate with a generally good feedback assessment will help them get improve their Candidate Score value which is calculated based on SAS score, resource cost and feedback. Preferably, the skill assessment of candidate may be completed every 6 months or some other predetermined time interval.
[0049] The Recruiter Interface 41 is depicted in greater detail in FIG. 4 . The Recruiter Interface 41 may also be named the Franchise Interface. Preferably, the Recruiter Interface 41 may be engaged through the Report a Need area 24 in the Candidate interface, My Jobs Area 27 , or Skill Assessor Interface 31 . The Recruiter Interface 41 may function to allow a recruiter or employer to engage with the candidates and monitor status and progress through the system.
[0050] Preferably, the Recruiter Interface 41 may include a Search Candidates area 44 . Area 44 may allow the recruiter to search for candidates based on any of the following combinations of search types including: costing, keywords, skills, SAS Score 45 , Candidate Value Score 46 and other needs. Automatic skill assessment algorithm would find out list of relevant candidates based on Skill Assessment score 45 . Preferably, the System may also confirm or verify candidates availability based on real time availability algorithm 47 or data/information added by candidates in their respective profile.
[0051] System may also automatically provide Candidate Value Score 46 for each of the candidate based on his SAS score, client feedback and daily rate. Preferably, the Candidate Value Score may be calculated as per the flowchart depicted in FIG. 10 . Further details of the Candidate Value Score are further described within the accompanying description to FIG. 10 .
[0052] The recruiter interface 41 also may engage the system to calculate points/credits to be awarded to referring people. Preferably, these points or credits will be calculated based on Point or Credit Calculation Algorithm (this algorithm is described in greater detail in relation to FIG. 11 ). The system will report to the recruiter the exact quanta of points or credits issued to the referring people or persons and the recruiter will be aware how much points will each of the participants in the system will be issued.
[0053] The Sales lead tracking module or area 42 , may allow the recruiter to gain system reports relating to the following areas: Customer relationship management interface to track all the leads generated by the system; all the leads assigned to recruiter/franchises can be tracked; and point/credit calculation and invoice creation, which the system may to a finance or accounting system 53 (as described in respect of FIG. 5 ).
[0054] The Job Flash area or module 43 , may allow the recruiter to “flash job” or post to entire list of candidates in that job category. The recruiter may also have access to Smart Job Flash which may allow them to send job opportunities to only relevant candidates or candidates shortlisted based on SAS score and Candidate Value score.
[0055] FIG. 5 depicts the Administrator Interface 51 or Admin Interface. This interface 51 is generally comprised of four general areas or modules: overall candidate tree 52 , finance system 53 , system reports 54 , and Access Level Controls 55 . This interface is generally adapted for use by a system administrator or other person with administration privileges to the system.
[0056] Preferably the Admin Interface 51 , may allow a user to search for candidates, looks for leads, assign leads to sales consultants, look at finance reports, flash job to candidates, add/update new candidate or existing candidates.
[0057] Preferably, the Overall Candidate Tree module 52 , may allow the user to conduct any of the following actions using the system: View overall job tree subarea wherein the user may be able to view overall tree of candidate IDs through this sub area; Search candidates subarea wherein the user is able to search candidates based on candidate-ID (which is generated when candidate registers) and administrator will be able to see candidate details, skills and its network tree; Update Candidate Details subarea wherein the user may be able to update details of selected candidates; Create new Candidates subarea wherein the user may be to create new candidate based on request received using offline mode.
[0058] The Finance System module 53 , may be adapted and modified to allow the user to track invoices, payments, overdue accounts and taxes (where applicable). Reports may also be generated of relevant financial information and data over a predetermined time interval.
[0059] The System Reports area 54 , may allow the user to generate or view all or at least some of the system level reports and these may include: Finance reports area—Various finance reports for the whole system to be generated which would integrate invoice system with points redeemed by candidates; Point Tracking report area—This report may track the points or credits awarded or issued by the system, redeemed by each of the candidate; and Invoice Tracking area—In this area, the user will be able to track pending invoices and make comparisons to payments made.
[0060] In respect of the Access Level Controls 55 , the user may be granted control in the system over the Recruiter, Candidate and Skill Assessment interfaces. The user may be granted access and privileged to all features of recruiter, candidates and skill assessment interfaces. In respect of the Candidate Skill Assessment—For each candidate skill assessment to be done and correct fields (which are predefined for every job category) to be updated. This may be used by the Recruiter to search right candidates for a specific role. This can also be done from Recruiter and Skill Assessor interface and Pre-existing fields in each job category to be added which can be updated by admin or skill assessor. In respect of the Sales lead tracking, the user may control: Customer relationship management interface to track all the leads generated by the system; and also all the leads assigned to recruiter/franchises may be tracked.
[0061] FIG. 6 depicts an example of a referral tree relative to candidates. On top of the referral tree is the system itself or the administrator user located at position 62 . The system initially invited some key users or candidates and these are shown at position 63 . Typically, the user of the candidate system is depicted at location 63 near to the top of the referral tree 61 . The user 63 has invited several second tier candidates to join the system and they agreed. The second tier candidates are located at location 64 and in this example two second tier candidates are shown. The second tier candidates 64 then invited a further tier of candidates and this next tier become third tier candidates 65 . Fourth tier candidates 66 were invited by third tier candidates 65 . In this example, the system continues forming a referral tree by linking associated and invited candidates along the lines of the referrals sent to them. Theoretically, there is no limit to the amount of tiers that may be generated to form the referral tree. In this example, a hypothetical fifth tier candidate was placed or employed by a recruiter or employer.
[0062] FIG. 11 depicts the point or credit system calculation screen used to calculate consideration paid to referring parties. In this embodiment, all parties forming part of the referral tree and in the linkage chain to the top most position receive some form of consideration. The consideration may take many forms include: cash, credits or points. The credits or points may be used as currency within the system or traded for preapproved external service providers.
[0063] The screen 110 shown in FIG. 11 depicts the basic elements of the consideration or payment system. This screen sets out the pay-out percentages of referral fee. Generally, the referral fee is a predetermined set amount and this divided amongst the qualifying referring candidates. The screen 110 is adapted to calculate and populate the fields once the CALCULATE button is depressed on the screen.
[0064] A hypothetical worked example of point calculation is depicted in FIG. 12 . Section 121 of the screen depicted in FIG. 12 shows a sample of share division of the points or credit reward on a percentage basis. The network individual share depicts the percentage share of the consideration to be attributed to the qualifying members of the referral tree.
[0065] Sub-screen 122 depicts the breakdown of percentage shares allocated to qualifying individuals within the selected referral tree. Preferably, the percentage of consideration is split between qualifying members. However higher percentages are paid to generally higher positions on the referral tree.
[0066] Algorithms
[0067] The following description defines the preferred means and methods of calculating the algorithms, calculations and scores referred to this specification:
[0068] Points Calculation Algorithm
[0069] Preferably, the points or credits are awarded by the system to referring people or persons according to the following calculations, rules and assumptions:
Extra/Unused points go to System Maximum point for Network Individual cannot be greater than selected Candidates points Network Individual do not include Top Most network individual
[0073] The Key variables for this algorithm may include: (Note: levels are calculated from bottom to top)
[0074] 1. SystemlPortal Share-a%
[0075] 2. Franchise/Recruiter share-b%
[0076] 3. Sales lead reporter share-c%
[0077] 4. Candidate (who gets job) Share-d%
[0078] 5. Topmost network individual-f%
[0079] 6. Total Direct Networked Individuals share-g%
[0080] 7. # of direct levels (excluding topmost and candidate)=y%
[0000]
Algorithm for calculation of percentage points for individual (IND)
If y>5 and IND is between level 1-5 directly connected to candidate
P1 = (INTEGER Division (g/y))+1)
Elseif y>5 and IND is between level 6- topmost directly connected to
candidate
P2 = (g − 5*P1)/y−5
Elseif Y<5
P3 = g/y
Till P3 >=d
{
d = d+2.5
f = f+2.5
g = g−5
P3 = g/y
[0081] The following is an example of the algorithm applied to hypothetical data:
[0000]
Scenarios -1 - Where y = 11 levels and IND is at level 6
1. System/Portal Share - 10%
2. Franchise share - 35%
3. Sales lead reporter share - 5%
4. Candidate (who gets job) Share - 15%
5. Topmost network individual - 5%
6. Direct Networked Individuals share - 30%
Answers
P1 = 30/11 + 1 = 3
P2 = (30 − 15)/6 = 2.5
Scenarios -2 - Where y = 7 levels and IND is at level 7
1. System/Portal Share - 10%
2. Franchise share - 35%
3. Sales lead reporter share - 5%
4. Candidate (who gets job) Share - 15%
5. Topmost network individual - 5%
6. Direct Networked Individuals share - 30%
Answers
P1 = 30/7 + 1 = 5
P2 = (30 − 25)/2 = 2.5
Scenarios -3 - Where y = 3 levels and IND is at level 2
1. System/Portal Share - 10%
2. Franchise share - 35%
3. Sales lead reporter share - 5%
4. Candidate (who gets job) Share - 15%
5. Topmost network individual - 5%
6. Direct Networked Individuals share - 30%
Answers
P3 = 10
Scenarios -4 - Where y = 1 levels and IND is at level 1
1. System/Portal Share - 10%
2. Franchise share - 35%
3. Sales lead reporter share - 5%
4. Candidate (who gets job) Share - 15%
5. Topmost network individual - 5%
6. Direct Networked Individuals share - 30%
Answers
P1 = 10
[0082] Skill Match Algorithm
[0083] The skill match algorithm is preferably calculated as part of the Skill Assessor interface 31 . The preferred calculation, steps and processing assumptions are herein described in relation to this algorithm:
[0084] Step-1—Assessor update skill ratings
[0085] For each skill category in the system there will be sub categories defined. For each of these sub-categories there will be rating on a scale of 1-10.
[0086] For instance for Software Quality and Testing category there can be sub-categories like
Overall Testing experience Functional Testing User acceptance testing Datawarehouse testing Test Automation tools Performance testing HP QTP Selenium Tosca Lead Test Team Test management
[0098] Assessor based on resource profile, call or face to face interview will update skill rating. These ratings will be updated in the system. Further details are shown regarding these ratings, scores and values in relation the FIGS. 7 to 11 of the accompanying figures.
[0099] Step2—Recruiter search
[0100] When recruiter searches for candidate he can search based on key criterion needed by client. For instance, if recruiter is looking for a candidate with overall experience of 4+and experience in using tool HP QTP with a rating of 9 or 10, recruiter can easily find that person within the system based providing correct search criterion.
[0101] When recruiter gives this search a SAS score will be calculated based on how many parameter match the score. Higher the number of matches, higher the score.
[0102] For instance if recruiter searches for above criterion and there is a candidate who has 3+years of experience and rating of 9 In QTP, he will be given 5 points for criterion match for HP QTP and 3 points for overall experience as he did not completely match the criterion. So he gets a SAS rating of 8.
[0103] If there is another candidate who has 5 years of experience and 9 rating in HP QTP, he will get SAS rating of 10. Preferably the recruiter then identifies and chooses the most preferred candidate. The recruiter searches are generally referred to and depicted within the preferred embodiment of the present invention in relation to FIGS. 7 to 12 .
[0104] Step3—Recruiter update/downgrade rating
[0105] Recruiter if required can either downgrade the rating of candidate based on client feedback or he can ask assessor to re-skill the candidate if he/she feels candidate has good skills.
[0106] Real-time Availability Status Update Method
[0107] A significant issue problem with candidates is that it is hard to find or detect when the specific candidate will be available and finish their current assignment especially if they are contracting. But usually recruiters are not able to reach correct candidates leading to waste of their time and effort.
[0108] As part of initial profile information, the system may ask for candidate Linkedin™ details (just username) or details of some other social media based internet website; and link those users to its System Linkedln profile. Once linked, system will automatically run a software job to check if candidate status has changed on his role. If yes, an automatic email will be triggered to the candidate to update his profile in system and by default his status will be set to ‘under observation’
[0109] FIG. 9 depicts the system methodology in relation to checking and confirming candidate availability. The candidate profile 91 stores information and data about the current status of the candidate in relation to whether they are currently looking for work opportunities and preferably information about possible or likely start dates for new employment offers. The system may preferably automatically update this information from linked social media websites 93 or from other external systems 94 . If there is no change, the system waits for a predetermined period of time elapse 95 (in this example—1 day). If yes, the system reconfirms the data changes with the candidate in step 96 . If the candidate agrees, the system will update the information as step 97 .
[0110] Smart JobFlash Method
[0111] Most of the recruiters send mass email campaigns to registered users with them when they get a need. Lot of candidates who apply do not match the criterion and recruiter has to go through painful process of opening the resume and reject the candidate
[0112] To generally improve this mass email, recruiter may be more selective in this mail campaigns if he knows list of relevant candidates. The selectivity may be effected by using SAS score to create a short listing process, Recruiter may send mass email to candidates who match the criterion so that only relevant candidates reply to him.
[0113] FIG. 8 generally depicts the system methodology relating to the Smart Job Flash and Smart Search capabilities of the system. The system starts with the recruiter generally requiring a search 81 . The system produces a list of possible candidates based on the candidate profiles stored in its databases. The recruiter then shortlists the preferred candidates which are usually chosen based on the SAS score or Candidate Value Scores 82 . The search step 82 may be named Smart Search.
[0114] The recruiter is then given an option by the system to Smart Job Flash the short listed candidates at step 84 . The Smart Job Flash is preferably a computerised system of contacting the shortlisted candidates with the job opportunity and asking them to formally apply.
[0115] The next step 83 is for the shortlisted candidates to apply for the job opportunity and the recruiter employs the most suitable candidate.
[0116] Smart Resume Screening Method
[0117] As part of Smart resume screening algorithm, once a candidate within the system replies to job flash posted to them, recruiter interface will automatically match the candidate profile against their skill assessment score and add them to 2 separate buckets. First bucket is of high priority candidates who fit into the skill assessment score and second category of candidate who do not fit into the skill assessment score. Resumes will be matched using the SAS score.
[0118] Candidate Value Score
[0119] Often along with the SAS score (skill match score), recruiter may also require to know which candidate will give them more value in terms of business benefit. Candidate whose skills match the best and recruiter can get at lowest rate will have the best score value. Also another factor important for the calculation will be is the feedback received from client.
[0120] The calculation of SAS Score is depicted in detail in FIG. 7 , wherein the first step 71 is for the skill assessor to enter a numerical assessment of predetermined skills based on a grading of 1 to 10. The skills are preferably sorted into subcategories to cover multiple fields or skillsets of the most candidates.
[0121] Preferably, the next step 72 is for the recruiter to search the databases of the system by setting minimum threshold values for certain skills for which they are looking for in a preferred candidate. The next step 74 , the system calculates an aggregated score based on the preferred skillsets chosen by the recruiter and the aggregated and averaged score forms the SAS Score. In the example shown in FIG. 7 , the SAS score is scored out of 10 marks however other maximum mark limits are possible including 100 or 1000.
[0122] In FIGS. 10 , the candidate value score procedure or process is depicted and described. Preferably, the recruiter conducts a search for candidates 100 . The system reports a list of candidates with SAS scores 101 , and then the recruiter is allowed by the system to short list the candidates based on the candidate value score 103 . The candidate value score preferably includes the capacity to grade candidates based on the any of the following field or combinations thereof: SAS Score, resource cost, local experience and previous client feedback (which may also be stored in the candidate's profile). The recruiter may then select the most preferred candidate 102 and employment may commence.
Preferred Features of the First Embodiment
[0123] Preferably, the candidate may initially register their resume as part of their profile. The Candidate may then refer more candidates into the database who can then refer more candidates forming a multi-level tree or referral tree. In this way tree of job candidates is formed with the first candidate at the top of the tree.
[0124] When a recruiter or an employer instruct the system for right candidates for a particular job opportunity, this user searches for candidates in the system's database. Once the candidate is selected, generally 50% of the overall profit will be kept by system and remaining 50% will be distributed between qualifying people or persons within linked within the referral tree in terms of points based on an incentive based algorithm. In this way not only the specific candidate employed earns but also the individuals who have referred the candidate to the system will earn on this placement (candidate Employment and Candidate network or referral tree).
[0125] Points earned by candidates may be redeemed in form of training services or royalty at a predetermined time. For the sales, candidates can refer a lead to the portal and they further get paid extra 5% for providing the lead on closure which is part of overall inventive.
[0126] Preferably, this system may be integrated with other training providers so that its points or credits can be redeemed for discount vouchers by their system.
[0127] In their profile, candidates will be able to setup their skills and rating in each of the known category. Skill assessment may be completed by technical experts in their respective fields and system updated for future needs. Preferably, automatic Candidate Skill assessment mechanism will help searching of candidates innovatively based on their skill assessment score (SAS) algorithm.
[0128] Another challenge with previous recruitment system has been the ability to get real-time candidate availability check of candidate on when he is next available. System will be integrated with social platforms like Linkedln™ to get real-time update on candidate availability status. It will also send auto mailer to candidates if there existing status is not updated within the system. This will help recruiter when they are looking for candidate to make sure they find right candidates.
[0129] The preferred system may also include the Smart resume screening algorithm, once a candidate within the system replies to job flash posted to them, recruiter interface will automatically match the candidate profile against their skill assessment score and add them to 2 separate buckets. Preferably, the first bucket may be of high priority candidates who fit into the skill assessment score and second category of candidate who do not fit into the skill assessment score.
[0130] Another challenge may be that with recruiters may need to direct their job opportunities to specific candidates. Preferably, the recruiters may flash jobs (email campaign or advertisement) to right candidates so that they get only relevant profiles. As part of Smart Job flash algorithm, mass email campaigns are going to be addressed to candidates who fit into skill assessment score requirement for that specific role.
[0131] Also included is Candidate Value Score algorithm which may preferably shortlist candidates by fitting them into the criterion which gives best value for money for client and recruiter. The preferred system may be also suitable for franchises to access across to the world who can manage individual recruitment areas globally.
[0132] Preferably, the Job Flash interface may flash job to registered candidates for jobs posted within JobTree and jobs posted on other online sites like seek.com.au, monster.com
[0133] Innovative Algorithm using which redeemable points will be distributed to all the individuals and candidate in the network tree or referral tree
[0134] Skill assessment process and automatic skill assessment score (SAS) calculator which will match resumes with the job need and come
[0135] System to link Redeemable points with Training providers and online course providers for further skill enhancement
[0136] Real-time candidate availability update feature will immensely help recruiter to know the current status of the candidate when they urgently need resources
[0137] As part of Smart Job flash algorithm, mass email campaigns are going to be addressed to candidates who fit into skill assessment score requirement for that specific role
[0138] Enhancement and security mechanism of the system with privileges to franchises
[0139] Candidate will have option to add multiple profiles (say a Java profile and Dot-net profile) under same candidate id. This will be score independently by assessor
[0140] Although the invention has been described with reference to specific examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms, in keeping with the broad principles and the spirit of the invention described herein.
[0141] The present invention and the described preferred embodiments specifically include at least one feature that is industrial applicable.
|
A network based referral system for recruitment, comprising: a job profile corresponding to inputs by a first user of said system; an applicant description module which includes data from an applicant description profile corresponding to characteristics of a second user and an applicant referred to the system by the second user; and a database for storing a plurality of said job profiles and for receiving said applicant description profile over said network and for matching characteristics of said applicant description profile with corresponding characteristics of said job.
| 6
|
FIELD OF THE INVENTION
This invention relates to the synthesis of unsaturated insect pheromones, including (7Z,11Z)- and (7Z,11E)-7,11-hexadecadien-1-yl acetate, gossyplure, of the female pink bollworm moth Pictinophora gossypiella, and the intermediates therefor.
BACKGROUND OF THE INVENTION
A frequently used synthetic method for the preparation of unsaturated aliphatic compounds has been the Wittig coupling of an arylphosphonium ylid with an aldehyde or ketone. Suitable procedures for the preparation of ylids and the Wittig reaction are described in A. W. Johnson, "Ylid Chemistry" Academic Press, Inc., New York (1966). The method has proven to be of particular importance in the preparation of unsaturated aliphatic compounds useful as insect sex pheromones. A review describing the preparation of these attractants is "The Synthesis of Insect Sex Pheromones" by Clive A. Hendrick in Tetrahedron, Volume 33, pp. 1845-1889 (1977). Additional reports on the preparation of unsaturated alkyl compounds using phosphonium ylids can be found in U.S. Pat. Nos. 3,712,880; 3,732,282; and 3,671,558.
More specifically, the sex pheromone of the female pink bollworm moth has been identified as a mixture of the 7Z,11Z)- and (7Z,11E)-7,11-hexadecadien-1-yl acetate, Hummel, et al., Science, 181, 873 (Aug. 31, 1973). A number of syntheses of this pheromone and related compounds have also been described by Anderson and Hendrick in U.S. Pat. Nos. 3,919,329; 3,953,532; 3,987,073; and 3,989,729, and by Sonnet, in the Journal of Organic Chemistry, 30, pp. 3793-3794 (1974).
A disadvantage of these described procedures is that the phosphonium ylid used for the coupling normally is used to introduce only one double bond thus necessitating a number of additional chemical reactions, reagents, solvents and so forth to introduce additional double bonds into the aliphatic carbon chain. It has been further found that previously described methods suffer from a number of inherent disadvantages, including multiple reaction steps which lead to poor results for large-scale preparations.
It would therefore be extremely valuable to have a process for preparing unsaturated aliphatic compounds utilizing a single cyclic phosphonium ylid by reaction with a suitable carbonyl derivatives to afford the desired unsaturated aliphatic compounds easily and in high yield and purity, and that is also readily adaptable to large-scale commercial production.
DETAILED DESCRIPTION OF THE INVENTION
The present invention concerns a coupling process whereby a cyclic phosphonium ylid is coupled with a suitably protected aldehyde or ketone to produce the corresponding phosphine oxide in high yield. This compound is subsequently treated with a second aldehyde followed by conversion to an ester, for example, an acetate. Such acetates are valuable and useful as insect sex pheromones in the control of specific insect populations.
These compounds having multiple double bonds have a number of geometrical isomers with different physical and chemical properties. These isomers are described as "trans" designated by "E" and "cis" designated by "Z". Thus, a compound having two carbon-carbon double bonds could have the following isomers: Z,Z; Z,E; E,Z; and E,E. A number usually precedes the letter, e.g., 7Z, to indicate the position of the double bond in the carbon chain.
More specifically, this invention concerns the preparation of specific unsaturated aliphatic compounds and mixtures of compounds, such as (7Z,11)- and (7Z,11Z)-7,11-hexadecadien-1-yl acetate, gossyplure, the insect sex attractant of the pink bollworm moth which is described in U.S. Pat. No. 3,919,329, which is incorporated herein by reference.
The synthesis of this invention is outlined as follows: ##STR1##
The isomer ratio of Z,E to Z,Z (and E,Z and E,E) for Compounds, such as IX and XI, produced by this process may be changed by changing the order of the addition in the process. Therefore, the process may also be described according to the following sequence: ##STR2##
In summary, the present invention relates to two processes for the preparation of a compound (IX) of the formula ##STR3## wherein m is an integer from 1 to 11
n is an integer from 1 to 9
p is an integer from 1 to 6, and
R 1 is selected from the group consisting of tetrahydropyranyl, benzyl, triphenylmethyl, trimethylsilyl, t-butyldimethylsilyl;
which first process comprises:
(a) contacting a cyclic phosphonium halide of the formula (I) ##STR4## wherein R 2 is selected from the group consisting of hydrogen, and straight and branched chain lower alkyl groups,
R 3 and R 4 are independently selected from the group consisting of phenyl, lower alkyl-substituted phenyl, lower alkoxy-substituted phenyl, and halo substituted phenyl;
X is a halogen selected from the group consisting of chlorine, bromine, and iodine; and
n is as set forth above,
with an alkali metal alkoxide to produce an ylid of the formula (II) ##STR5## wherein R 2 , R 3 , R 4 and n are as set forth above;
(b) treating said ylid with a protected hydroxyalkyl aldehyde of formula (III) ##STR6## wherein R 1 and m are as set forth above, to produce a phosphine oxide of formula (IV) ##STR7## wherein m, n, R 1 , R 2 , R 3 and R 4 are as set forth above,
(c) contacting said compound with an organic lithium compound (V) in an aprotic solvent medium to produce a lithium salt of formula (VI) ##STR8## wherein m, n, R 1 , R 2 , R 3 and R 4 are as set forth above,
(d) treating said lithium salt with an aldehyde of formula (VII) ##STR9## wherein p is an integer from 1 to 6, to produce an alcoholate of formula (VIII) ##STR10## wherein m, n, p, R 1 , R 2 , R 3 and R 4 are as set forth above
(e) heating said alcoholate in an aprotic solvent medium to produce a diene of formula (IX) ##STR11## wherein m, n, p, R 1 , and R 2 are set forth above, and which second process comprises:
(a) contacting a cyclic phosphonium halide of formula (I)
wherein n, X, R 2 , R 3 and R 4 are as set forth above,
with an alkali metal oxide to produce an ylid of the formula (II)
wherein R 2 , R 3 , R 4 and n are as set forth above,
(b) treating said ylid with an aldehyde of formula (VII) wherein p is an integer from 1 to 6, to produce a phosphine oxide of formula (XII) ##STR12## wherein n, p, R 2 , R 3 , and R 4 are as set forth above,
(d) treating said lithium salt with a protected aldehyde of formula III ##STR13## wherein m and R 1 are as set forth above, to produce an alcoholate of formula (XIV) ##STR14## wherein m, n, p, R 1 , R 2 , R 3 and R 4 are set forth above, and
(e) heating said alcoholate in an aprotic solvent medium to produce a diene of formula (IX) wherein m, n, p, R 1 and R 2 are as set forth above.
In both of the above processes there was further included the step of converting the diene of formula (IX) to its corresponding acetate (XI).
The reaction scheme of the invention is shown above in six steps. However, this representation was made only for purposes of clarity of description, and each compound depicted need not be isolated at the end of each such step or purified. Those skilled in the art will recognize that this is, in effect, a three-step process wherein Step 1 progresses from the starting phosphonium halide (I) to the aliphatic phosphine oxide (IV), Step 2 is the conversion of (IV) to the diene (IX); and Step 3 is the optional conversion of (IX) to the acetate derivative (XI).
Phosphonium halides, as represented by Compound (I), are prepared by treating the corresponding hydroxyalkyl diarylphosphine in an aprotic solvent medium with the appropriate hydrogen halide followed by treatment of the product thus formed with a base.
The presently preferred compounds of Formula I are those where n equals 2, 3, 4 or 9. The most preferred compound is when n equals 3. R 2 may be selected from the group consisting of hydrogen, and straight and branched chain lower alkyl groups. The lower alkyl groups include those groups containing 1 to 5 carbon atoms, such as the methyl, ethyl, n-propyl, iso-propyl, n-butyl iso-butyl and pentyl groups. The presently preferred compound is where R 2 is hydrogen.
R 3 and R 4 are independently selected from the group consisting of phenyl and phenyl substituted with alkyl groups, alkoxy groups and halogens. Lower alkyl groups include those defined above. Lower alkoxy groups include those straight and branched groups containing 1 to 4 carbon atoms including methoxy, ethoxy, n-propoxy, iso-propoxy and butoxy; and halosubstituted phenyl includes those phenyl compounds substituted at any position with one or more fluorine, chlorine, bromine, or iodine, and combinations thereof. Presently preferred R 3 and R 4 groups are unsubstituted phenyl.
The solvents used to prepare Compound (I) may be any aprotic solvent capable of forming azeotropic mixtures with water. Presently preferred solvents include benzene, toluene, xylene, n-hexane, n-pentane, ethers, cyclohexane, cyclopentane, and mixtures thereof. A presently preferred solvent is toluene.
The hydrogen halide used to prepare Compound I may include hydrogen chloride, hydrogen bromide and hydrogen iodide. The presently preferred hydrogen halide is hydrogen bromide. The hydrogen halide may also be formed in situ by ordinary methods used in the art.
The usual reaction temperatures employed are in the range between -20° C. and 150° C. Usually the removal of the water during this reaction occurs by azeotropic distillation and the temperature of reaction and water removal will be dictated by the choice of the azeotropic mixture. For example, in a presently preferred mode the azeotropic mixture of toluene and water will boil under standard conditions at about 84° C. The boiling temperature of a normal toluene reaction at reflux will be about 110° C. The time for the reaction to go to completion ranges from several hours to several days, and will depend upon the specific cycloalkyl phosphonium halide being prepared.
Other methods may be used to prepare Compound I that are known to those skilled in this art. For instance, G. A. Gray et al. describes a number of methods in the Journal of the American Chemical Society, vol. 98, pp. 2109-2118 (1976) and references cited therein which are incorporated herein by reference.
In the conversion of Compound I to Compound IV or to Compound XII, I is initially treated with an alkyl alkali metal oxide, such as potassium t-butoxide, sodium t-butoxide, calcium t-butoxide, sodium ethoxide, potassium ethoxide, or mixtures thereof. A presently preferred reagent is potassium t-butoxide.
The solvent system for this step should be essentially anhydrous, and an inert gas, such as nitrogen, may be used to maintain anhydrous conditions during the reaction. Further, the solvent may be any aprotic solvent medium, such as ethers, including diethyl ether, tetrahydrofuran, diphenyl ether, diethylene glycol dimethylether, or aromatic and hydrocarbon solvents such as benzene, toluene, xylene, pentane, hexane, cyclohexane, cyclopentane, petroleum ether or mixtures thereof. A presently preferred solvent is tetrahydrofuran.
In Compound III, R 1 as a protecting group may be selected from the group consisting of tetrahydropyranyl, benzyl, triphenylmethyl, trimethylsilyl, t-butyldimethylsilyl and the like. A presently preferred group is tetrahydropyranyl. Presently preferred compounds of III are those where m equals 2, 3, 5, 6 or 8. The most preferred is where m equals 6.
The reaction may be conducted at a temperature between -20° C. and 100° C. A presently preferred temperature is about +20° C. The reaction time is in the range of several minutes to 24 hours. A presently preferred method is to form the ylid over about 90 minutes followed by addition of the protected aldehyde (III) and stirring of the reaction mixture for 20-24 hours.
In the conversion of Compound IV (or of Compound XII) to Compound IX, Compound IV is initially treated with an organic lithium Compound V to form the lithium salt VI. The organic lithium compound may be aliphatic or aromatic, such as methyllithium, ethyllithium, propyllithium, butyllithium, pentyllithium, phenyllithium, and benzyllithium. A presently preferred Compound V is n-butyllithium. The solvent for this reaction should be an essentially anhydrous aprotic solvent, such as hexane, pentane, cyclohexane, cycopentane, petroleum ether, benzene, toluene, diethyl ether, tetrahydrofuran and mixtures thereof. A presently preferred solvent mixture is tetrahydrofuran, diethyl ether and hexane. The solvent mixtures may range from 0.1 to 99.9 percent for each component. A presently preferred ratio for tetrahydrofuran, diethyl ether and hexane is about 49/49/2 by volume.
The reaction is initially performed at about -78° C. and is gradually allowed to warm to ambient temperature of about 20° C. as it proceeds.
Presently preferred aldehydes of Formula VII are those where p equals 1, 4 or 5. The most preferred aldehyde VII is where p equals 4.
The lithium salt VIII (or XIV) may be decomposed to the diene IX by various methods. One method is to slowly heat VIII (or XIV) in an aprotic solvent such as hexamethylphophoramide, dimethylformamide, or mixtures thereof at temperatures between 40° and 100° C. A preferred method is to heat VIII in hexamethylphosphoramide at about 70° C. for about two hours. A second preferred method is to treat the salt VIII with water, dissolve in an aprotic solvent and treat with an alkali or alkaline earth hydride, such as sodium hydride, for a few minutes to a few hours. A preferred method is to treat the lithium salt with water, dissolve the alcohol in dimethylformamide and treat with sodium hydride under routine conditions. The reaction mixture is then purified by standard techniques to give the protected diene.
Diene IX is converted to acetate XI by treatment with Compound (X), ##STR15## wherein Y is selected from the group consisting of chloride, bromide, hydroxy, methoxy, ethoxy, acetoxy and mixtures thereof. A presently preferred method is to dissolve IX in glacial acetic acid (e.g., where Y=hydroxy) followed by acetyl chloride (e.g., where Y=chloride) at about 20° C. for about 30 minutes followed by normal isolation and purification.
Specifically, the process with minor variations is useful to prepare the following insect sex pheromones; (9Z,12E)-9,12-tetradecadienyl-1-acetate, of the almond moth (Cadra cautella) and also the Indian meal moth (Plodia interpunctella); (4E,7Z)-4,7-tridecadienyl-1-yl acetate of the potato tuberworm moth (Phthorimaea operculella); (7Z,11E)-and (7Z,11Z)-7,11-hexadecadien-1-yl acetate of the pink bollworm moth (Pectinophora gossypiella), the 7Z,11E isomer of the angoumois grain moth (Sitograga cerealella Oliv), and also the (7E,11Z)- and (7Z,11Z)- isomers of the cherry tree borer moth (Synanthedon hector); (3E,13Z) and (3Z,13Z)-3,13-octadecadien-1-yl acetate of the lesser peachtree borer (Synanthedon pictipes) and the peachtree borer (Sanninoidea exitiosa); and (6E,11Z)-6,11-hexadecadien-1-yl acetate of the polyphemus moth (Antherea polyphemis).
In a similar manner, the following insect pheromones may also be prepared: (8E,10E)-8,10-dodecadien-1-ol, of the coddling moth (Laspeyresia pomonella); (7E,9Z)-7,9-dodecadien-1-yl acetate, of the European grapevine moth (Lobesia botrana); (E)-9,11-dodecadien-1-yl acetate, of the red bollworm moth (Diparopsis castanea); (9Z,11E)-9,11-tetradecadien-1-yl acetate, of the Egyptian cotton leafworm (Spodoptera littoralis), and (10E,12Z)-10,12-hexadecadien-1-ol, of the silkworm moth (Bombyx mori).
The most preferred application of this process is the preparation of the about 1 to 1 mixture of (7Z,11E) and (7Z,11Z)-7,11-hexadecadienyl-1-yl acetate gossyplure as the insect sex pheromone of the pink bollworm moth (Pectinophora gossypiella).
The isomerism of the carbon-carbon double bonds (E or Z) in the compounds produced by this process may be fixed as a result of stereospecific or stereoselective syntheses. However, this isomerism (E or Z) may be altered by standard equilibration or isomerization techniques, such as halogenation and dehalogenation, that are well known in the art. Such olefin isomer transformations are described, for instance, by P. E. Sonnet, Journal of Organic Chemistry, vol. 45, pp. 154-157, (1980) which is incorporated herein by reference.
The mixture of the isomers formed (E,E; E,Z; Z,E; and Z,E) are separable from the reaction mixture and from each other by virtue of their different physical properties using conventional separation techniques, such as chromatography (including thin layer, gas-liquid, and high pressure liquid chromatography) and also fractional distillation.
The isomer ratio of Z,E to Z,Z (and E,Z and E,E), for the compounds produced by this process may also be altered in the conversion of IV to VI to VIII by using different aprotic solvents, addition temperatures or methods of decomposition. The effect of changing these variables is shown in the following table:
______________________________________(7Z,11E)- and (7Z,11Z)-7,11-Hexadecadiene-1-yl Acetate(Z,E/Z,Z ratio)(Changes due to solvent, temperature,decomposition method)Addition temp. Method of Isomer RadioSolvent n-buLi.sup.a aldehyde.sup.b decompostion % ZE % ZZ______________________________________Et.sub.2 O.sup.c -78° C. 20° C. NaH.sup.d /DMF.sup.e 61.4 38.6Et.sub.2 O -78° C. -78° C. NaH/DMF 68.4 31.6THF.sup.f -78° C. -78° C. HMPA.sup.g /heat 41.7 58.3THF -78° C. -78° C. HMPA/heat 37.2 62.8hexane/ -78° C. -78° C. HMPA/heat 55.8 44.2Et.sub.2 O(9:1)THF/ -78° C. -78° C. HMPA/heat 54.4 45.6Et.sub.2 O(1:1)HMPA 0° C. 0° C. HMPA/heat 33.6 66.3______________________________________ .sup.a nbuLi is nbutyllithium .sup.b aldehyde is valeraldehyde .sup.c Et.sub.2 O is diethyl ether .sup.d NaH is sodium hydride .sup.e DMF is dimethylformamide .sup.f THF is tetrahydrofuran .sup.g HMPA is hexamethylphosphoramide
Another aspect of the invention is the preparation of novel Compounds, including Compounds IV, VI, VIII, IX, XII, XIII and XIV.
DESCRIPTION OF SPECIFIC EMBODIMENT
The following specific description and examples are given to enable those skilled in this art to understand and practice the present invention. It should not be considered as a limitation upon the scope of the invention but merely as being illustrative and representative thereof. All temperatures are reported in degrees Centigrade.
EXAMPLE 1
A solution of 103 g of 4-hydroxybutyldiphenylphosphine in 150 ml of toluene is added at room temperature to 1.5 liters of toluene saturated with hydrogen bromide with stirring. The resulting milky suspension is brought to reflux with azeotropic removal of water using a Dean-Stark trap. After one hour the mixture is cooled to 80° and resaturated with hydrogen bromide. The suspension is then brought to reflux and maintained for one hour, after which the mixture was again saturated with hydrogen bromide. The reaction mixture is then maintained at reflux overnight, and allowed to cool to room temperature. The supernatant toluene was decanted from the residual oil, and was replaced with 1.5 liters (1) of water containing 80 g. each of sodium carbonate and sodium bicarbonate. The resulting aqueous mixture is stirred for 72 hours at room temperature, saturated with sodium bromide and extracted six times with 300 ml of chloroform. The combined organic layers are dried over sodium sulfate, filtered and evaporated to yield 94.1 g, a 71% yield based on theoretical, of tetramethylene 1,1-diphenylphosphonium bromide, which on trituration with acetone has a melting point of 163°-4°.
Repeating the above procedure, in a similar manner, and substituting a stoichiometrically equivalent of
2-hydroxyethyldiphenylphosphine,
3-hydroxypropyldiphenylphosphine,
5-hydroxypentyldiphenylphosphine,
6-hydroxyhexyldiphenylphosphine,
7-hydroxyheptyldiphenylphosphine,
8-hydroxyoctyldiphenylphosphine,
9-hydroxynonyldiphenylphosphine, and
10-hydroxydecyldiphenylphosphine for
4-hydroxybutyldiphenylphosphine there are obtained the following cyclic phosphonium compounds:
dimethylene-1,1-diphenylphosphonium bromide
trimethylene-1,1-diphenylphosphonium bromide,
pentamethylene-1,1-diphenylphosphonium bromide,
hexamethylene-1,1-diphenylphosphonium bromide,
heptamethylene-1,1-diphenylphosphonium bromide,
octamethylene-1,1-diphenylphosphonium bromide,
nonamethylene-1,1-diphenylphosphonium bromide, and
decamethylene-1,1-diphenylphosphonium bromide.
EXAMPLE 2
To 24.1 g of solid tetramethylene 1,1-diphenylphosphonium bromide and 8.42 g of potassium t-butoxide under a blanket of nitrogen is added 100 ml of anhydrous tetrahydrofuran using a syringe. The resulting orange solution is allowed to stir one hour at room temperature. Using a syringe, 10.7 g of 7-(2-tetrahydropyranyloxy)heptanal was added over 30 minutes, which resulted in a noticeable rise in temperature. The reaction is allowed to stir overnight at room temperature, then was quenched with 50 ml of water. The mixture is partitioned between 200 ml of diethyl ether and water, and the resulting organic layer is washed three times with 100 ml of water and three times with 100 ml of brine. The organic extract is dried, filtered through silica gel, and evaporated to yield 22.3 g of 11-(2-tetrahydropyranyloxy)-4Z-undecenyldiphenylphosphine oxide.
Repeating the above procedure in a similar manner, and substituting a stoichiometrically equivalent of
2-(2-tetrahydropropanyloxy)acetaldehyde,
3-(2-tetrahydropyranyloxy)propanal,
4-(2-tetrahydropyranyloxy)butanal,
5-(2-tetrahydropyranyloxy)pentanal,
6-(2-tetrahydropyranyloxy)hexanal,
8-(2-tetrahydropyranyloxy)octanal, and
9-(2-tetrahydropyranyloxy)nonanal for
7-(2-tetrahydropyranyloxy)heptanal, there are obtained the following diaryl alkyl phosphine oxides:
6-(2-tetrahydropyranyloxy)-4Z-hexenyldiphenylphosphine oxide,
7-(2-tetrahydropyranyloxy)-4Z-heptenyldiphenylphosphine oxide,
8-(2-tetrahydropyranyloxy)-4Z-octenyldiphenylphosphine oxide,
9-(2-tetrahydropyranyloxy)-4Z-nonenyldiphenylphosphine oxide,
10-(2-tetrahydropyranyloxy)-4Z-decenyldiphenylphosphine oxide,
12-(2-tetrahydropyranyloxy)-4Z-dodecenyldiphenylphosphine oxide, and
13-(2-tetrahydropyranyloxy)-4Z-tridecenyldiphenylphosphine oxide.
EXAMPLE 3
To a cooled solution of 0.45 g of 11-(2-tetrahydropyranyloxy)-4Z-undecenyldiphenylphosphine oxide in 10 ml of dry tetrahydrofuran/diethyl ether (50/50) is added 0.75 ml of 1.6 M n-butyllithium in hexane, 1.2 mmol) dropwise using a syringe. After 15 min, 0.132 ml of n-valeraldehyde is added using a syringe, and the resulting solution is stirred 30 minutes, then allowed to warm to room temperature. The lithium salt is obtained, and can then be decomposed by either of the following two methods, both monitored by thin layer chromatography:
A. via heating in HMPA--Addition of 5 ml of hexamethylphosphoramide to the lithium salt followed by warming for 2 hours at 70° affected decomposition to a mixture of the dienes, (7Z,11E)- and (7Z,11Z)-7,11-hexadecadien-1-yl 1-tetrahydropyranate.
B. via NaH in DMF--Decomposition of the lithium salt to the alcohol by aqueous extraction, followed by dissolution in 5 ml of dimethylformamide, and addition of 0.12 g of sodium hydride affected decomposition to the dienepyranates in approximately 30 minutes.
In both cases, the reaction mixture is partitioned between ether and water, and the organic layer is washed with brine, dried over sodium sulfate, filtered and evaporated to give the crude tetrahydropyranates.
The crude diene-tetrahydropyranates are dissolved in glacial acetic acid (2 ml) and to the solution is added 1 ml of acetyl chloride. The reaction mixture is stirred at room temperature for 30 minutes, at which time thin layer chromatography shows complete conversion to diene acetates.
The mixture is partitioned between ether and water, and the acetic acid carefully quenched by cautious portionwise addition of solid sodium bicarbonate. The organic layer is washed with saturated aqueous bicarbonate and brine, dried with sodium sulfate, filtered and evaporated to give an amber oil, and purified by column chromatography on silica gel in methylene chloride to yield 180 mg of (7Z,11E)- and (7Z,11Z)-7,11-hexadecadien-1-yl acetate mixture, as a clear colorless oil. The nearly 1:1 ratio of isomers is determined by gas-liquid chromatography.
On a larger scale, the diene acetates are purified by distillation.
Repeating the above procedure in a similar manner, and substituting a stoichiometrically equivalent of
acetaldehyde,
n-propanol,
n-butanal,
n-hexanal,
n-heptanal,
n-octanal, and
n-nonanal for n-valeraldehyde,
there are obtained the following mixtures of diene acetates:
7,11-tridecadien-1-yl acetate,
7,11-tetradecadien-1-yl acetate,
7,11-pentadecadien-1-yl acetate,
7,11-heptadecadien-1-yl acetate,
7,11-octadecadien-1-yl acetate,
7,11-nonadecadien-1-yl acetate, and
7,11-eicosadien-1-yl acetate.
By substituting a stoichiometrically equivalent of 3-hydroxypropyldiphenylphosphine oxide for 4-hydroxybutyldiphenylphosphine oxide in Example 1, 9-(2-tetrahydropyranyloxy)nonanal for 7-(2-tetrahydropyranyloxy)heptanal in Example 2, and acetaldehyde for n-valeraldehyde in Example 3, respectively there is obtained (9Z,12Z)- and (9Z,12E)-9,12-tetradecadien-1-yl acetate. A presently preferred process is where m is 8, n is 2, p is 1, R 1 is tetrahydropyranyl, R 2 is hydrogen, and R 3 and R 4 are phenyl.
By substituting a stoichiometrically equivalent of 3-hydroxypropyldiphenylphosphine oxide for 4-hydroxybutyldiphenylphosphine oxide in Example 1, 4-(2-tetrahydropyranyloxy)butanal for 7-(2-tetrahydropyranyloxy)heptanal in Example 2, and n-hexanal for n-valeraldehyde in Example 3, there is obtained (4Z,7Z)- and (4Z,7E)-tridecadien-1-yl acetate. A presently preferred process is where m is 3, n is 2, p is 5, R 1 is tetrahydropyranyl, R 2 is hydrogen, and R 3 and R 4 are phenyl.
By substituting 10-hydroxydecyldiphenylphosphine for 4-hydroxybutyldiphenylphosphine oxide in Example 1, 3-(2-tetrahydropyranyloxy)propanal for 7-(2-tetrahydropyranyloxy)heptanal in Example 2, and using n-valeraldehyde as in Example 3, there is obtained (3Z,13Z)- and (3E,13Z)-3,13-octadecadien-1-yl acetate. A presently preferred process is where m is 2, n is 9, p is 4, R 1 is tetrahydropyranyl, R 2 is hydrogen, and R 3 and R 4 are phenyl.
By substituting 5-hydroxypentyldiphenylphosphine for 4-hydroxybutyldiphenylphosphine oxide as in Example 1, 6-(2-tetrahydropyranyloxy)hexanal for 7-(2-tetrahydropyranyloxy)heptanal in Example 2, and using n-valeraldehyde as in Example 3, there is obtained (6Z,11Z)- and (6Z,11E)-6,11-hexadecadien-1-yl acetate. A presently preferred process is where m is 5, n is 4, p is 4, R 1 is tetrahydropyranal, R 2 is hydrogen, and R 3 and R 4 are phenyl.
The products of Example 2 or the final products of Example 3 are equilibrated by standard techniques to produce a mixture of stereochemical isomers which are then separated by chromatography (including thin layer or gas-liquid high pressure liquid chromatography) and or fractional distillation.
The present invention has been described with reference to the specific embodiments thereof, it should, however, be noted and understood by those skilled in this art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention. Further, many modifications may be made to adapt a particular situation, material, or composition of matter, process, process step or steps, or then-present objective to the spirit of this invention without departing from its essential teachings.
|
This process relates to the synthesis of unsaturated aliphatic esters useful as insect sex attractants, including gossyplure, the insect sex pheromone of the pink bollworm moth, Pectinophora gossypiella, and intermediates therefor. The process utilizes a cyclic phosphonium (Wittig) reagent.
| 2
|
CROSS-REFERENCE TO RELATED APPLICATION
This is a continuation, of application Ser. No. 360,837, filed May 16, 1973, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The subject invention relates to a decorative surface covering.
2. Description of the Prior Art
The use of felt backings for floor coverings is well known. Conventionally resilient thermoplastic decorative floor coverings have been backed with flooring felts of several types. In order to provide more resiliency underfoot, a foamed vinyl or rubber layer have been incorporated in products, either as a backing replacing the felt, as an integral part of the decorative layer itself or as underlayments. In addition, it is known from U.S. Pat. No. 3,490,985 to decorate a glass fabric with a plastisol which may be expanded by using any suitable blowing agent. It is also known from U.S. Pat. No. 2,920,977 to print decorative designs in such a way that some of the elements are foamed, whereas others are of an unfoamed structure.
SUMMARY OF THE INVENTION
Our invention is concerned with the production of a resilient decorative thermoplastic sheet material which also embodies an element in its structure to give an added degree of resiliency. This is achieved by utilizing, as a backing web for the decorative vinyl wear layer, a non-woven, needle-punched mat of fibers which is reinforced with a dimensionally stable scrim. This needle-punched web, which is lofty and resilient, is bonded throughout by a latex binder.
The latex saturated needle-punched web is decorated by printing with non-foamable and/or foamable plastisol inks on a rotary screen printer to form the desired design on the face of the backing web and this layer is then simultaneously pressed and gelled by passing the printed web through a heated laminator whereby a planished, continuous, decorative, gelled layer is formed which is embedded firmly in the needle-punched web with the surface fibers being locked therein. A thin nonporous plastisol clear coat is then applied, and the coated fabric is passed through an oven where the decorative and wear coatings are fused and any design elements formed of foamable material are foamed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic illustration of the process of preparing the decorative sheet material in accordance with our invention;
FIG. 2 is a cross-sectional view illustrating a typical sheet produced in accordance with our invention; and
FIG. 3 is a typical nomograph used in determining a cushioning index.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
To form the needle-punched backing mat or web, a woven glass scrim or other dimensionally stable woven or non-woven scrim is sandwiched between two non-woven webs of synthetic organic fibers and the sandwich construction is needle-punched using a conventional needle loom and providing between about 200 and 300 penetrations per square inch. Generally, the needle penetrations are to a depth of at least 1/4 inch and may pass through the web. Any organic fibers having deniers of from about 3 to 40, preferably between about 5 and 17; lengths of 11/2 to 6 inches, preferably between about 2 and 3 inches; and melting points in excess of about 280° F. may be used in the non-woven webs. Using non-woven webs which together with the scrim have a total weight of from approximately 4 to about 20 ounces and typically between 9 and 11 ounces forms a backing giving the required degree of resiliency underfoot to the finished product.
Among the synthetic organic fibers which may be used in forming the non-woven webs are staple fibers formed of polyester, acrylic, acetate, rayon or nylon.
The needle-bonded backing is then saturated with a latex solution by conventional methods such as spraying the latex onto the web or using a waterfall technique. The saturated web is then dried using steam-heated drums, can driers, or an air impingement oven. Pressing may be done as desired.
Conventional water emulsion latexes, many of which are readily available commercially, may be used. By way of example, acrylic water emulsions such as Rhoplex HA8 (Rohm and Haas) or a stabilized poly(vinyl chloride) water emulsion work well, the only criterior being that the latex should have a heat stability greater than about 280° F. Generally speaking, a weight pickup of 3 to 30 percent based on the weight of the needled backing web is sufficient to form a well-bonded backing.
The needle-bonded mat or web forms the carrier for the decorative wear layers. The decorative wear layer is applied by means of a conventional rotary screen printer, such as a Zimmer printer, utilizing foamable or non-foamable plastisol inks applied by means of, for example, 40 to 60 mesh pattern screens and 11/8 inch steel ruled rods or foam-covered rods in the printing cylinders. A series of designs is laid down on the web by a successive number of screens to form an aesthetic design of the desired configuration. One may form all of the design elements utilizing conventional non-foamable plastisol inks, or one may, if desired, form elements in the overall design with foamable plastisol inks or any combination thereof.
A preliminary coat, if desired, is also applied at the printer using a non-patterned 40 mesh screen with a 3/4 inch steel squeegee rod prior to printing the design. The plastisol layer or layers are then gelled by contact with a steam-heated (280° F.) laminator roll with a sufficient wrap to provide a 3 to 10 second contact time. The roll also acts to smooth and close the face preparatory to application of a subsequent wear layer coating. Generally speaking, application rates for the first coat of 5 to 10 ounces of plastisol per square yard and for the decorative layer of 8 to 30 ounces of plastisol per square yard form a decorative layer of the desired structure.
The mat with the faced print surface is then coated with 5 to 20 mils of clear plastisol using a reverse roll coater. The coating is cured and the inks forming the decorative layer fused in a hot-air impingement oven and, in those instances where foamable inks are used for some or all of the design elements, the curing and fusion is accompanied by expansion of the foamable inks. No subsequent facing or embossing is required, and the resultant product has a closed face with a textured surface as well as a pattern emboss if a combination of foamable and nonfoamable inks is used. Of course, if desired, the fused decorative wear layer construction may be embossed in a separate operation before or after the clear coat application.
The following example will serve to illustrate this invention:
EXAMPLE 1
Preparation of Carrier
A needled web was formed by needling two non-woven webs formed of crimped polyester fibers (Avlin 101-FMC Corp.) of 6 denier and about 21/2 inches in length, into a woven glass fiber scrim sandwiched therebetween using a conventional needle loom with 294 needle penetrations per square inch. The fiber web weight for the needle-punched backing thus formed was 8 ounces per square yard. The needle-punched web was then saturated by spraying on a latex binder of the following formulation to a weight pickup of solids of about 10 percent by weight of the web and the web pressed and dried in a conventional air impingement oven at about 300° F.
______________________________________Latex for Web Saturation Parts By Weight______________________________________Acrylic Emulsion (Rohm & Haas Rhoplex 20.9 HA8) 45% Solids in WaterWater 23.9Ammonium Chloride (Rohm & Haas Catalyst A) 0.05Fatty Acid Type Defoamer (Nopco NDW) 0.1Alkyl Aryl Ether Surfactant (Triton CF10) 0.1______________________________________
Pattern Formation
With reference to FIG. 1 of the drawings which diagrammatically illustrates the formation of a resilient decorative floor covering in accordance with this invention, a latex-bonded needle-punched web 7 produced as above described is unwound at 5 and passed over an idler roll 6. A preliminary coat was first applied by the first printing screen of a Zimmer Rotary Printer indicated by the box 8 using a non-patterned 40 mesh screen with a 3/4 inch steel squeegee rod. The backing web 7 is then decorated by printing a pattern with foamable and non-foamable plastisol inks on the Zimmer Rotary Screen Printer 8 using a series of 40 to 60 mesh screens with 11/8 inch steel rods positioned in the screens. The first screen provides a continuous coat of about 9 ounces per square yard and the initial design print coat is approxiamtely 12 ounces per square yard. The screens are so patterned as to give a design covering the surface of the carrier web 7. The preliminary and design coats are gelled by passing between heated laminating rolls 9 and by contact through a 90° wrap with one of the heated (280° F.) laminating rolls 9 for 6 seconds. The laminating rolls 9 also act to smooth and close the printed decorative facing layer for subsequent coating. The following formulations are utilized for the inks and clear coatings:
Plastisol Ink - Foamable Parts By WeightPoly(Vinyl Chloride) Homopolymer Resin 50.0 Exon 605Poly(Vinyl Chloride) Homopolymer Resin 50.0 Geon 124DOP Di-2-Ethyl Hexyl Phthalate 33.8TXIB Texanol Isobutyrate 16.9Ferro 5245 Stabilizer (Ba-Cd Type) 2.5Kempore SD60 (Azodicarbonamide Paste) 12.0Cab-O-Sil -- Silica Thickener 0.63Pigment (as desired)Plastisol Ink - Non-Foamable Parts By WeightPoly(Vinyl Chloride) Homopolymer Resin 50.0 Tenneco 1732Poly(Vinyl Chloride) Homopolymer Resin 50.0 Exon 654DOP Plasticizer 41.6TXIB Plasticizer 15.8Ferro 5245 Stabilizer 2.0Drapex 4.4 Epoxy Stabilizer 5.8Cab-O-Sil Thickener 0.36Pigment (as desired)Plastisol Clear Coat Parts By WeightPoly(Vinyl Chloride) Homopolymer Resin 50.0 Exon 605Poly(Vinyl Chloride) Homopolymer Resin 50.0 Blacar 1732DOP Plasticizer 37.5TXIB Plasticizer 23.9Mark 275 Tin Stabilizer 2.9Atlas G695 Surfactant -- Thickener 0.75Cab-O-Sil Thickener 0.63
The mat with the faced, printed surface is then passed over an idler roll 10 and coated with 10-12 mils of clear plastisol of the above formulation utilizing a reverse roll coater 11. All of the coatings are then cured, accompanied by expansion of the foamable inks, in a hot-air impingement oven 12 (at 410° F.). Dwell time in the oven is approximately 1.5 to 2 minutes. No subsequent facing or embossing is required, although a subsequent embossing of the fused product could be utilized if desired. The resultant product, as shown in cross section in FIG. 2, has a closed face with a textured surface as well as a pattern emboss resulting from the use of the combination of foamable and non-foamable inks.
The use of foamable inks in the practice of this invention is, of course, optional and some texture is attained where only non-foamable inks are utilized due to the texture of the needle-punched carrier. Design elements may be formed from clear or transluscent inks, in which case the needle-punched backing may be visible, or of opaque inks which would completely hide the backing. The ink formulations set forth above are clear formulations to which desired pigments are added to give opaque or transluscent characteristics to selected printed elements.
EXAMPLES 2-5
In order to evaluate the relative resiliency of products produced in accordance with this invention, a series of needle-punched reinforced backing webs of 4, 8, 12 and 16 ounces, respectively, were produced. Each of the backing webs was saturated (10 percent solids) with a latex of the following formulation and dried:
Latex for Web Saturation Parts By Weight______________________________________Acrylic Emulsion (Rohm & Haas Rhoplex 15.0 HA24) 44.5% Solids in WaterAcrylic Emulsion (Rohm & Haas Rhoplex 15.0 TR-407) 45.5% Solids in WaterWater 90.0Ammonium Chloride (Rohm & Haas Catalyst A) .03Fatty Acid Type Defoamer (Nopco NDW) .01Dioctyl Sodium Sulfosuccinate (Triton GR-5) .03______________________________________
The saturated webs were first printed with a continuous plastisol coat (9 ounces per square yard) of the following formulation:
Parts By WeightBlacar 1732 Poly(Vinyl Chloride) Homo- 57.14 polymer ResinBorden UC-285 PVC Copolymer Resin 42.85DOP Plasticizer 33.67TXIB Texanol Isobutyrate Plasticizer 10.36Ferro 5245 Stabilizer 2.50Drapex 4.4 Epoxy Stabilizer 5.00Cab-O-Sil .66Pigment (as desired)
A second continuous coat (12 ounces per square yard) was applied using a foamable plastisol of the following formulation:
Parts By WeightExon 605 Poly(Vinyl Chloride) Homo- 37.99 polymer ResinSCC-20 PVC Homopolymer Resin 36.52M-70 Homopolymer Blending Resin 25.57DOP Di-2-Ethyl Hexyl Phthalate Plasticizer 53.11Drapex 4.4 Epoxy Stabilizer .99Ferro 5245 Stabilizer (Ba-Cd Type) 1.99Kempore AF (Azodicarbonamide) 2.41Cab-O-Sil Silica Thickener .60Pigment (as desired)
These coats were then gelled by passing the coated webs between heating laminating rolls (280° F.) and by contact for about 6 seconds with one of the heated rolls. A plastisol clear coat of about 10 mils was applied with a reverse roll coater. The clear coat was of the following formulation:
Parts By WeightBlacar 1738 Poly(Vinyl Chloride) Homo- 44.89 polymer ResinExon 6337 Poly(Vinyl Chloride) Homo- 14.86 polymer ResinTenneco 501 Homopolymer Blending Resin 40.24DOP Plasticizer 17.46Santicizer 160 (Butyl Benzyl Phthalate 7.92 Plasticizer)Drapex 4.4 Stabilizer .99Nuodex U-1366 Stabilizer 2.97TXIB Plasticizer 14.86Tinopal SFG .005
All of the coatings were then cured accompanied by expansion of the foamable layer in a hot-air impingement oven (410° F.) with a dwell time of about 1.5 minutes.
The thus prepared products were then subjected to test procedures to determine their cushioning index under standard conditions and to compare these values with values for conventional floor products commercially available.
A special Cushioning Test Apparatus was utilized for all tests reported below and comprised a Storage oscilloscope, cathode follower, a dropping device consisting of a steel cylinder projectile with one end slightly rounded (3 inch radius of curvature) weighing 357 grams, a Columbia Research Laboratory Accelerometer (Ser. No. 1432) attached to the projectile and a clear acrylic tube provided with slotted openings to provide guidance, a solid steel substrate on which the specimen is positioned, and an electromagnet to hold the projectile unitl release. Necessary interconnecting cables and an aluminum base section designed to support the assembly are provided.
To determine the Cushioning Index of the products, a specimen is placed on the steel substrate and the projectile released by cutting power to the electromagnet. The projectile is allowed to freely fall a prescribed drop height of 1.75 inches and squarely strike the specimen with the rounded end. The impact signal is picked up by the accelerometer and fed to the cathode follower and, in turn, relayed to the Storage oscilloscope screen which is set for a single sweep operation (rebounds are not indicated). The values of peak acceleration and time to peak acceleration are taken from the oscillogram and plotted on a nomograph so the cushioning index can be read off when the peak acceleration and time to peak acceleration are known. FIG. 3 of the drawings shows a nomograph with the sample line plotted for the specimen having a 12 ounce per square yard needle-punched web backing.
The cushioning index for each of the floor products produced as above described are set forth in Table I.
Table I______________________________________ Time CushioningMaterial Acceleration (Milliseconds) Index______________________________________4 oz. backing 190.00 .75 4.78 oz. backing 108.00 2.00 18.712 oz. backing 60.00 2.50 34.216 oz. backing 80.00 2.00 23.8______________________________________
A standard vinyl composition sheet flooring (60 mil fused vinyl composition wear layer bonded to a rubber saturated asbestos fiber felt) and a standard linoleum sheet flooring (50 mil cured linoleum wear layer bonded to a 40 mil drying oil saturated cellulosic fiber felt) had cushioning indexes of between about 1.1 and 1.5 when tested as above described. A 15.36 ounce per square yard non-woven needle-punched polypropylene fiber carpet reinforced with a polypropylene scrim had a cushioning index of about 25.9. Foamed rotovinyl sheet flooring products (10 mil clear coat, 30 to 35 mil foamed layer and 30 mil rubber saturated asbestos fiber felt backing) had cushioning indexes of from 2.8 to about 6. Another cushioned flooring (40 mil fused vinyl composition wear layer reinforced with a saturated woven fiber glass scrim and bonded to a 125 mil cellular vinyl composition backing) had a cushioning index of between about 21.9 and 29.5.
As shown by the above, the decorative surface coverings produced in accordance with this invention may be designed so as to have superior cushioning properties or properties comparing favorably to commercially available sheet vinyl composition flooring and to the cushioning properties of non-woven needle-punched carpets.
|
A non-woven fabric floor having the desirable attributes of a non-woven carpet construction combined with the desirable attributes of a decorative thermoplastic surface covering and a method for its production are described.
| 3
|
FIELD OF THE INVENTION
[0001] The invention relates to devices for measuring flow parameters of fluid (oil, water, gas and mixtures thereof) such as temperature, velocity and gas composition, and can be used in geophysical studies of boreholes as well as in monitoring transportation of liquid hydrocarbons through a pipeline system.
BACKGROUND ART
[0002] It is known a downhole hot-wire thermoanemometer disclosed in SU 440,484. The thermoanemometer comprises a sealed housing made as two cavities one of which contains a heating element arranged therein while another one contains a thermosensitive element arranged therein.
[0003] The disadvantages of the known thermoanemometer are:
there is no way to measure a temperature and a velocity of a fluid flow simultaneously, because the thermosensitive element measures the temperature only when the heater is turned off; switching into a fluid temperature measurement mode requires a certain amount of time during which the heater will get cold and will not have an influence upon operation of the thermosensitive element, wherein the fluid temperature and composition can be much different from the initial values, which situation affects the reliability of received information; the fluid flow velocity is calculated according to the complicated algorithm with taking into account a mass flow rate of the fluid and thermophysical properties thereof; the monitoring of the fluid composition is absent.
[0008] Also known is a downhole sensor disclosed in SU 2,384,699. The sensor comprises an electrical insulator and a hollow cylindrical metal housing with a thermoanemometer sensor arranged in a cavity thereof.
[0009] The disadvantages of the prior art sensor are:
there is no way to measure a temperature and a velocity of a fluid flow simultaneously, because the temperature is measured only when the thermoanemometer heater is turned off; the switching into a fluid temperature measurement mode requires a certain amount of time during which the heater will get cold and will not have an influence upon operation of the thermosensitive element, wherein the fluid temperature and composition can be much different from the initial values, which situation affects the reliability of received information; the presence of a dielectric layer on the external surface of the hollow cylindrical housing of the thermoanemometer, said layer having an essential influence upon the heat exchange between the housing and the fluid, as a consequence of which metrological characteristics of the thermoanemometer deteriorate.
SUMMARY
[0013] The disclosure provides for enhanced functionality of the sensor and increased measurement efficiency.
[0014] A downhole sensor comprises a hollow metal housing opened at one end and having a thermoanemometer sensor arranged in a cavity thereof, an electrical insulator, a second hollow housing opened at one end, identical to the first housing and having a second thermoanemometer sensor arranged in a cavity thereof. At the same time, symmetry axes of the housings are aligned, open ends of the housings face each other and are rigidly fastened in the electrical insulator and electrical leads of the sensors are within the cavities of the housings and extend outside through the electrical insulator.
[0015] The electrical insulator can be coated with a dielectric layer and also can have a shape which provides minimal flow structure distortion. The sensor housings also can be embodied so as to provide minimal flow structure distortions, for example, as a cylinder or a cone.
BRIEF DESCRIPTION OF DRAWINGS
[0016] The invention is illustrated with the drawing where FIG. 1 shows a downhole sensor of the invention.
DETAILED DESCRIPTION
[0017] The downhole sensor comprises a first hollow metal housing 1 having a thermoanemometer sensor 2 arranged in a cavity thereof and a second hollow housing 3 having a thermoanemometer sensor 4 arranged in a cavity thereof. Symmetry axes of the housings 1 and 3 are on one line O-O, the sensor housings are electrically insulated from each other by an electrical insulator 5 and are rigidly terminated therein from sides of open ends. The metal housings 1 and 3 of the thermoanemometer sensors to inner surfaces of which electrical leads 6 and 7 are connected are electrodes of a fluid composition resistive sensor. The thermoanemometer sensor 2 as well as the sensor 4 consists of a heating element and a temperature sensor (not shown in the drawing), has a thermal contact with an inner surface of a respective hollow metal housing and is electrically insulated therefrom. The heating element and the temperature sensor are electrically insulated from each other as well. Such sensors are described, for example in “Skvazninny termoconductivny debitometer STD” (Downhole Thermodonductive Flowmeter DTF). I. G. Zhuvagin, S. G. Komarov, V. B. Cherny.—“Nedra” (Depths Publishers), or in “Geofizicheskie issledovania skvazhin: spravochnik mastera po promyslovoi geofizike” (Geophysical Studies of Boreholes: Oilfield Geophysics Handbook of Foreman)/Under the general editorship of V. G. Martynov, N. E. Lazutkina, M. S. Khokhlova.—Moscow: “Infrainzheneria” (Infra-Engineering Publishers), 2009.
[0018] The electrical leads of the sensors 2 and 4 pass within the cavities of the respective housings, extend outside through the electrical insulator 5 and are coupled to an electronic unit (not shown in the drawing). To improve moisture resistance and chemical resistance, the electrical insulator can be coated with an additional dielectric layer (not shown in the drawing), while a the insulator and the housings 1 and 3 can have a shape providing minimum distortions into the flow structure, for example, the shape of a cylinder or a cone.
[0019] The downhole sensor operates as follows.
[0020] The downhole sensor is placed in a borehole so that an axis of the sensors coincides with an axis of the borehole, the sensor 2 is directed towards a dib hole while the sensor 4 is directed towards a borehole mouth. Depending upon a direction of the fluid flow and/or a direction of a downhole sensor movement relative to the flow (round-trip operations in the borehole), it is possible to use the sensor 2 and the sensor 4 in a flow temperature measurement mode or in a flow velocity measurement mode. When lowering the downhole sensor into the borehole or in a static position of the downhole sensor if the fluid flow is directed toward the housing 1 , the thermoanemometer sensor 2 is used in the temperature measurement mode while the sensor 4 is used in the flow velocity measurement mode. In this case, the heating element of the sensor 2 is turned off and only its thermosensitive element operates, while the heating and thermosensitive elements of the thermoanemometer sensor 4 operate, and heat generated by the heating element of the sensor 4 has no affects on operation of the thermosensitive element of the sensor 2 . Simultaneously, a fluid composition is determined according to a change in an electrical conductance of the fluid between the housings 1 and 3 of the thermoanemometer sensors (cf., “Geofizicheskie issledovania skvazhin: spravochnik mastera po promyslovoi geofizike”/Under the general editorship of V. G. Martynov, N. E. Lazutkina, M. S. Khokhlova.—Moscow: “Infrainzheneria” (Infra-Engineering Publishers), 2009).
[0021] If a change in a direction of the flow takes place, i.e., the device is lifted, or if the borehole operates in an injection mode when the flow is directed towards the housing 3 , the thermoanemometer sensor 4 is used in the temperature measurement mode while the thermoanemometer sensor 2 is used in the flow velocity measurement mode. In this case, the heating element of the sensor 4 is turned off and only its thermosensitive element operates, while both the heating and thermosensitive elements of the sensor 2 operate, and heat generated by the heating element of the sensor 2 has no affects on operation of the thermosensitive element of the sensor 4 .
[0022] The sensor is used in a similar way to measure a temperature, a speed and a phase composition of a multi-phase flow (oil, water, gas and mixtures thereof) in pipelines. The downhole sensor is placed in a pipe so that the axis of the sensors coincides with an axis of the pipe, wherein the sensor 2 and the sensor 4 are directed oppositely to each other. Depending upon a direction of the fluid flow, it is possible to use the sensor 2 and the sensor 4 in the flow temperature measurement mode or in the flow velocity measurement mode. In case if the fluid flow is directed towards the housing 1 , the thermoanemometer sensor 2 is used in the temperature measurement mode while the sensor 4 is used in the flow velocity measurement mode. In this case, the heating element of the sensor 2 is turned off and only its thermosensitive element operates, while both the heating and thermosensitive elements of the sensor 4 operate, and heat generated by the heating element of the sensor 4 has no affects on operation of the thermosensitive element of the sensor 2 . Simultaneously, a fluid composition is determined in accordance with a change in an electrical conductance of the fluid between the housings 1 and 3 of the thermoanemometer sensors.
[0023] If a change in a direction of the flow takes place, i.e., when the flow is directed towards the housing 3 , the thermoanemometer sensor 4 is used in the temperature measurement mode while the thermoanemometer sensor 2 is used in the flow velocity measurement mode. In this case, the heating element of the sensor 4 is turned off and only its thermosensitive element operates, while both the heating and thermosensitive elements of the sensor 2 operate, and heat generated by the heating element of the sensor 2 has no affects on operation of the thermosensitive element of the sensor 4 .
[0024] Each sensor is switched from the temperature measurement mode to the velocity measurement mode by a command received from the electronic unit.
[0025] The fluid temperature, velocity, and composition are determined from results of the preliminary calibration of respective sensors. Calibration data is stored in memory elements of the electronic unit.
[0026] The alternative use of the thermoanemometer sensors in active and passive modes allow determination of a flow direction. For example, the thermoanemometer sensor 4 is first used in the passive temperature measurement mode (the heating member of the sensor 4 is turned off and only its thermosensitive element operates) while the thermoanemometer sensor 2 is used in the active measurement mode (the heating and thermosensitive elements are operated in the sensor 2 . A temperature difference ΔT 1 between readings of the sensor 2 and the sensor 4 is recorded. Next, on the contrary, the thermoanemometer sensor 4 is used in the active temperature measurement mode while the thermoanemometer sensor 2 is used in the passive temperature measurement mode. A temperature difference ΔT 2 between readings of the sensor 2 and the sensor 4 is recorded. If the value ΔT 1 in modulus is larger than the value ΔT 2 in modulus, then the flow is directed towards the housing 3 . If the value ΔT 1 in modulus is smaller than the value ΔT 2 in modulus, then the flow is directed towards the housing 1 .
[0027] Use of two thermoanemometers, apart from their direct purpose, for determination of a fluid composition as well widens the functionality of the inventive downhole sensor, while localization of the fluid temperature, velocity, and composition sensors in a single low-volume module enhances the reliability of resulted information directly in a measurement point in real-time mode.
|
The downhole sensor is intended for measuring fluid flow parameters. It comprises two identical hollow metal housings opened at one end, whose symmetry axes are aligned. The open ends of the housings face each other and are rigidly fastened in the electrical insulator. A thermoanemometer sensor is arranged in each housing. Electrical leads of the sensors are within the cavities of the housings and extend outside through the electrical insulator.
| 4
|
This is a continuation of application Ser. No. 07/266,201 filed Oct. 27, 1988 now abandoned, which is a continuation of Ser. No. 913,688, filed Sept. 30, 1986 now abandoned.
FIELD OF THE INVENTION
This invention relates to a pressure-sensitive adhesive film article. In particular, this invention relates to an article comprising a film of pressure-sensitive adhesive, which article is useful in the moist healing of wounds.
BACKGROUND OF THE INVENTION
In recent years, the technique of wound repair known as moist healing has become well established. It is an improvement in many cases over the traditional method of letting a wound dry out, forming a scab or crust over the surface, followed by regrowth of tissue underneath the scab. It has been found that, relative to dry healing, moist healing often results in cleaner repair, with less scarring and less pain to the patient than dry healing, especially when the wound is an extensive burn or large abrasion. Dressings for moist healing therapy are frequently made of thin films of synthetic polymers such as polyurethanes as described in U.S. Pat. No. 3,645,835. One of the characteristics of these films is their ability to selectively allow water molecules ("moisture vapor") to pass through them while preventing the passage of liquid water or aqueous solutions and, most importantly, bacteria. By careful selection of film and adhesive, a dressing can be provided which keeps a wound moist and sterile, but which allows excess liquid to evaporate. It also conforms well to the skin, and is unobtrusive in use.
Such dressings, however, have several disadvantages when used with certain kinds of wounds. When a wound is seeping copiously the "moisture vapor transmission" (MVT) capability of the film cannot remove excess liquid fast enough. As a result, fluid may accumulate under the dressing which can result in skin maceration. In practice, a film of sufficiently high MVT to be useful as a dressing on highly exudative wounds would have to be too thin to be practical. Even film dressings in commercial use today are so thin and flimsy that they are extremely difficult to apply without special delivery means such as those described in U.S. Pat. Nos. 4,513,739, 4,598,004 and Canadian Patent No. 1,192,825.
The problem of handling copiously-seeping wounds was addressed in U.S. Pat. No. 4,499,896 by providing a reservoir dressing with one or more extra layers of thin film, sealed together at their peripheries, to form pouches into which excess liquid can flow temporarily. These pouches or reservoirs have additional surface area through which moisture evaporation can take place. These dressings have found utility, but are clearly more complicated and costly than dressings made from a single film.
Another disadvantage of conventional thin film dressings is that they provide very little mechanical cushioning to a wound. Wound protection against bumps and scrapes is not addressed by these thin dressings.
Foam backings for wound dressings are known (e.g. Microfoam™ brand surgical tape, 3M Co.) where the foam provides a thicker, more conformable, more cushioning material than would be provided by the same weight of unfoamed backing. The backing of Microfoam™ brand surgical tape is open cell polyvinylchloride which is not a barrier for micro organisims. If the polyvinylchloride was made with closed cells, it would not have a sufficiently high MVT for moist wound healing without skin maceration.
U.S. Pat. No. 4,559,938 (Metcalfe) discloses an adhesive dressing comprised of a backing and a conventional pressure-sensitive adhesive. The backing is a film formed from a blend of a continuous matrix of 1,2-polybutadiene and an incompatible polymer which forms a discrete particulate phase within the matrix. This film is stretched to introduce a plurality of small, preferably closed, voids in the film which nominally enhance the moisture vapor permeability of the film. It is believed that the moisture vapor permeability of the dressing (through film and adhesive) is too low to be used in moist wound healing without skin maceration.
Thus, there exists a need for a wound dressing which provides controlled transmission and/or absorption of water vapor away from a wound so that the wound remains moist but not excessively so, and which is also thick and flexible enough to alleviate the need for elaborate delivery means and to provide mechanical cushioning of a wound.
SUMMARY OF THE INVENTION
According to the present invention, there is provided a pressure-sensitive adhesive article for use on skin comprising a continuous film of pressure-sensitive adhesive having dispersed therein a discontinuous gaseous phase contained within voids within said film, which gaseous phase constitutes at least 10 percent of the volume of said pressure-sensitive adhesive. The film has a moisture vapor transmission and absorbency sufficient to permit moist healing of wounded skin without skin maceration, e.g., an MVT of at least about 400 g/m 2 per 24 hours measured at 40° C. and 80% relative humidity differential.
The adhesive film of the invention has cellular voids containing a gaseous phase to effect control of adhesive thickness and to provide a multiplicity of microreservoirs or micropouches. The film allows water vapor to pass at a controlled rate by diffusion of water vapor through the adhesive surrounding the voids and collection of water vapor in the voids, but prevents liquid media (e.g., water) and bacteria from traversing the film. This controlled diffusion of water vapor allows for the presence of an optimal amount of moisture at the site of a healing wound covered by the film. The cellular construction of the film also provides mechanical cushioning of the wound.
In a preferred embodiment of the adhesive article of the invention, a film of cellular pressure-sensitive adhesive is in contact with one face of a conformable sheet. The conformable sheet preferably has high moisture vapor transmission i.e., at least about 1000 g/m 2 per 24 hrs at 40° C. and 80% humidity differential.
Another aspect of this invention relates to a method of preparing a pressure-sensitive adhesive article as described above comprising:
(a) forming a hydrophilic polymerizable composition which polymerizes to a pressure-sensitive adhesive state;
(b) foaming said composition;
(c) coating a carrier with said foamed composition; and
(d) polymerizing said coating to a pressure-sensitive adhesive state.
The hydrophilicity of the polymerizable composition may be provided by the inclusion of: (1) a hydrophilic, ethylenically unsaturated monomer, e.g., acrylic acid or an acrylate or acrylamide terminated polyether; (2) by a hydrophilic additive, e.g., a polyhydric polyol, or polyether; or (3) both a hydrophilic monomer and a hydrophilic additive. The degree of hydrophilicity required of the polymerizable composition is that degree which is sufficient to provide a pressure-sensitive adhesive having the desired degree of moisture vapor transmission.
DETAILED DESCRIPTION
The pressure-sensitive adhesive films of this invention must have a sufficiently high moisture vapor transmission and absorbency to permit moist healing of a wound without skin maceration. Moist healing is the retention at a wound of an optimum amount of moisture which (1) prevents the formation of a scab, (2) increases the rate of epithelial cell migration, and (3) does not allow pooling of moisture or wound exudate. Skin maceration is a deleterious effect of pooling of excess liquid, e.g., water or bodily fluid, on the normal skin surrounding a wound. Skin maceration is indicated by whitening and softening of the affected skin. In general, adhesive films of this invention having a moisture vapor transmission of at least about 400 g/m 2 per 24 hrs measured at 40° C. and 80% relative humidity differential are sufficiently absorptive and transmissive to avoid skin maceration and promote moist wound healing. The moisture vapor transmission is preferably at least about 500 g/m 2 per 24 hrs., and most preferably from about 600 to about 2400 g/m 2 per 24 hrs. The adhesive film useful in this invention is cellular, i.e., non-porous, such that it possesses substantially total impermeability to liquid water and bacteria.
Moisture vapor transmission as referred to herein and in the claims, except as otherwise noted, refers to moisture vapor permeability determined in accordance with the test described below. Impermeable to liquid water as used herein means impermeable to liquid water as indicated by the dye penetration test described below.
The adhesive film is rendered moisture vapor permeable and absorbent by the hydrophilicity of the adhesive composition and the cellular voids in the film. The thickness of the adhesive film, along with the hydrophilicity and the voids, affects the absorption capacity of the adhesive film. The adhesive film is rendered hydrophilic by the addition of hydrophilizing agents to the polymerizable premix from which the adhesive is prepared such as those described below.
As used herein, "percent void volume" means that portion of the thickness of the cellular adhesive membrane attributable to cellular voids. Percent void volume is conveniently measured by the equation: ##EQU1## wherein d u is the unfoamed density and d f is the foamed density of the adhesive. Unfoamed density can be determined from the density of the starting materials or by compressing the foamed adhesive. Adhesive films according to the invention should have void volumes of from about 10 to about 85 percent. The higher the void volume of the adhesive film, the greater the MVT, absorbency, conformability, and cushioning ability of the dressing.
The adhesive films of this invention possess useful absorbency in addition to their ability to transmit water vapor. When the film is composed of an adhesive having low absorbency, the difference in absorbency between the foamed state and the unfoamed is pronounced (See Examples 1-6). This effect is less pronounced in the case of adhesives which are already highly absorbent, but in both cases the end product has the ability to absorb significant quantities of water. The water is not easily removable from the foam by squeezing. This is a useful distinction from conventional reservoir dressings used on highly exudative wounds, wherein the contents of the reservoirs may leak out when the dressing is manipulated.
Also, typical pressure-sensitive adhesive films of the invention have remarkably good flexibility and conformability which are advantageous properties in a wound dressing.
The pressure-sensitive adhesive films of the invention are derived from a hydrophilic polymerizable premix into which cellular voids are introduced. The premix is made hydrophilic by the addition of a hydrophilizing agent such as a hydrophilic, ethylenically unsaturated monomer, a hydrophilic additive or both. Preferred hydrophilic additives are polyhydric alcohols, polyethers, or mixtures thereof. The polyhydric alcohol or polyether is present in the premix in an amount sufficient to raise the moisture vapor transmission of the adhesive to the desired level This amount ranges, in general, from about 20 to about 85 parts by weight of the premix, with about 30 to about 70 being preferred. Examples of useful polyhydric alcohols and polyethers include glycerin, propylene glycol, polypropylene oxide glycols, polyethylene oxide glycols, 1,2,4-butanetriol, and sorbitol and mixtures thereof. The dihydric alcohol, ethylene glycol is useful in the present invention, but may cause dermal reactions which limit its utility.
The hydrophilizing agent may also have ethylenic unsaturation which will allow it to copolymerize with other free radically polymerizable materials in the premix as described below. For example, a polyether polyol can be terminated with acrylic or methacrylic acid, or a reactive derivative thereof, to yield an acrylate or methacrylate terminated polyether, e.g., poly(oxyethylene)acrylate. Also, an amine terminated polyether can be terminated with acrylic or methacrylic acid, or a reactive derivative thereof, to yield an acrylamide or methacrylamide terminated polyether, e.g, N-poly(oxypropylene)acrylamide.
The premix is also comprised of an unsaturated free radically polymerizable material which when polymerized renders the premix pressure-sensitive adhesive, and which is preferably miscible with the hydrophilizing agent. This material may consist of a single monomer or a mixture of comonomers. These monomers or comonomers are present in the premix in amounts of from about 100 to about 10 parts by weight of the premix preferably from about 50 to about 20. Examples of useful monomers or comonomers are alkyl acrylates having an average of 4-12 carbon atoms in their alkyl groups, acrylic acid, methacrylic acid, and salts thereof, acrylamide, methacrylamide, hydroxyalkylacrylates, hydroxyalkylmethacrylates, acrylonitrile, methacrylonitrile, cyanoethylacrylate, maleic anhydride and N-vinyl pyrrolidone.
It is preferred that the premix contain a plasticizing component which is conveniently provided by the polyether or polyol hydrophilic additive or the polyether- or polyol-containing monomer.
The premix is also preferably comprised of a thickening agent of polymeric material which is preferably soluble in the polymerizable composition. These polymeric materials are present in the premix in amounts of about 0.1 to about 70 parts by weight of the premix. Examples of useful polymeric materials are sodium carboxymethyl cellulose, hydroxyethylcellulose, methoxyethyl cellulose, chitosan, polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid, polyvinylethers, copolymers of maleic anhydride and polyvinylethers, starch, hydroxypropyl-cellulose, polyacrylamide, copolymers of alkyl acrylates and acrylic acid or its salts, polyethylenimine, ethylene oxide polymers and propylene oxide polymers.
The adhesive film is preferably crosslinked. One means of crosslinking is the inclusion of a multi-ethylenically unsaturated, free radically polymerizable material, generally in an amount of from about 0.1 to about 5 parts by weight per 100 parts of the polymerizable materials in the premix. Examples are triethylene glycol-bis-acrylate, triethylene glycol bis-methacrylate, ethylene glycol-bis-acrylate, ethylene, glycol-bis-methacrylate, and methylene-bis-acrylamide. These multi-ethylenically unsaturated, free radically polymerizable materials crosslink the polymeric material. Other means of crosslinking include crosslinking the polymer with radiation, e.g., E-beam.
Polymerization of the premix is carried out using conventional methods, e.g. ultra-violet radiation, heat, E-beam and the like. Polymerization by ultra-violet radiation or heat is facilitated by the presence of a free radical initiator which is soluble in the polymerizable composition. The initiator is generally present in an amount of at least about 0.01 parts by weight per 100 parts of the polymerizable materials in the premix. Examples of useful thermal initiators are benzoyl peroxide, azobisisobutyronitrile, di-t-butyl peroxide, and cumyl peroxide. Examples of useful photoinitiators are disclosed in the article "Photoinitiators--An Overview" by G. Berner et al in the Journal of Radiation Curing (April, 1979) pp. 2 through 9. The preferred photoinitiator is benzildimethylketal.
It is often desirable to include a surfactant in the premix, preferably a silicone or fluorochemical surfactant. By doing so, the stability and density of the frothed premix are improved. These surfactants are not always necessary, but when used, are present, as shown in Table III, below, in amounts ranging from 0.5 to 6 parts by weight of the premix. Examples of useful surfactants are described in U.S. Pat. No. 4,415,615. A preferred fluorocarbon surfactant is available under the trade name FC 430, from the 3M Company.
Filler materials can also be incorporated in the premix prior to frothing and coating of the premix or during coating of the premix, the amount of filler being dependent upon the type of filler material being used and the properties desired. Useful filler materials include fibrous reinforcing strands, woven and non-woven reinforcing fabrics, glass beads, plastic hollow microspheres or beads, viscosity-adjusting agents, pigments and absorbent particles. These may be used to enhance the internal strength of the adhesive film or to modify the adhesive and absorbent properties as shown in Example 22, below.
The pressure-sensitive adhesive films of the invention may be prepared by the methods disclosed in U.S. Pat. No. 4,415,615, the disclosure of which is incorporated herein by reference thereto. In general, the process involves the polymerization of a premix containing voids to a pressure-sensitive adhesive state by conventional means. The cellular voids area preferably formed in the premix before coating the premix onto a carrier. The premix can be coated by any suitable means, which will not destroy the cellular voids in the foamed premix.
Absorption capacity, conformability, MVT and cushioning may be controlled by varying the thickness of the adhesive film. Thickness of the adhesive film is determined by the dimensions of the aperture through which the frothed premix passes as it is being coated onto a carrier. Adhesive films having a thickness ranging from about 0.07 to about 1.7 mm are generally suitable. The minimum thickness of the adhesive film is dependent upon the maximum cell size generated in a particular film which is, in turn, determined by the processing conditions and chemical properties of the premix. For example, a surfactant-containing premix would result in an adhesive film with smaller cell diameters and could be coated thinner without the risk of discontinuities than a premix which does not contain surfactant. The maximum thickness is limited by the MVT desired and, as a practical matter, the amount of energy available to effect a complete cure.
An adhesive film of the present invention is preferably made by the sequential steps of:
(1) foaming a premix,
(2) coating the foamed premix onto a carrier, and
(3) polymerizing the coated premix in situ to a pressure-sensitive adhesive state.
Foaming of the premix is conveniently accomplished by whipping a gas, e.g. air, into the premix as disclosed in U.S. Pat. No. 4,415,615. Foaming of the premix could also be accomplished by including a blowing agent in the premix which can be volatilized to produce cellular voids in the adhesive.
Because the viscosity of a mixture of polymerizable monomers tends to be too low to provide a coatable froth or foam, several techniques have been used to thicken the mixtures before frothing or foaming, to provide a composition having a viscosity in the range of 1000 to 40,000 cps. One method is to add thickeners such as those described above to the polymerizable premix. Another method is to thicken the premix with a partially photopolymerized solution or syrup of isooctylacrylate (IOA) and acrylic acid (AA), or IOA and AA in polypropylene glycol.
After coating the foamed composition onto a substrate, the polymerization can be initiated by ultraviolet radiation as taught in U.S. Pat. No. 4,181,752. in situ polymerization can also be effected by electron beam. Because air tends to quench photopolymerization, the foaming gas is preferably inert, such as nitrogen or carbon dioxide.
When the polymerization is to be effected by ultraviolet radiation, the polymerizable coating is preferably protected from air by polymerization in an inert atmosphere or by the use of a plastic film overlay which is fairly transparent to ultraviolet radiation and has a low-adhesion surface. Biaxially-oriented polyethylene terephthalate film which is about 75% transparent to ultraviolet radiation is very useful as an overlay. If the underlying carrier also has a low-adhesion surface, both the carrier and the overlay can be stripped away so that the self-supporting adhesive film may be obtained.
Normally, one does not wish to have an unprotected film of the adhesive at this point in production. In practice, one may either retain the original carrier and overlay or replace one or both (e.g. by lamination) with a liner or backing more suitable for the product. For example, one may wish to use a release liner or a backing bearing a logo, a decorative design, or instructions for use of the product. Ideally, the carrier and the plastic film overlay have sufficiently attractive appearance and properties of low adhesion to the adhesive film that they can be used as protective liners for each face of the adhesive through converting operations and, most preferably, until the final product reaches the hands of the user. For example, when the pressure-sensitive adhesive film is to be used as a means of attaching an ostomy appliance to the skin of a patient, it is desirable to have easy-release liners on each face which are removed sequentially. For example, one might attach the first face of the adhesive to the skin and then an appliance to the second, exposed face of the adhesive.
When the adhesive film is used without a backing, it may be desirable to embed a layer of reinforcing material in the film to structurally support the film. This can be accomplished by coating a carrier with a layer of the polymerizable premix, laying down a layer of reinforcing material, e.g. a fabric, on the coating of premix and coating the exposed layer of reinforcing materials with another portion of polymerizable material. It may be necessary to polymerize the first coating of polymerizable premix before laying down and coating the layer of reinforcing material if the energy used to initiate polymerization radiates from a single source which is not sufficient to completely polymerize the premix throughout its entire thickness.
When making a wound dressing, one face (the skin-contacting side) of the adhesive film is covered with an easy-release liner, which is removed immediately prior to use, but the other face is usually covered with a backing, i.e., a material which reduces or eliminates the tack of that face of the adhesive and which is permanently attached to the adhesive layer. The backing must not reduce the MVT of the dressing below the required level. A number of materials are suitable for this purpose. For example, a coating of a finely divided inert solid, e.g., talc, or a microporous non-woven fabric or plastic film, e.g., polyethylene, polyvinylchloride, etc. can be used. A very thin continuous film (e.g. ca 25 micrometers) of polyurethane, e.g., Estane™ available from B. F. Goodrich, is preferred as a backing. This polyurethane is a polyoxyethylene polyurethane which contributes to the high MVT. This film has several advantages. It is very soft, and conforms well to body contours. It possesses high moisture vapor transmission (ca 1500 gm/m 2 /hr), allowing absorbed water vapor to escape from the adhesive into the atmosphere. It is also impervious to bacteria.
For use, a dressing of this invention is attached to a patient's skin over a wound. In the normal healing process, aqueous fluid-bearing cells, etc. needed for wound repair, will ooze from the damaged tissue. When the wound is of considerable size, excess fluid may be produced. As a result of fluid production a significant pressure will build up in the wound cavity. As described above, the adhesive film already possesses a significant moisture vapor transmission (MVT), so that water vapor from the wound exudate will begin to penetrate the film. As it penetrates, it can encounter one or more of the small voids or reservoirs in the adhesive film. The effective thickness of the dressing as seen by molecules of water vapor passing through the dressing, is controlled by the number of reservoirs the molecules encounter, and by the thickness of the solid zones traversed by the molecules. It will be appreciated that the absorption capacity of the film is dependent upon both the diffusion of water molecules into the solid zones, and the capacity of the reservoirs to contain liquid water which has diffused into them as vapor. A film with only a relatively small number of reservoirs and relatively large solid zones between reservoirs would have a lower MVT than a low density, closed-cell foam adhesive film, in which the solid zones between the reservoirs are very small. A dressing of the latter type will have very high MVT relative to conventional dressings of comparable thickness. As a result, dressings of the present invention can provide optimum MVT previously obtainable only with films that are too thin and flimsy to handle easily.
There may be occasions when it would be desirable to include an extra, protective backing or embedded reinforcing layer, e.g., a fibrous and/or fabric filler as discussed above, when, for example, a dressing may be expected to be subjected to mechanical wear-and-tear. Such a backing or reinforcing layer need not be functional from the standpoint of controlling MVT, so long as it doesn't reduce the MVT of the dressing below the desired level. However, backing and reinforcing layers which affect MVT may be utilized to achieve the MVT properties desired in the dressing.
EXAMPLES
General Procedure For Frothing And Coating Adhesives
The uncured adhesive and surfactant solutions were pumped simultaneously using two Zenith QM1416 metering systems, one system at a 20:1 ratio and the other at a 30:1 ratio, (Fenner DC Controllers) and two Zenith gear pumps (BMC 5334 and BPB 5566) through a 99 mm single-stage mixer (SKG Industries) with introduction of nitrogen gas. The resulting frothed premix was coated between two low-adhesion carriers, at least one of which was transparent to UV radiation. The thickness of the coating was controlled by a nip roll or knife. The coating was irradiated through the transparent film(s) with 15 watt fluorescent black lights having a maximum at 350 nm. Conditions for frothing and coating were as follows unless otherwise noted.
______________________________________Uncured adhesive flow rate 96 cc/min.Surfactant flow rate 4 cc/min.N.sub.2 flow rate 100 cc/min.Mixer Speed 300 rpmBack Pressure 211 g/cm.sup.2Adhesive Thickness 0.760 mmExposure 4 × 10.sup.6 ergs______________________________________
Following the curing process, one of the low-adhesion carriers was removed and the adhesive was laminated onto a 0.025 mm thick, polyoxyethylene polyurethane film backing prepared as follows. A one mil, i.e., 25 micron film of Estane™ 58309-021 polyurethane resin (B. F. Goodrich, Cleveland, Ohio) was extruded using a three-quarter inch (1.9 cm) Rheomex Model 252 screw extruder (manufactured by Haake, Saddlebrook, N.J.), a sheeting die and a melt temperature of 190° C. The film was extruded onto the back clay-coated side of a 78 pound (35412 grams) paper which was clay-coated on one side by roll coating (No. 70-05-04-000, Boise Cascade Corporation, International Falls, Minn.). Immediately after extrusion the paper/resin combination was passed through a nip roll at 80 psi (5624 grams per square centimeter).
Premix Starting Materials
The following materials were used to prepare the adhesives shown in the following examples.
Thickeners
Thickener A. A solution composed of 30 parts of isooctylacrylate, 30 parts of acrylic acid, 40 parts of polypropylene glycol-425 (PPG-425, Dow Chemical), and 0.04 parts "Irgacure" 651 (2,2-dimethoxy-2-phenylacetophenone, Ciba Geigy) was simultaneously purged with nitrogen gas and irradiated with fluorescent black lights until a temperature of 79° C. was attained. The exposure was then stopped and the reaction was quenched with air. The resulting syrup had a viscosity of 11,000 cps at 25° C. and contained 75% residual acrylate monomer.
Thickener B. A solution containing 25 parts of isooctylacrylate, 25 parts of acrylic acid, 50 parts of polypropylene glycol 425 and 0.04 parts of "Irgacure" 651 was simultaneously purged with nitrogen gas and irradiated with fluorescent black lights until a temperature of 77° C. was attained. The irradiation was then stopped and the reaction was quenched with air. The resulting syrup had a viscosity of 6200 cps at 25° C. and contained 71% residual acrylate monomer.
Thickener C. A solution containing 80 parts of isooctylacrylate, 20 parts of acrylic acid and 0.04 parts of "Irgacure" 651 was purged with nitrogen and irradiated with fluorescent black lights. The resulting syrup had a viscosity of 11,000 cps at 25° C. and contained 89% residual monomer.
Thickener D. A solution containing 60 parts of glycerin and 40 parts of "Goodrite"K722 (a 37% aqueous solution of polyacrylic acid, MW 100,000, B. F. Goodrich) (PAA) was fed through a film extruder available from LUWA Co. at a rate of 100 lbs./hr., 160° F. and 5 mm Hg. The resulting syrup, consisting of 79.8% glycerin, 19.2% polyacrylic acid and 1.0% H 2 O, had a viscosity of 200,000 cps at 25° C.
Thickener E. A solution containing 90 parts of isooctylacrylate, 10 parts of acrylic acid and 0.04 parts of "Irgacure" 651 was purged and irradiated as in C, above. The resulting syrup had a viscosity of 4330 cps at 25° C.
Thickener F. Sodium carboxymethyl cellulose, Type 7H, Hercules, Inc.
Thickener G. Polyvinylpyrrolidone K-90, GAF.
Thickener H. Low viscosity chitosan from Protan Laboratories, Inc.
Thickener I. A solution containing 80 parts of isooctylacrylate, 20 parts of acrylic acid and 0.04 parts of "Irgacure" 651 was simultaneously purged with nitrogen gas and irradiated with fluorescent black lights until a temperature of 67° C. was attained. The irradiation was then stopped and the reaction was quenched with air. The resulting syrup had a viscosity of 32,000 cps at 25° C.
Photoinitiators
Photoinitiator A: 2,2-dimethoxy-2-phenylacetophenone available as "Irgacure" 651 from Ciba-Geigy.
Photoinitiator B: hydroxycyclohexyl phenyl ketone available as "Irgacure" 184 from Ciba-Geigy.
Difunctional Monomers
TGBM: Triethylene glycol bis-methacrylate available from Sartomer Company.
EGBM: Ethylene glycol bis-methacrylate available from Sartomer Company.
Surfactants
Surfactant A. A solution of 70 parts of polypropylene glycol having a molecular weight of 425, 40 parts of a fluorosurfactant available as Fluorad™ FC171 from 3M and 60 parts of a fluorosurfactant available as Fluorad™ FC431 from 3M.
Surfactant B. A solution of 50 parts of polypropylene glycol 425 and 100 parts of a fluorosurfactant available as Fluorad™ FC431 from 3M.
Surfactant C. A solution of 50 parts of polypropylene glycol-425 and 50 parts of a fluorosurfactant available as Fluorad™ FC430 from 3M.
Surfactant D. A solution of 50 parts of polypropylene glycol-425 and 50 parts of a fluorosurfactant available as Fluorad™ FC171 from 3M.
Surfactant E. To a solution of 60 parts of a fluorosurfactant available as Fluorad™ FC431 from 3M and 40 parts of a fluorosurfactant available as Fluorad™ FC171 from 3M was added 30 parts of carbitol acetate. Under reduced pressure, 30 parts of ethyl acetate were removed by distillation.
Test Methods
The tests used to evaluate the samples and generate the results shown in Table 4 were accomplished as follows.
Moisture Vapor Permeability
A modified Payne cup method is used. The method comprises the following steps:
(1) A 13/8 inch (35 mm) diameter sample of material to be tested containing no perforations is cut.
(2) The sample is entered between the adhesive surfaces of two foil adhesive rings, each having a one inch (2.54 cm) diameter hole. The holes of each ring are carefully aligned. Finger presure is used to form a foil/sample/foil assembly that is flat, wrinkle-free and has no void areas in the exposed sample.
(3) A 4 ounce glass jar is filled half full of distilled water. The jar is fitted with a screw on cap having a 1.50 inch diameter hole in the center thereof and with a 1.75 inch diameter rubber washer having a 1.12 inch diameter hole in its center.
(4) The rubber washer is placed on the lip of the jar and the foil/sample assembly is placed on the rubber washer. The lid is then screwed loosely on the jar.
(5) The assembly is placed in a chamber at 100° F. (38° C.) and 20 percent relative humidity for four hours.
(6) The cap is tightened inside the chamber so the sample material is level with the cap (no bulging) and the rubber washer is in proper seating position.
(7) The assembly is removed from the chamber and weighed immediately to the nearest 0.01 gram (initial weight -W 1 ).
(8) The assembly is returned to the chamber for at least 18 additional hours.
(9) The assembly is removed from the chamber and weighed immediately to the nearest 0.01 gram (final weight -W 2 ).
(10) The water vapor transmission in grams of water vapor transmitted per square meter of sample area in 24 hours is calculated according to the following formula: ##EQU2## W 1 =initial weight (grams) W 2 =final weight (grams)
T 2 =time (hours)
When a 1/2 inch sample is tested, the formula is changed to the following: ##EQU3##
(11) Three samples of each material should be run and the average taken.
Absorbency
To determine absorbency, a sample of the cured adhesive was initially weighed and then immersed in deionized water at room temperature for one hour. The sample was then retrieved and weighed again . Absorbency is reported as the difference in weight divided by the initial weight. Optimal absorbency varies greatly depending upon the intended use of the adhesive film. For use on intact skin, low absorbencies are acceptable. Highly exudative wounds require higher absorbency films. Absorption capacity of the film can be controlled by the thickness of the film. In general, an absorbency of at least 50% over 1 hour is preferred.
180° Peel Adhesion
One inch (2.54 cm) wide test samples of the cured adhesive are self-adhered to the skin of a human volunteer under the weight of a 2.04-kg hard rubber roller, 2 passes in each direction. After 15 minutes dwell, 180° peel is measured by moving the free end of each tape away from the skin at a rate of about 0.5 cm per second (using a tensile tester). Samples were tested immediately after application (Initial) and at 6 hours after application (Final) and results reported. Preferred adhesives have an initial adhesion of at least about 5 g/cm, more preferably at least 10 g/cm and most preferably at least about 20 g/cm. The final adhesion is preferably less than double the initial adhesion.
Density
The density of the samples was measured by simply weighing a sheet of each sample and measuring the area and depth of the sheet to calculate volume.
EXAMPLES 1-5 and Comparative Example A
Examples 1-5 and Comparative Example A, summarized in Table I, below, were prepared by combining the thickener specified with additional isooctylacrylate ("IOA") and acrylic acid monomers ("AA") and polypropylene glycol ("PPG") to give the IOA:AA:PPG ratios (ratio includes copolymerized IOA and AA in thickener) and % solids (IOA-AA copolymer) indicated in Table I. "Irgacure" 651 was added at a level of 0.1% by weight. Triethylene glycol bis-methacrylate (TGBM) was added at the levels indicated and the mixture was mechanically stirred. The resulting solution was frothed in a 96:4 ratio with surfactant E, coated and cured as described in the "General Procedure".
TABLE I__________________________________________________________________________Composition of Examples 1-5 and Comparative Example AMonomer-Solvent Thickener Solids TGBMExampleRatio (wt. %) (wt. %) (wt. %) Thickness (mm)__________________________________________________________________________1 IOA-AA-PPG A (69.3) 10.4 2.9 0.7622.5-22.5-552 IOA-AA-PPG A (69.3) 10.4 2.9 0.2522.5-22.5-553 IOA-AA-PPG C (50) 7.3 1.5 0.7640-20-404 IOA-AA-PPG C (44) 6.4 2.0 0.7635-25-405 IOA-AA-PPG C (50) 7.3 2.0 0.7640-20-40A IOA-AA E (100) -- -- 0.7690-10__________________________________________________________________________
EXAMPLES 6-18
Examples 6-18 were prepared by combining thickener D [an 80/20 glycerin-polyacrylic acid ("PAA") solution] with acrylic acid and glycerin to give the AA:glycerin:PAA ratio indicated in Table II. To this was added "Irgacure" 651 at a level of 0.1%, difunctional monomer TGBM or EGBM, and, optionally, lithium hydroxide as indicated, and the mixture was mechanically stirred. The resulting solution was frothed in combination with the surfactant indicated, coated and cured according to the "General Procedure".
TABLE II__________________________________________________________________________Composition of Examples 6-18 DifunctionalEx. AA Glycerin PAA Monomer LiOH Surfactant ThicknessNo. (wt. %) (wt. %) (wt. %) (wt. %) (wt. %) (wt. %) (mm)__________________________________________________________________________ 6 25 67.5 7.5 TGBM (0.2) -- E (4) .762 7 25 67.5 7.5 TGBM (0.2) -- E (4) .330 8 25 67.5 7.5 TGBM (0.2) -- E (4) .127 9 30 60 10 TGBM (0.3) -- E (4) .76210 25 67.5 7.5 TGBM (0.2) -- C (4) .76211 25 67.5 7.5 TGBM (0.2) -- C (2) .76212 25 67.5 7.5 TGBM (0.2) -- C (1) .76213 25 67.5 7.5 TGBM (0.2) -- none .76214 25 67.5 7.5 TGBM (0.2) -- D (4) .76215 25 67.5 7.5 TGBM (0.2) -- A (4) .76216 25 67.5 7.5 TGBM (0.2) -- B (4) .76217 19.4 68.4 5.9 TGBM (0.2) 5.9 E (3) .76218 19.4 68.4 5.9 EGBM (0.2) 5.9 E (4) .762__________________________________________________________________________
Examples 11 and 12 were the same as Example 10 with the exception that the level of surfactant was varied. In Example 13, no surfactant was used. The absence of an effect from these variations upon the foamed density is shown in Table III.
TABLE III______________________________________Foam Density of Examples 10-13 Surfactant C Foam DensityExample (wt. %) (g/cc)______________________________________10 4 0.5111 2 0.5312 1 0.5113 0 0.53______________________________________
EXAMPLE 19
To 1500 g of the uncured adhesive solution described in Example 6 was added 105 g of glass bubbles (Product #B-22-AS, 3M) with mechanical stirring. The suspension was frothed in 96:4 ratio with surfactant E, coated and cured according to the general procedure.
EXAMPLE 20
To 900 g of the uncured adhesive solution described in Example 6 was added 63 g cross-linked polyvinylpyrrolidone (#85,648-7, Aldrich Chemical Company) with mechanical stirring. The resulting suspension was frothed, coated and cured according to the "General Procedure" in a 96:4 ratio with surfactant E.
EXAMPLE 21
To a mechanically stirred solution of 875 g of glycerin, 375 g of H 2 O, 500 g of acrylic acid, 120 g of lithium hydroxide, 6.0 g of triethylene glycol bis-methacrylate, 1.0 g of Irgacure 651 and 1.0 g of methyl hydroquinone, an antioxidant hereinafter referred to as MEHQ, was added 50 g of sodium carboxymethyl cellulose (Type 7H, Hercules). The resulting solution having a viscosity of 6500 cps at 25° C. was frothed, coated and cured according to the General Procedure in a 96:4 ratio with surfactant E.
EXAMPLE 22
To a mechanically stirred solution of 720 g of glycerin, 720 g of H 2 O, 400 g of acrylic acid, 2.0 g of Irgacure 184, 120 g of lithium hydroxide and 1.0 g of MEHQ was added 60 g of low viscosity chitosan (Protan Laboratories, Inc.). The resulting solution having a viscosity of 2000 cps was frothed, coated and cured according to the "General Procedure" in a 96:4 ratio with surfactant E.
EXAMPLE 23
The uncured adhesive solution described in Example 14 was frothed according to the "General Procedure" in a 96:4 ratio with surfactant E and was coated in two 0.015" layers with a spun-bonded nylon fabric (1.0 oz., Cerex) sandwiched between the layers. The resulting multi-layer coating was cured according to the "General Procedure".
The properties of the adhesives prepared in Examples 1-23 and Comparative Example A are shown in Table IV, below.
TABLE IV__________________________________________________________________________Properties of Dressings with BackingsFoamed Unfoamed 180° Peel Adhesion VoidEx. MVT Absorbency MVT Absorbency Initial Final Density VolumeNo. (g/m.sup.2 - 24 h) (Percent) (g/m.sup.2 - 24 h) (Percent) (g/cm) (g/cm) (g/cc) (Percent)__________________________________________________________________________ 1 477 13.2 316 -- 27.5 36.6 0.915 15 2 411 10.0 283 7.9 34.6 49.2 0.903 17 3 299 17.5 141 4 27.6 21.6 0.946 12 4 266 13 166 9 20.9 19.7 0.952 14 5 291 17 183 5.7 -- -- 0.671 67 A 207 21 102 19 41.3 116 -- 42 6 921 1478 859 788 98.4 70.9 1.007 23.6 7 1198 6977 1059 4323 88.6 74 1.129 7.4 8 1179 9926 1202 6085 35.4 59.1 -- -- 9 1223 1519 1141 734 7.1 17.7 1.129 1310 1339 1023 1226 -- 88.6 82.6 1.025 21.514 1271 1259 1388 -- 72.8 87.4 1.068 18.315 1405 1651 1257 -- 74.8 69.7 1.019 21.716 1315 1191 1285 -- 66.9 71.7 0.995 23.717 1249 1837 1016 3601 88.9 118.7 -- --18 1083 4016 1029 4641 49.4 43.7 -- --19 1264 1937 936 908 54.3 88.6 0.84 15.420 1090 459 1032 427 44.5 61.0 1.03 18.621 1194 6383 1215 5379 0.98 9.06 1.08 14.622 1266 dissolved 1074 dissolved 7.3 12.4 0.616 45.223 1125 312 899 262 70.1 68.9 1.09 15.0__________________________________________________________________________
EXAMPLE 24
A sample was prepared as described in Example 6 with the following modification. During the coating process, the froth was coated directly onto the 0.01 inch thick polyurethane backing film described in the "General Procedure", and covered with a transparent low-adhesion liner. The General Procedure for curing provided a foamed adhesive with a polyurethane backing on a low-release liner. In this case, the additional step of laminating a backing to the cured adhesive was eliminated.
EXAMPLE 25
A foamed pressure-sensitive adhesive in which the hydrophilizing component is covalently bonded into the polymer network can be prepared by the following procedure: To a solution of 300 g of Thickener I, 100 g of acrylic acid, 5.0 g of TGBM and 2 g of Irgacure 651, add 600 g of a polyoxyalkyleneacrylate. (A polyoxyalkyleneacrylate can be obtained by adding dropwise, 155 g of 2-isocyanatoethylmethacrylate to a nitrogen purged solution of 4 drops of dibutyltindilaurate and 2170 g of an amine-functional poly(alkylene oxide) having the formula (CH 3 OCH 2 CH 2 O(CH 2 CH 2 O) n (CH 2 (CH 3 )CHO) m CH 2 (CH 3 )CHNH 2 where n/m=2/32, (available as Jeffamine M-2005 from the Texaco Chemical Company), and heating to 35° C. for 2 hours.) The resulting adhesive premix solution is frothed, coated and cured and the resulting film is laminated to a 0.025 mm polyurethane film as described in the General Procedure.
EXAMPLES 26-31
In Examples 26-31, earlier examples were repeated with the exception that a different backing or no backing was used when the MVT of the adhesive was tested.
EXAMPLE 26
A sample was prepared as described in Example 6 except that the backing lamination step was omitted. The final product consisted of a foamed adhesive layer between two low-adhesion liners. Removal of both liner films at the time of application provided a dressing which was tacky on two sides and was suitable for attachment of additional devices such as an ostomy or exudate collective device.
EXAMPLE 27
A sample was prepared as in Example 6, except a rayon non-woven web as described in U.S. Pat. No. 3,121,021 to Copeland, the backing used in Micropore™ brand tape (3M), was substituted for the polyurethane film in the backing lamination step.
EXAMPLE 28
A sample was prepared as described in Example 3 except that the backing lamination step was omitted.
EXAMPLE 29
A sample was prepared as described in Example 4 except that the backing lamination step was omitted.
EXAMPLE 30
A sample was prepared as described in Example 1 except that the backing lamination step was omitted.
COMPARATIVE EXAMPLE B
A sample was prepared as described in Comparative Example A above, except that the backing lamination step was omitted.
TABLE V______________________________________Effect of Backing on MVT MVTExample IOA/AA/PPG Backing* (g/m.sup.2 - 24 hr)______________________________________ 6 -- I 92126 -- none 347627 -- II 3219 3 40/20/40 I 29928 40/20/40 none 447 4 35/25/40 I 26629 35/25/40 none 566 1 22.5/22.5/55 I 47730 22.5/22.5/55 none 531A 90/10/0 I 207B 90/10/0 none 329______________________________________ *Backings: I: 0.025 mm polyurethane film II: nonwoven rayon web
The data shown in Table V illustrate the general superiority, in terms of MVT, of the adhesives of this invention as compared with adhesives of the type shown in Comparative Examples A and B.
EXAMPLE 31
In order to confirm the impermeability to liquid water, the adhesive described in Example 23 was evaluated by the following procedure. The apparatus used consisted of a pressure loop made of copper tubing, 4.13 cm in diameter One end of the loop was connected to a source of compressed air and was fitted with a pressure regulator. The opposite end of the loop had a flat rigid flange of 7.6 outer diameter and 3.6 cm inner diameter with a rubber O-ring of 4.4 cm diameter embedded in the flange for sealing. A matching top ring was used to clamp the test samples in place.
The pressure loop was fitted with a solution of 692 parts deionized water, 7 parts DOWFAX™ 2A1 surfactant available from Dow Chemical Co., and 0.7 parts methylene blue dye. The adhesive sample with both low-adhesion carriers removed, was laminated to a single layer of Whatman 4-Qualitative filter paper. With the filter paper side facing away from the dye solution, the test sample was secured between the two flanges of the apparatus described above, and the apparatus was rotated to exclude air between the sample and the dye solution. Air pressure of 76.2 cm of water was applied for two minutes at which time no evidence of dye solution wetting the paper was observed. The air pressure was increased until the filter paper split due to expansion of the adhesive; still no evidence of wetting of the paper was observed which indicated that the foamed adhesive sample was not permeable to liquid water.
|
A method is disclosed for treating a wound or attaching a device or article to the skin using a film of pressure sensitive adhesive having dispersed therein a discontinuous gaseous phase contained within voids in the adhesive. The adhesive is formed from the polymerization of a hydrophilic premix and exhibits high moisture vapor transmission and fluid absorbency.
| 8
|
BACKGROUND OF THE INVENTION
1. Field of the invention
The present invention relates to a process for the production of dihydric phenols, such as resorcin etc., in particular, by oxidizing diisopropylbenzenes followed by acid cleavage of the resulting dihydroperoxides.
2. Desrciption of the Prior Art
It has been known that hydroperoxides, such as, diisopropylbenzene dihydroperoxide (DHP), diisopropylbezene monocarbinol monohydroperoxide (HHP), diisopropylbezene monohydroperoxide (MHP) and so on, are produced together with carbinols, such as, diisopropylbezene dicarbinol (DC) and so on, by oxidizing diisopropylbezenes with molecular oxygen in the presence of a base.
It has also been well known that industrially useful chemicals, such as, resorcin, hydroquinone and so on, can be obtained by subjecting DHP to an acid cleavage using an acid catalyst, such as, sulfuric acid or so on, in the presence of an aromatic hydrocarbon solvent, such as toluene etc., or a ketone solvent, such as, acetone, methyl isobutyl keytone (MIBK) or so on.
While these prior techniques can be employed as a useful process for obtaining resorcin and hydroquinone from diisopropylbezene, there has been a strong demand for producing hydroperoxides, especially DHPs at higher yeild by oxidizing diisopropylbezene more efficiently in order to obtain resorcin or hydroquinone at a more higher over-all yield from diisopropylbezene.
Attempts had been proposed for converting the carbinols, such as, HHP, DC etc., present in the reaction product mixture of the oxidation of diisopropylbezene further into DHP by oxidizing them by contacting the product mixture with hydrogen peroxide (H 2 O 2 ), as disclosed, for example, in the British Patent No. 910,735, in the Japanese Patent Application Lay Open Nos. 23939/1978, 53265/1980 and so on. According to the disclosures of the above Japanese Patent Application Lay Open Nos. 23939/1978 and 53265/1980, it is taught that dihydric phenols can be obtained in a high efficiency by oxidizing carbinols, such as, HHP, DC and so on, with subsequent acid cleavage of the oxidation products, by conducting the process step of oxidization of the carbinols into DHPs with hydrogen peroxide separately from the process step of acid cleavage of the DHPs into the corresponding dihydric phenols.
In summary, the prior technique for the production of dihydric phenols, such as resorcin etc., by oxidzing isopropylbezenes with subsequent acid cleavage of the oxidation product proposed previously has been based on the following reaction scheme:
Upon oxidizing diisopropylbenzenes with molecular oxygen in the presence of a base using, if necessary, a radical initiator, a reaction mixture containing DHP, HHP, MHP, DC and so on as explained above is obtained. This oxidation product mixture is then subjected to a further oxidation with hydrogen peroxide in order to oxidize HHP, DC and so on contained in the product mixture into DHP in a heterogeneous reaction system consisting of an oily phase of an aromatic hydrocarbon solvent, such as toluene etc., containing dissolved therein said oxidation product mixture and of an aqueous phase containing hydrogen peroxide and an acid catalyst, such as sulfuric acid, by contacting the two phases with each other. Then, the so formed DHP is subjected to an acid cleavage in a separate process step to convert it into the corresponding dihydric phenol, such as resorcin or so on.
The process step of oxidizing the HHP, DC and so on with hydrogen peroxide into DHPs may be realized by supplying the product mixture of oxidization of diisopropylbenzene in a form of an oil phase containing said product mixture in an aromatic hydrocarbon solvent, such as toluene etc., to a tank reactor equipped at its top with a distillation column and a water separator, while supplying to this reactor simultaneously hydrogen peroxide and an acid catalyst, such as sulfuric acid, in a form of aqueous phase, so as to cause the two phases to contact with each other in order to effect oxidation of the said HHP, DC etc., by hydrogen peroxide at a temperture of 20°-70° C. Then, the oily phase in the resulting reaction mixture is separated from the aqueous phase and the aqueous phase is recirculated to the reactor under supplement of the consumed hydrogen peroxide and the acid catalyst, while the oily phase is supplied to the subsequent acid cleavage step after it has been neutralized and concentrated. It was proposed to supply hydrogen peroxide to the reactor in an amount of about 16 moles per mole of HHP. Here, the weight ratio of oily phase to aqueous phase in the reactor is maintained at a value of about 1.6. The reaction water formed by the oxidation of HHP is removed fromm the reaction mixture by an azeotropic distillation with the aromatic hydrocarbon under a reduced pressure to the outside of the system, wherein the aromatic hydrocarbon is recirculated to the reactor. In the above procedure, it is necessary to maintain the reaction temperature by supplying vapor of an inert solvent for avoiding any detrimental influence due to localized heating. The reason why the ratio of oily phase/aqueous phase is to be maintained at about 1.6 in the reactor is such that the acid cleavage of the peroxide will scarcely occur when an ample aqueous phase is present, even if a concentrated acid catalyst resulting from the concentration of the aqueous phase may come to contact with the reaction liquor. However, use of large amount of water is not preferable, since predominant part of the by-products is transferred to the aqueous phase which accumulate therein after repeated recirculation cycles. In addition, it is necessary to maintain the concentration of hydrogen peroxide in the reaction system at about 16 times of HHP in mole ratio due to employment of large amount of water.
Thus, the prior technique of oxidizing HHP, DC and so on by hydrogen peroxide into DHPs has disadvantages, since quite large amount of hydrogen peroxide relative to the amount of HHP etc., should be supplied and laborious and uneconomical procedures of dehydration by an azeotropic distillation under a reduced pressure and recirculation of the aromatic hydrocarbon are necessary, beside the necessity of controlling the concentrations of hydrogen peroxide and of the acid catalyst for the requisite recirculation of the aqueous phase with simultaneous demand of large amount of water for maintaining the ratio of oily phase/aqueous phase at a lower value in oder to conduct the operation smoothly.
SUMMARY OF THE INVENTION
An object of the present invention is to obviate the above disadvantages and to provide a novel process for the production of dihydric phenols which permits to dispense with the removal of the reaction water, recirculation of the aromatic hydrocarbon and of the aqueous phase, while allowing a higher ratio of oily phase/aqueous phase and thus allowing reduction of the requisite amount of hydrogen peroxide and of the acid catalyst with simultaneous decrease in the reaction time.
The novel process for the production of dihydric phenols according to the present invention comprises steps of:
oxidizing diisopropylbenzenes with molecular oxygen to obtain a reaction product mixture (A) containing at least diisopropylbenzene dihydroperoxide (DHP) and diisopropylbenzene monocarbinol monohydroperoxide (HHP),
supplying said reaction product mixture (A) in a form of an oily phase as a solution in an aromatic hydrocarbon solvent to an agitation reactor,
supplying thereto at the same time, as an aqueous phase, hydrogen peroxide at a feed rate of 1-5 moles per mole of HHP contained in the reaction mixture (A) and an acid catalyst in an amount sufficient to reach a concentration in the aqueous phase of 10-40% by weight, the concentration of hydrogen peroxide in the aqueous phase being maintained at a value of at least 20% by weight and the weight ratio of the oily phase/aqueous phase being at least 10,
causing oxidization of the HHP into corresponding DHP by hydrogen peroxide while maintaining the reaction temperture at 30°-60°C. to obtain a reaction product mixture (B),
separating the aqueous phase from the oily phase in the reaction product mixture (B) and
subjecting the DHP in the so separated oily phase to acid cleavage to form corresponding dihydric phenol.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 show each a flow chart of preferable embodiment of the process according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
In the process for the production of dihydric phenols according to the present invention, hydrogen peroxide and the acid catalyst are supplied to an agitation reactor in a form of aqueous phase, wherein the feed rate of hydrogen peroxide is such that the amount of hydrogen peroxide will be 1-5 moles per mole of HHP contained in the product mixture (A) and the concentration of the acid catalyst in the aqueous phase is maintained at 10-40% by weight, whereupon the oily phase and the aqueous phase are brought into contact with each other to cause the HHP etc. in the product mixture (A) to be oxidized into corresponding DHPs under such a condition that the concentration of hydrogen peroxide in the aqueous phase is kept to be at least 20% by weight and the weight ratio of oily phase/aqueous phase is maintained at a value of at least 10, without specifically reducing the pressure. Therefore, there is no occurrence of concentration of acid catalyst in the aqueous phase and, at the same time, recirculation of aromatic hydrocarbon solvent can be dispensed with. Moreover, in the case of no repeated use of the aqueous phase, there is no need for adjusting or controlling the concentration of hydrogen peroxide and of the acid catalyst with simultaneous permission of reduction of the requisite amount thereof.
In this specification, the dihydric phenols are meant to include, beside resorcin, hydroquinone and so on, also those having substituents, such as alkyl etc. The same applies also to the diisopropylbenzenes, DHPs, HHPs, DC and so on.
In the process according to the present invention, the oxidation of a diisopropylbenzene by molecular oxygen is first effected to form an oxidation product mixture (A) containing at least diisopropylbenzene dihydroperoxide (DHP) and diisopropylbenzene monocarbinol monohydroperoxide (HHP).
For the oxidation of diisopropylbenzenes (DIPBs) with molecular oxygen to produce DHPs and HHPs, any process widely known hitherto can be employed. In general, the oxidation of diisopropylbenzenes (DIPBs) by molecular oxygen, such as air, is effected in the presence of a base using, if necessary, a radical initiator.
Upon this oxidation of DIPBs with molecular oxygen, by-products such as, diisopropylbenzene dicarbinol (DC), diisopropylbenzene monohydroperoxide (MHP) and so on are formed besides DHP and HHP.
Then, the so obtained oxidation product mixture (A) is dissolved in an aromatic hydrocarbon solvent to form an oily phase and the alkaline aqueous phase is separated off, whereupon the thus formed oily phase is supplied to an agitation reactor arrangement, such as, a multistage agitation reactor assembly 1 as shown in the appened FIG. 1 or to a tubular reactor 11 as shown in the appended FIG. 2. The multistage agitaion reactor assembly 1 shown in FIG. 1 consists of several agitation reactors 2a, 2b, 2c . . . cascadingly connected in series in multistages each equipped with an agitation device 3a, 3b, 3c . . . driven by a motor 4a, 4b, 4c . . . for the agitation device 3a, 3b, 3c . . . , those which rotate at a revolution rate corresponding to a peripheral speed of at least 1 m/sec may be preferable. The tubular reactor 11 as shown in FIG. 2 is provided with a rotatable coil 13 which is disposed in a horizontal tube 12 and is driven by a motor 14.
For the aromatic hydrocarbon solvent for dissolving the oxidation product mixture (A), there may be enumerated, for example, benzene, toluene, xylene, ethylbenzene, cumene, cymene, diisoprpylbenzene and so on, among which toluene is most preferable.
To the multistage agitation reactor assembly 1 or to the tubular reactor 11, hydrogen peroxide is supplied at a rate corresonding to 1-5 moles, preferably 1.0-3 moles per mole of HHP contained in the oxidation product mixture (A). Thereto is supplied simultaneously an acid catalyst in such an amount that the concentration thereof in the aqueous phase will be 10-40% by weight. The concentration of hydrogen peroxide in the aqueous phase supplied to the reactor assembly 1 or the tubular reactor 11 may be at least 20% by weight, preferably 40-55% by weight. Here, the weight ratio of the oily phase to the aqueous phase within the reactor 1 or 11 may preferably be at least 10, in particular, wihtin the range from 20-35.
For the acid catalyst, inorganic acids, such as, sulfuric acid, hydrochloric acid, perchloric acid, phosphoric acid and so on may be employed, among which sulfuric acid is particularly preferabl.
In the process according to the present invention, the weight ratio of the oily phase to the aqueous phase in the reactor 1 or 11 is settled at a value of at least 10, preferably from 20 to 35, which is quite high as compared with that in the conventional techniques. This means that the amount of aqueous phase in the reactor 1 or 11 is considerably small. Therefore, it is now made possible to settle the amount of hydrogen peroxide employed for the oxidation of HHP present in the oxidation product mixture (A) at a considerably low level as low as 1-5 moles per mole of HHP. It is also made possible to choose a concentration of hydrogen peroxide in the aqueous phase supplied to the reactor 1 or 11 at a value of at least 20% by weight, preferably in the range from 40 to 55% by weight.
The oxidation of HHP contained in the oxidation product mixture (A) by hydrogen peroxide is effected while maintaining the temperture of the reaction system containing these reactants at 30°-60° C., preferably at a temperture in the range from 40°to 55° C., to obtain DHP. Here, it is preferable to maintain the reaction mixture in the reactor under an intensively agitated condition.
In the process according to the present invention, the reaction liquor is held in an agitated state using an agitation reactor arrangement to effect the oxidation efficiently. Examples of such agitation reactor arrangement include:
(1) a tank reactor with mechanical agitation equipped with an ordinary agitation device, such as, a stirrer having varying form of agitation vane (for example, turbine type, curved paddles, inclined paddles and so on) or with a high speed rotary shearing stirrer, such as, Homomixer (trademark) of the firm Tokushu-Kika Kogyo K. K. or so on, and
(2) a tubular reactor in which the reaction liquor flows inside the reactor tube in a turbulent flow.
The agitation condition of the mechanical agitation reactor of above (1) according to the present invention implies a peripheral speed of the rotary agitation vane transmitting the agitation energy directly to the reaction liquor of at least 1 m/sec, preferably at least 5 m/sec. Here, the peripheral speed as used in this specification is expressed by the value calculated by r×ω, assuming r to be the distance from the center of rotation to the outer-most periphery of the rotating vane in m and ω to be the angular velocity of the vane in radian/sec.
In the process according to the present invention, it is more advantageous to realize the oxidation of HHP etc. in the product mixture (A) with hydrogen peroxide in a multistage system than in a single stage system, if the oxidation reaction is performed in a continous process.
While the reaction time may be different in accordance with the reaction temperture, concentration of the acid catalyst, concentration of hydrogen peroxide and so on, it varies, in particular, by the condition of agitation. Thus, a reaction time of 10-30 minutes is usually necessary at a peripheral speed of the agitation device of 1.1 m/sec, while it may be reduced consiberably by increasing the peripheral speed an may amount to, for example, 3-15 minutes at a peripheral speed of 3.8 m/sec and 0.5-5 minutes at a peripheral speed of 11 m/sec.
In the process according to the present invention, the problem of acid cleavage of aromatic hydroperoxide which is assumed to be due to the evaporation of water at the interface between the liquid phase and the gas phase can be avoided by fully charging the agitation reactor with the reaction liquor, wherein the internal temperture can be adjusted by flowing hot water through the surrounding water jacket.
In the tubular reactor of above (2), the reaction liquor is flown through the reactor tube in a turbulent flow in order to facilitate the agitation of the reaction liquor within the reactor tube. A turbulent flow of the reaction liquor in the tubular reactor can be attained by selecting the rate of the reaction liquor appropriately. It is possible, if necessary, to install a rotatable coil within the reactor tube for effecting mechanical agitation to facilitate the turbulence of the reaction liquor flowing inside the tube. The critial condition between turbulent flow and laminar flow may be discriminated, as well known in the art, by calculating the Reynolds number (Re) from the flow velocity. The accepted critical Reynolds number for a non-obstructed flow path lies at about 2,000, above which a turbulent condition occurs.
For a circular tube, Reynolds number, which is a dimensionless number, is calculated by the following equation: ##EQU1## in which d represents the inner diameter of the tube, U is the average flow velocity of the fluid, ρ is density of the fluid and μ is the viscosity of the fluid.
In the case of tubular reactor, the inner diameter of the reactor tube may, in general, be 10-100 mm, with the average flow velocity of the reaction liquor of, usually, 0.1-5.0 m/sec. The length of the reactor tube may, in general, be in the range from 10 to 500 m, which may be determined appropriately taking into account of the residence time of the liquor therein.
When mechanical agitation reactor mentioned previously is employed, the amount of hydrogen peroxide required for the oxidation reaction can be reduced and, in addition, the reaction time may also be decreased as compared with the case where no such mechanical agitation device is employed.
Now, the oxidation product mixture (B) resulting from the above oxidation by hydrogen peroxide is subject to separation of the oily phase from the aqueous phase in the separator 5 shown in FIG. 1 or 2 after addition of, if necessary, an amount of water for termination of the oxidation reaction. The thus separated oily phase is then, if necessary, neutralized and concentrated and fed to the acid cleavage step, in order subject the DHPs contained in the oily phase to an acid cleavage to convert it into corresponding dihydric phenols, such as resorcin and so on.
For effecting the acid cleavage of DHPs contained in the oily phase, any of the conventional techniques known hitherto may be applied. Thus, the acid cleavage may be realized at a temperture of 40°-100° C., preferably 60°-90° C., by adding to the oily phase a ketone solvent, such as, acetone, methyl ethyl ketone and diethyl ketone, and adjusting the concentration of the acid catalyst at a value in the range from 0.001 to 15% by weight.
As the acid catalyst, there may be employed, for example, inorganic acids, such as, sulfuric acid, sulfuric acid anhydride, hydrofluoric acid, perchloric acid, hydrochloric acid, phosphoric acid and so on; strongly acidic ion-exchange resin; solid acids, such as, silicaalumina; organic acids, such as, chloroacetic acid, methanesulfonic acid, bemzenesulfonic acid, p-toluenesulfonic acid and so on; heteropolyacids, such as, phosphowolframic acid, phosphomolybdic acid and so on.
In the process for the production of dihydric phenols according to the present invention, hydrogen peroxide and the acid catalyst are supplied, as explained above, to an agitation reactor as an aqeuous phase at such a rate that the amount of hydrogen peroxide will be 1-5 times, based on mole ratio, of the amount of HHP contained in the product mixture (A) supplied also thereto as an oily phase and the concentration of the acid catalyst in the aqueous phase will be 10-40% by weight, whereupon the oily phase and the aqueous phase are brought into contact with each other to cause oxidation of HHP etc. by hydrogen peroxide into corresponding DHPs under such a condition that the concentration of hydrogen peroxide in the aqueous phase is kept to be at least 20% by weight and the weight ratio of oily phase/aqueous phase is maintained at a value of at least 10, without specifically reducing the pressure. Therefore, no concentration of acid catalyst in the aqueous phase occurs and, at the same time, recirculation of aromatic hydrocarbon solvent can be dispensed with. Moreover, in the case of no repeated use of the aqueous phase, there is no need for adjusting or controlling the concentration of hydrogen peroxide and of the acid catalyst with simultaneous permission of reduction of the requisite amount thereof. Furthermore, the employment of an agitation reactor capable of realizing a powerful agitation affords a marked reduction of the reaction time in the oxidation of the product mixture (A) with hydrogen peroxide with simultaneous increase in the over/all yield of DHPs.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the following, the present invention will further be described in more detail by way of Examples and Comparison Examples. Here, it is to be emphasized that these specific Examples should not be understood as restrictive to the scope of the invention in any sence.
REFERENCE EXAMPLE 1
m-diisopropylbenzene was oxidized with air in the presence of an aqueous solution sodium at a temperture of 100°C. After the oxidation, toluene was added to the product mixture to cause phase separtion. By removing the so separated alkaline aqueous phase, a toluene solution of th eoxidation product mixture (A) having the composition given in the following Table 1 was obtained.
TABLE 1______________________________________Composition of the Product Mixture (A) ProportionComponent (wt. %)______________________________________DHP 24.5HHP 7.2DC 0.9MHP 3.5Toluene 59.3______________________________________
EXAMPLES 1 TO 3 AND COMPARISON EXAMPLE 1
To a multistage agitation reactor assembly as shown in FIG. 1, there was supplied the toluene solution (an oily phase) of the oxidation product mixture (A) obtained in the above Reference Example 1 at a rate of 549 parts by weight per hour and, at the same time, an aqueous phase containing hydrogen peroxide and sulfuric acid was supplied thereto at each specific rate as given in Table 2 which is calculated from the conditions given also in Table 2. The oxidation reaction was performed continuously while maintaining the peripheral speed of the agitation device, reaction temperture and the reaction time at each value as given in Table 2 respectively. The oxidation product liquor [oxidation product mixture (B)] derivered from the outlet of the reactor was subjected to separation of the oily phase from the aqueous phase and concentration of the hydroperoxides in the oily phase was analyzed. From this analysis, each yield of DHP was determined. The results are summarized in Table 2. Here, the flow of the aqueous phase was realized in "once-through" and no recirculation thereof was incorporated. ##EQU2##
EXAMPLES 4 AND 5
To a tubular reactor as shown in FIG. 2 having arranged internally a rotatable coil (tube inner diameter=10 mm, tube length=1 m, revolution rate of the coil=2,000 r.p.m.), the toluene solution (oily phase) of the oxidation product mixture (A) obtained in Reference Example 1 was supplied at a rate of 549 parts by weight per hour, while supplying thereto at the same time an aqueous phase containing hydrogen peroxide and sulfuric acid at a rate given in Table 2 which is calculated from the conditions given also in Table 2. Oxidation reaction was effected in a continuous manner while maintaining the reaction temperature and the reaction time at each value as given in Table 2. The reaction product mixture (B) delivered from the outlet of the reactor was subjected to separation of the oily phase from the aqueous phase and concentration of the hydroperoxides in the oily phase was anaylzed. The yield of DHP was determined from this analysis. The results are summarized also in Table 2.
COMPARISON EXAMPLE 2
To a tank reactor with mechanical agitation equipped at the top with a distillation column and a water separator and at the lower portion thereof with a gas injection pipe, the toluene solution of the oxidation product mixture (A) obtained in Reference Example 1 was supplied at a rate of 549 parts by weight per hour, while supplying thereto simultaneously an aqueous phase containing hydrogen peroxide and sulfuric acid each in a concentration given in Table 2 at a rate of 449 parts by weight per hour with concurrent introduction of heated vapor of toluene from the gas injection pipe at a rate of 161 parts per hour. The oxidation was effected while maintaining the conditions as to the reaction temperture and the average residence time (reaction time) at each value given in Table 2 under a pressure of 150 Torr. The entire amount of toluene in the effluent product stream discharged form the top of the reactor was recirculated again to the reaction system, while a part of the aqueous phase separated from the effluent stream was removed to the outside of the system. The reaction product mixture was extracted continuously from the overflow line and was subjected to separation of the oily phase from the aqueous phase, whereupon the aqueous phase was recirculated to the system after the concentrations of hydrogen peroxide and of sulfuric acid had been re-adjusted to the values given in Table 2. Here, the amount of H 2 O 2 in the reaction system was 16 times of the amount of HHP in mole ratio due to the recirculation of the aqueous phase, though the amount of H 2 O 2 requisite for converting the net amount of HHP into DHP were 3.0 times of HHP. By analyzing the oily phase after the reaction, the DHP yield was determined. The results are summarized also in Table 2.
TABLE 2__________________________________________________________________________Example Periph. Feed Consu-or Speed of Reac- Reac- Aqueous Phase Weight Rate mption DHPComp. Agitat. tion tion H.sub.2 O.sub.2 H.sub.2 SO.sub.4 Ratio of of YieldExample Device Time Temp. Conc. Conc. O/W H.sub.2 O.sub.2 H.sub.2 O.sub.2 (moleNo. Type of Reactor (m/sec) (min.) (°C.) (wt. %) (wt. %) *1 *2 *3 %)__________________________________________________________________________Exam. 13-Stage Mechanical Agi- 1.1 15 49 48 19 27 1.5 1.5 87tation Reactor AssemblyExam. 23-Stage Mechanical Agi- 3.8 5 49 48 19 27 1.5 1.5 89tation Reactor AssemblyExam. 33-Stage Mechanical Agi- 11 1.5 49 48 19 27 1.5 1.5 90tation Reactor AssemblyComp.3-Stage Mechanical Agi- 0.85 15 49 48 19 27 1.5 1.5 85Exam. 1tation Reactor AssemblyExam. 4Tubular Reactor -- 15 50 50 15 29 1.5 1.5 86Exam. 5" -- 30 45 48 19 28 1.5 1.5 87Comp.Tank Reactor with -- 10 49 24 12 1.6 16 3.0 88Exam. 2Mechanical Agitation__________________________________________________________________________ Notes: *1 Weight ratio of the oily phase/aqueous phase *2 Feed rate = [moles of H.sub.2 O.sub.2 in aq. phase supplied]/[mole of HHP in oily phase supplied *3 Mole ratio of H.sub.2 O.sub.2 /HHP
As shown in Table 2, the over-all DHP yields for Examples 1-3 were compared to that of Comparison Example 2. Therefore, it is clear that the performances realized by Examples 1-3 are superior in respect of apparatus, processibility, amount of hydrogen peroxide and of the acid catalyst and so on. It is furthermore made clear that the reaction time can be reduced for the case where the peripheral speed of the agitation device is over 1 m/sec by comparing the results of Examples 1-3 with those of Comparison Example 1.
|
A process for the production of dihydric phenoles by oxidizing diisopropylbenzenes, which comprises oxidizing diisopropylbenzenes with molecular oxygen to obtain a reaction product mixture (A) containing at least diisopropylbenzene dihydroperoxide (DHP) and diisopropylbenzene monocarbinol monohydroperoxide (HHP), supply said product mixture (A) in a form of oily phase as a solution in an aromatic hydrocarbon solvent to an agitation reactor, supplying thereto at the same time, as an aqueous phase, hydrogen peroxide at a feed rate of 1-5 moles per mole of HHP contained in the product mixture and an acid catalyst in an amount sufficient to reach a concentration in the aqueous phase of 10-40% by weight, the concentration of hydrogen peroxide in the aqueous phase being maintained at a value of at least 20% by weight and the weight ratio of the oily phase/aqueous phase being at least 10, causing oxidization of the HHP into DHP by hydrogen peroxide while maintaining the reaction temperature at 30°-60° C. to obtain a reaction product mixture (B), separating the aqueous phase from the oily phase in the reaction product mixture (B) and subjecting the DHP in the so separated oily phase to an acid cleavage to form corresponding dihydric phenol. The process permits to dispense with the removal of the reaction water, recirculation of the aromatic hydrocarbon and of the aqueous phase, while allowing a higher ratio of oily phase/aqueous phase and thus allowing reduction of the requisite amount of hydrogen peroxide and of the acid catalyst with simultaneous decrease in the reaction time.
| 2
|
CROSS REFERENCE TO RELATED PATENT APPLICATION
[0001] This application claims priority from the provisional patent application, Serial Number 60/273,850, filed Mar. 7, 2001, and the subject matter of which is incorporated herewith by reference.
TECHNICAL FIELD
[0002] The present invention relates to implantable devices, such as stents, used for implantation in tissue for cardiovascular intervention and other purposes and the delivery of drugs placed on or in the stent. In particular, the present invention relates to a stent prepared to deliver drugs when heated by electromagnetic fields and a method and system for causing drug-coated or drug-loaded stents to deliver their drugs into the blood stream of a cardiovascular vessel or into surrounding tissue.
BACKGROUND OF THE INVENTION
[0003] Different techniques are known to prevent in-stent restenosis of cardiovascular or other stents. In-stent restenosis affects nearly 50% of all stenting procedures. Known techniques to prevent in-stent restenosis are the use of radioactive stents (brachytherapy), biodegradable stents, drug-coated stents and inductive heating of stents.
[0004] Stents can be coated or loaded with different drug formulations, including materials such as biologically active micro-spheres used for controlled release of biologically active agents inhibiting restenosis of the stent. These drugs can be included in encapsulations such as polyethylene glycol substances that are formulated to dissolve within a period of time to release the biologically active micro spheres into the vessel wall of the organ or the vessel in which the stent is located.
[0005] One problem with these drug-coated and drug-loaded stents is that the dissolving or eluting mechanism of the drug is not controllable or selectable by the physician. Whatever time release is designed into the drug coating or loading, together with conditions within the patient, will cause the drug to be delivered in a manner that cannot be controlled or selected once the coated or loaded stent is inserted. Thus, the drug effect will continue to run its course. If the drug is designed to have an inhibiting effect on tissue growth, that effect may go too far and actually be deleterious to the tissue. This problem is addressed by this invention.
SUMMARY OF THE INVENTION
[0006] An object of the present invention is to provide a mechanism for controlling the delivery or activity of a drug placed on or in a drug-delivery stent and to provide such control non-invasively from outside the patient's body. In German Gebrauschmuster DE 295 19 982.2 and in European patent application EP 1 036 574 A1 inductive or hysteresis-loss methods for heating up stents non-invasively with electromagnetic fields have been presented. The stated purpose of this heating is to prevent or retard cell growth in the regions adjacent the stent. The heating of the stent is contemplated to be sufficient to render the cells adjacent the stent non-viable.
[0007] During inductive heating as described in, e.g., patent DE 295 19 982.2 the stent heats up from normal body temperature of 37.6° C. to higher temperatures, typically above 40° C. The heat energy can then be used in several different ways to control activity of a drug that is coated on or loaded in a stent. First, the heat within a stent can be used to activate a heatsensitive drug-releasing material (e.g., a fiber) from which the stent is made. The heat thus makes available a drug that is otherwise captured within the stent material and is wholly or largely not available for activity with adjacent tissue. With a properly-selected drug-releasing material, the opposite effect is also possible, i.e., that heat deactivates the material or prevents or inhibits release. Second, the heat within the stent is conducted by thermal heat conduction to the outer surface of the stent. If a drug coating is at that surface, the heat can be used to activate a drug that is wholly or largely inactive at normal body temperatures. Alternatively, if the drug is contained in a heat-sensitive release coating that is on the stent surface, the heat energy at the stent surface can cause the drug to be released, so that it can diffused or dissolved into adjacent tissue. Again, with a properly selected drug formulation, heating to cause drug deactivation or inhibition of drug release is also possible. Third, as the heat energy at the stent surface travels by heat conduction into the tissue adjacent the stent, the proteins and other molecules in the tissue will also become heated. Thus, not only is the drug released, but the microenvironment in which the drug and adjacent tissue interact will be heated. This heating may enhance or otherwise affect the drug-tissue reactions in ways that are not present when one or both are at lower temperatures.
[0008] In one particular embodiment, the drug coated on or loaded in the stent is a restenosis-preventing drug. According to the above possibilities, the drug can be released by elevated temperatures from within or at the surface of the stent, it can be activated (or deactivated) by elevated temperatures at the stent surface and/or the drug-adjacent tissue reaction can be enhanced by elevated temperatures in the stent or at its surface and also in the adjacent tissue.
[0009] The present invention uses the stent heating method to provide control over delivery of one or more drugs from a drug-coated or drug-loaded stent. The dissolution and/or dispersion of a drug is usually a function of temperature. The higher the temperature is, the faster the drug will dissolve or disperse into the surrounding medium from the surface where it is placed. Duration of the elevated temperature also plays a role in increasing the amount of drug delivered.
[0010] According to the present invention, a stent can be made for selective drug delivery by placing the drug to be delivered onto the stent in such a way that it is encapsulated in a release layer, or the drug can be coated on the stent directly without such a layer. In the latter case, the drug on the stent is not removed from encapsulation by heating. Rather it is selected and/or formulated so that it has its active effect when it and/or the surrounding tissue is at or above an elevated threshold temperature; when the drug and/or the surrounding tissue is below the elevated threshold temperature, the drug has no active effect.
[0011] Although stents prepared with variety of drugs that can be delivered in this way are possible, one application is a stent bearing a drug that would help prevent restenosis from occurring. We propose a stent to deliver or activate a restenosis-preventing drug. The drug may be located directly on the surface of the stent or within the stent or inserted in an encapsulation layer on the surface of the stent. In all cases the stent-carried drug will not be available or be active at body temperature, but it becomes available or active at a certain temperature point above body temperature. (The reverse effect of a drug active at body temperature and selected to become inactive is also possible and may be useful.) The invention also involves a treatment method. In order to make the drug available or active at the stent surface, the stent with the drug has to be heated. The patient will come to the hospital in a defined sequence to be treated for a certain period of time with stent heating to certain temperatures selected based on the drug and/or its encapsulation and/or the drugtissue interaction at various layers. The drug then will be delivered into or at the patient's blood or vessel wall.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a schematic, cross-sectional view of a stent with a layer of encapsulated drug material on the stent surface.
[0013] [0013]FIG. 2 is a schematic, cross-sectional view of a stent with drug layer that is on the stent surface and not encapsulated.
[0014] [0014]FIG. 3 is a schematic, cross-sectional view of a stent with drug material captured within the stent material.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0015] [0015]FIG. 1 shows an embodiment of the invention. A thin-walled stent 20 of generally cylindrical shape is shown inserted within tissue, where such tissue may be the interior of a blood vessel with opposing walls 10 enclosing the stent 20 . On the exterior of the stent 20 is a layer of drug material 40 , which is in direct contact with the tissue 10 . (In reality, the stent 20 will normally be woven wires or a grid of some kind; thus, the “exterior” of the stent 20 is not solely the outer surface of the cylindrical form of the stent, but also includes other portions of the stent 20 that contact the tissue 10 , whether these are on the outer surface of the cylindrical form or the inner surface or interstitial surfaces in between the two.) In this embodiment, the drug material 40 comprises an active drug dispersed in an encapsulation material that prevents the active drug from having effective contact with the tissue 10 at normal body temperatures. However, at elevated temperatures, the encapsulation material that is part of the drug material 40 breaks down to release the active drug and permit molecules of the active drug to interact with molecules of the tissue 10 .
[0016] For example, the active drug can be a restenosis-preventing drug. The restenosis preventing drug is inserted into or encapsulated in a biodegradable polymer, such as a polyethylene glycol composition, to form the drug material layer 40 . The stent 20 is then heated at a temperature of 39° C. and the biodegradable polymer dissolves. This makes the drug available to contact or interact with the tissue 10 surrounding the stent 20 . In fact, the drug will in most cases diffuse somewhat into the surrounding tissue, thus making its active effect available not only at the exterior of the stent 20 , but also at small distances therefrom. Preferably, the heating is applied non-invasively. This can be done by a radio frequency generator device that generates an electromagnetic field sufficient to cause inductive (and/or hysteresis loss) heating in the stent. Such devices are described in Gebrauchsmuster DE 295 19 982.2 and in European patent application EP 1 036 574 A1. When the inductive heating treatment is turned off, the stent 20 will cool down to normal body temperature and the heat-activated process stops. This procedure can be repeated several times. (As noted above, the opposite effect is also possible, i.e., that heat deactivates the material or prevents or inhibits release.) As long as the supply of the drug material is not exhausted, more of the encapsulation layer will break down and more of the active drug will be released.
[0017] Another embodiment is shown in FIG. 2. A thin-walled stent 120 of generally cylindrical shape is shown inserted within tissue, where such tissue may be the interior of a blood vessel with opposing walls 110 enclosing the stent 120 . On the exterior of the stent 120 is a layer of drug material 140 , which is in direct contact with the tissue 110 . (In reality, the stent 120 will normally be woven wires or a grid of some kind; thus, the “exterior” of the stent 120 is not solely the outer surface of the cylindrical form of the stent, but also includes other portions of the stent 120 that contact the tissue 110 , whether these are on the outer surface of the cylindrical form or the inner surface or interstitial surfaces in between the two.) In this embodiment, the drug material 140 comprises an active drug that is formulated so that it has substantially no effect on the tissue 110 at normal body temperatures. However, at elevated temperatures, the active drug undergoes a change that makes it active. Thus, the previously substantially inert molecules of the active drug begin to interact with molecules of the tissue 110 . (As noted above, with a properly selected drug formulation, heating to cause drug deactivation or inhibition of drug release is also possible.) This effect can be achieved by heating that causes changes in the activity level of either the active drug with which the stent is coated or by changes in the activity level of proteins or other molecules in the tissue 110 with respect to the active drug. That is, heating may have an effect on the reaction speed or nature of the interaction of the active drug and the tissue 110 at the drug-adjacent tissue interfaces.
[0018] A further embodiment is shown in FIG. 3. A stent 220 of generally cylindrical shape is shown inserted within tissue, where such tissue may be the interior of a blood vessel with opposing walls 210 enclosing the stent 220 . The walls 240 of the stent 220 are impregnated or loaded with drug material, which is mainly not in direct contact with the adjacent tissue 210 . In this embodiment, the drug-loaded walls 240 contain an active drug that is formulated into the wall material so that it has substantially no effect on the adjacent tissue 210 at normal body temperatures. However, at elevated temperatures, the active drug is released from within the walls 240 . Thus, the previously substantially unavailable molecules of the active drug begin to interact with molecules of the adjacent tissue 210 . This effect can be achieved by heating that causes changes in the binding of the active drug with which the stent is loaded or by actual dissolution of the walls 240 loaded with the active drug. That is, heating may have an effect on the release of the active drug from the walls 240 or the integrity of the walls 240 . In either event, the heating of the stent causes increased availability of the active drug at the drug-adjacent tissue interfaces.
EXAMPLES
[0019] The herewith claimed method of heating stents to heat a drug layer applied to the stent and heat surrounding tissue may help other drug delivery techniques to deliver their drugs in a controllable or selective way.
EXAMPLES ARE
[0020] In U.S. Pat. No. 5,980,566 an iridium oxide coating for a stent has a biodegradable carrier of drugs applied thereto for beneficial localized action, as by incorporating into the carrier along the inward-facing surface an anticoagulant drug to reduce attachment of thrombi with blood flow through the lumen of the stent. Heat delivered through the method as claimed here could selectively enhance drug release or availability to help the process to reduce the attachment of thrombi with blood flow through the lumen of the stent.
[0021] In U.S. Pat. No. 5,980,551 (see also PCT application W098/34669) a stent has biologically active micro spheres that release a biologically active agent into the vessel wall or organ. To inhibit restenosis of the stent the biologically active micro spheres include encapsulated PGE1 in a water soluble polyethylene glycol mix. The temperature increase process as described here could help selectively control the period of time to dissolve and release the PGE1 into the vessel wall or organ.
[0022] In the U.S. Pat. No. 5,980,551 an anti-coagulation drug is incorporated into a biodegradable material to form a liquid-coating material. The temperature process as described in the present invention could help to continue this integrated coating which is less than about 100 microns.
[0023] In the application described in U.S. Pat. No. 5,733,327 the temperature elevating process described in the present invention could help selectively control the dissolution mechanism of poly-e-caprolactone, poly-D, L-deca-lactone, poly-dioxane and copolymer.
[0024] In the application described in U.S. Pat. No. 5,700,286 the process as described in the present invention could help enhance effectiveness for the lubricious material, which can be polyethylene, oxide, polyethylene glycol, polyethylene acetate, polyvinyl pyrrolidone, polyvinyl alcohol, polyacrylamide, hydrophilic soft segment urethanes, some natural gums, polyanhydrides or other similar hydrophilic polymers, and combinations thereof.
[0025] In the application described in PCT patent WO 00/56376 the temperature method as described in the present invention could help selectively degrade devices formed of polyhydroxylkanoates. These are taught as used in conjunction with metal that can be inductively heated.
[0026] In the application described in German patent application DE 197 37 021 A1 the method as described in the present invention could help selectively oxidize the medical implant which is made of magnesia, iron or zinc or other suitable materials.
[0027] In the application described in PCT application WO 96/33757 the temperature treatment of the present invention could help selectively control the process of dissolving the surface coating with a physiological acceptable polymer, such as polyvinyl alcohol or fibrinin, containing dissolved or dispersed therein a nitroso compound, such as 2-metyhyl-2-nitrosopropane.
[0028] In the application described in German patent application DE 195 14 104 A1 the method as described in the present invention could support the selective dissolution of the drug such as poly-D, L-lactide, thrombine inhibitors and other derivates.
[0029] Inductive Heating
[0030] Heating of stents as contemplated by this invention can be performed with metallic stents having adequate magnetic permeability or field absorbing qualities according to the teachings of German Gebrauchsmuster DE 295 19 982.2 and European patent application EP 1 036 574 A1. (The disclosures of these are incorporated by reference.) In these, electromagnetic fields are generated at a coil or other sending antenna and the stent is placed in the field with an orientation and at a distance and location that permit sufficient power to be absorbed at the stent (acting as a receiving antenna), such that heat can be generated in the stent. The amount of heat energy delivered to stent and the duration of heating are important variables for the drug activity selective control contemplated by this invention. The electromagnetic energy may be provided in controlled, brief pulses to permit a more precise control of the energy delivered to the stent and resulting heating effects. The greater the control of heating, the greater the control of the resulting drug release, or drug activation or drug-adjacent tissue reaction enhancement.
[0031] As used herein, a “stent” is any implantable device that provides some support or structure to surrounding tissue. Thus, the invention is applicable to a variety of stents or supporting implantable devices, not just those that are used in blood vessels. As used herein, a “drug” means a substance that has therapeutic effect, which may include gene therapy formulations as well as more conventional drugs based on chemical formulations or biological derivatives.
[0032] It is appreciated that besides stents, any other type of suitable implantable devices can be used within the scope and spirit of the present invention to controllably elute a drug off of an implantable device. Also, the implantable devices may be used just for the purpose of eluting drugs into the body. One of such implantable devices may be a metallic hip joint which is coated with a drug for better biocompatibility. The drug may be eluted by temperature. Also, a device may be made as a ball shaped type or as many small pills which are implanted just to be heated inductively to elute the drug. Thus, the invention is applicable to any implantable object (whether or not it has a prosthetic or other function) that has the ability to be heated in the manner described herein so as to cause drug release and that can be placed in a position at which or from which drug delivery is desired.
[0033] It is also appreciated that the devices can be temporarily implanted or permanently implanted. These device may be used to help chemotherapy or any other therapy.
[0034] One exemplary application can be to implant a metallic coil or pellet in the patient's prostate and use the above described invention to control the elution of a drug to treat a prostate disease. Other exemplary applications may be to control the elution of insulin off of an implantable device in a diabetic patient, or to control the elution of a drug off of an ophthalmic device in the eye to treat vision related diseases.
[0035] Accordingly, the present invention provides an implantable device having at least one coated drug material capable of being heated inductively and delivering the drug material to a body when heated. The frequency of the inductive heat is preferably below 1 MHz. Under 1 MHz, the body tissue is generally opaque for radio frequency inductive heating, above that frequency the body tissue absorbs the energy and is heated itself.
[0036] While the present invention has been described with reference to several embodiments thereof, those skilled in the art will recognize various changes that may be made without departing from the spirit and scope of the claimed invention. For example, implantable devices can be energized by inductive heating, radio or microwave frequency and tissue transmitting light technology, etc. It is noted that light of certain lower wavelength can travel further into tissue than light of a higher wavelength and, therefore, is absorbed deeper in the tissue. This effect can be used to absorb the light deeper to heat up implants deeper in the tissue. Accordingly, this invention is not limited to what is shown in the drawings and described in the specification but only as indicated in the appended claims, nor is the claimed invention limited in applicability to one type of drug. Any numbering or ordering of elements in the following claims is merely for convenience and is not intended to suggest that the ordering of the elements of the claims has any particular significance other than that otherwise expressed by the language of the claims.
|
A method for controlling the activity of drugs on or in drug-coated or drug-loaded implantable devices, such as stents or other metallic devices, uses non-invasive, inductive heating of such device. The heating of a device, such as stent, can be used to release drugs applied to the stent in release layers, to activate drugs on the stent that have little or no activity at body temperature and to enhance for defined periods the reaction environment at the stent for drug-adjacent tissue interactions. Reverse effects of deactivation of drugs upon heating are also possible.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable.
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
Not Applicable.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to apparatus and methods for attenuating sound.
More particularly, the invention relates to a sound attenuation system installed on the upper floor of a building structure to reduce the volume of sound which travels from beneath the floor, through the floor, and into the living space above the floor.
In a further respect, the invention relates to a sound attenuation system of the type described which—in comparison to similar existing systems—employs materials that typically cost less, which requires less expense and labor to install, and which attenuate sound to a greater degree.
(2) Description of the Related Art Including Information Disclosed Under 37 CFR 1.97 and 1.98
In buildings including two or more stories, it is common practice to include sound attenuating material on upper floors. The sound attenuating material minimizes the volume of sound traveling upwardly from a room under an upper floor, through the upper floor, and into the room above the upper floor. Sound attenuating material functions by reflecting sound waves, absorbing sound waves, and/or disrupting sound waves. Conventional sound absorbing material comprises sheets of cork, asphalt, or other materials. The asphalt is typically about eighty percent tar, the remainder including clay, solvents, and other fillers. One disadvantage of asphalt is that with time, it tends to harden. It also hardens in cold weather. When the asphalt hardens, it tends to crack if the floor expands or contracts, or if a crack develops in the floor. Another disadvantage of asphalt is that prior to applying asphalt to a floor, a solvent must be applied. The solvent softens the asphalt and causes it to stick to the floor. Similarly, to apply cork, a mastic or adhesive must be utilized to cause the cork to adhere to the floor. Since cork comprises a matrix of particles pressed together, the cork also tends to develop cracks if a crack in the floor develops, or if the floor expands or contracts.
Accordingly, it would be highly desirable to provide a sound proofing system which did not require the use of an adhesive or solvent to apply a sound attenuating material, which would expand and contract with a floor, and which would not develop cracks when a crack developed in the floor supporting the sound proofing system.
Therefore, it a principal object of the invention to provide an improved sound attenuating system and method of installing the same on the upper floor of a building structure.
A further object of the invention is to provide an improved sound attenuating system which expands and contracts with the floor on which the system is applied.
Another object of the invention is to provide an improved sound attenuating system which can be applied directly to the upper floor of a building structure without pretreating the floor with a solvent or adhesive.
Still a further object of the invention is to provide an improved elastomeric sound attenuation system which remains pliable over extended periods of time.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
These and other, further and more specific objects and advantages of the invention will apparent to those skilled in the art from the following detailed description thereof, taken in conjunction with the drawings, in which:
FIG. 1 is a perspective view illustrating a building structure with a portion of the upper floor thereof enlarged to display a sound attenuation system constructed in accordance with the invention installed thereon;
FIG. 2 is a side section view illustrating an elastomeric laminate sheet used in the sound attenuation system of the invention; and,
FIG. 3 is a block flow diagram illustrating a method for installing a sound attenuation system in accordance with the invention.
BRIEF SUMMARY OF THE INVENTION
Briefly, in accordance with the invention, I provide an improved method for attenuating sound in a building structure. The building structure includes at least one upper floor. The method includes the steps of obtaining a sheet of an uncured sticky elastomeric material having a first side and a second side spaced apart from and opposing the first side; obtaining a sheet of backing material peelable from the first side when applied thereto; applying the sheet of backing material to the first side; obtaining a fabric layer; applying the fabric layer to the second side; the elastomeric sheet, sheet of backing material, and fabric layer collectively forming an elastomeric laminate; transporting the elastomeric laminate to the building structure; selecting a surface on the upper floor in the building structure; removing the sheet of backing material from the first side; applying the first side directly to the surface on the upper floor; and, applying flooring to the fabric layer.
In another embodiment of the invention, I provide an improved method for attenuating sound in a building structure. The building structure includes at least one upper floor. The method includes the steps of obtaining a sheet of an uncured sticky elastomeric material having a first side and a second side spaced apart from and opposing the first side; obtaining a fabric layer; applying the fabric layer to the second side; the elastomeric sheet and fabric layer collectively forming an elastomeric laminate; transporting the elastomeric laminate to the building structure; selecting a surface on the upper floor in the building structure; applying the first side directly to the surface on the upper floor; and, applying flooring to the fabric layer.
In another embodiment of the invention, I provide an improved method for attenuating sound in a building structure. The building structure includes at least one upper floor. The method includes the steps of obtaining a plurality of strips of an uncured sticky rubber material each having a first side and a second side spaced apart from and opposing the first side; obtaining a plurality of fabric layers; applying each fabric layer to the second side of one of said strips of elastomeric material; each elastomeric strip and fabric layer collectively forming an elastomeric laminate strip; transporting the elastomeric laminate strips to the building structure; selecting a surface on the upper floor in the building structure; applying the first side of each elastomeric laminate strip directly to the surface on the upper floor in overlapping relationship; and, applying flooring to the fabric layers.
DETAILED DESCRIPTION OF THE INVENTION
Turning now to the drawings, which describe the presently preferred embodiments of the invention for the purpose of describing the operation and use thereof and not by way of limitation of the scope of the invention, and in which like reference characters refer to corresponding elements throughout the several views, FIG. 1 is a perspective view of a building structure 10 including at least one upper floor 11 . A sound attenuation system constructed in accordance with the invention is included on upper floor 11 to attenuate sound traveling upwardly from the space 40 in the room beneath floor 11 .
The building structure can comprise a residence, a commercial building, a warehouse or another building in which individuals live or work.
Floor 11 includes, in conventional fashion, plywood sheet 16 nailed or otherwise fastened to the top of two-by-fours 17 , 18 or other horizontally oriented joists or supports. Sheet rock 26 is fastened to the bottom of two-by-fours 17 , 18 and forms the ceiling of the basement or other room which is beneath floor 11 . As is well known, concrete or any other desired building material can be utilized in place of plywood, two-by-fours, and/or sheet rock 26 .
Soundproofing material is applied to floor 11 and comprises a sheet 13 of uncured elastic sticky rubber material including about 64% by weight of a mixture of uncured butyl-isoprene rubber and styrene-butadiene rubber, 33.4% by weight of calcium carbonate particle filler, and 2.6% by weight crystalline silica particle filler. Since the rubber is uncured (i.e., has not been heated and baked) it is unusually sticky, and readily bonds to many surfaces, including most, if not all, floor surfaces like wood, tile, concrete, etc. Sheet 13 includes a generally flat upper surface 14 opposed to and spaced apart from a generally flat lower surface 15 . One reason surface 15 of sheet 13 readily adheres to a floor surface is that surface 15 ordinarily, but not necessarily, is a continuous flat, smooth surface with few, if any, indentations or holes formed in surface 15 . Further, if a floor 16 surface has depressions or upraised areas, elastic surface 15 tends to conform and adhere to such depressions and upraised areas such that surface 15 is adhering to floor 16 at the great majority of points on surface 15 . Such a smooth, continuous adherence of surface 15 to floor 16 is believed, or hypothesized, to be one of the reasons for the unexpected soundproofing qualities of the soundproofing system of the invention.
The weight percent of rubber or other sticky elastomer in the sheet 13 of elastomer material can vary as desired, but is in the range of 40% to 95% by weight, preferably 50% to 80% by weight. The use of a large weight percent of uncured rubber is critical in the practice of the invention because the rubber automatically sticks to a floor surface without requiring the use of a solvent or mastic, because the rubber is elastic, because the rubber retains its elasticity for long periods of time typically in excess of twenty years or more, and because the rubber retains its elasticity at freezing temperatures. While any sticky elastomer can be utilized in the practice of the invention, natural latex rubber, butyl-isoprene rubber, styrene-butadiene rubber, and other rubbers are presently preferred.
The weight percent of particle filler in sheet 13 is in the range of 5% to 60%, preferably 20% to 50% by weight. The width of each particle is in the range of 0.001 inch to 2.00 inches, preferably 0.01 to 1.00 inch. As used herein, the term width means the greatest dimension of a particle. For example, if a particle is a fiber that is one inch long and 0.1 inch wide, then the “width” of the fiber is one inch. If the particle is spherical and has a diameter of 0.2 inch, then the “width” of the particle is 0.2 inch. If a particle is elliptical and the long axis of the particle is 0.3 inch and the short axis of the particle is 0.25 inch, then the “width” of the particle is 0.3 inch. If a particle has an irregular shape and the greatest width of the particle is 0.12 inch, then the “width” of the particle is 0.12 inch.
The particle filler material is believed, or hypothesized, to disrupt or deflect sound waves, although specific tests have not been performed to confirm such. It is believed this is one of the reasons that the soundproofing laminate of the invention has unexpected and surprising soundproofing abilities. Any desired filler can be utilized, but it is preferred that the filler not adversely affect the elasticity and adherence qualities of the rubber in the material. While calcium carbonate and silica particle fillers are presently preferred, any desired fillers can be utilized in sheet 13 .
A fabric sheet or layer 12 is attached to top surface 14 of elastic sheet 13 . The fabric sheet 12 is preferably, although not necessarily, comprised of a dense, heavy stitched fabric because mastic is applied to sheet 12 to attach and anchor tile or other floor coverings to sheet 12 . Sheet 12 is also believed to assist in attenuating sound passing through sheet 12 . Upper surface 14 adheres to sheet 12 and maintains sheet 12 in fixed position adjacent surface 14 . As shown in FIG. 2, sheet 12 can comprise woven threads 27 , 28 . Sheet 12 is typically, although not necessarily, comprised of artificial hydrophilic threads or strands of fabric such a nylon, rayon, etc.
The thickness, indicated by arrows A in FIG. 2, of layer 12 and sheet 13 can vary, but is presently about 0.37 inch. This is about 50% less than the thickness of asphalt sheets currently applied to floors to provide sound attenuation. Even though the thickness of the laminate sheet utilized in the invention is less than the thickness of a conventional asphalt sheet, the sound impact/insulation ratio of layer 12 and sheet 13 is 71/71, which is unexpectedly and surprisingly significantly better than the ratio of 55/61 found in conventional asphalt sheets. The thickness of layer 12 and sheet 13 is preferably in the range of 0.1 inch to 0.75 inch, most preferably 0.25 inch to 0.50 inch.
A backing layer 30 is applied to the bottom surface 15 of sheet 13 . While layer 30 can, if desired, be omitted, layer 30 often is a necessity practically speaking because sheet 13 is typically rolled prior to being transported. Layer 30 presently preferably comprises a pliable plastic or other polymer or other material which can be readily peeled off and separated from surface 15 without removing any of the material comprising surface 15 .
FIG. 3 is provided to illustrate, without limiting the scope of the invention, a method of employing the sound insulation system of the invention. In step 19 , a sheet of uncured rubber material is obtained. The sheet includes a sticky self-adhering backing side 14 , a sticky self-adhering application side 15 , and filler particles 31 . In step 20 , a peel-off backing 30 is applied to the application side 15 of the sheet to prevent the application side from sticking to unwanted objects or surfaces. In step 21 , a pliable hydrophilic fabric layer 12 is obtained. A hydrophilic layer is preferred, although not required, because it repels water. In step 22 , the hydrophilic fabric layer is applied to the backing side of the rubber sheet. A sound proofing elastomeric laminate is produced which includes the rubber sheet 13 sandwiched between the fabric layer 12 and the peel-off backing 30 . In step 23 , a floor surface is selected on the upper floor 16 of a building structure. The floor surface preferably is clean and dry, as is normally the case when any supplemental flooring material is to be applied to the floor surface. The floor surface is free of any solvent or adhesive. The backing material 30 is, in step 24 , peeled off the self-adhering application side (bottom surface 15 ) of sheet 13 and the sheet 13 is applied directly to the plywood surface of floor 16 . The application side adheres to the surface of floor 16 . Tile or other flooring is applied to fabric layer 12 with mastic or another adhesive or fastening material.
Layer 12 , sheet 13 , and backing 30 typically are provided in rolled up rectangular strips. A first strip is applied to a floor surface by unrolling the strip, peeling off the backing 30 , and pressing side 15 against the floor surface. A second strip is applied parallel to the first strip in similar fashion such that one edge of the second strip overlaps an edge of the first strip. The third strip is applied parallel to the second strip such that one edge of the third strip overlaps an edge of the second strip, and so on. This overlapping of strips at the juncture 41 , 42 between the strips is important in the practice of the invention. If abutting strips do not overlap, but instead simply meet along their edges, sound can more readily penetrate through any space that exists between the edges of abutting strips.
Similarly, along the baseboards at the bottom of each wall in an upper room, it is preferred that layer 12 and sheet 13 extend beneath the baseboard or extend and bend from the floor continuously up the vertical face of the baseboard for a short distance, typically one or two inches. This limits the quantity of sound that can travel from below, pass between the edge of a strip and the baseboard and into the upper room. Or, if an edge of layer 12 and sheet 13 ends at the baseboard, caulk can be applied at the edge—baseboard junction.
Having described my invention is such terms as to enable those skilled in the art to understand and practice it and having described the presently preferred embodiments and best mode thereof.
|
A new system for soundproofing floors utilizes a laminate material having a thickness that is 50% less than conventional asphalt soundproofing material but which has better sound reducing properties than the asphalt soundproofing material. The new system does not require the use of solvents inherent in conventional soundproofing systems, and, accordingly, results in significant reductions in the cost of labor incurred to install the system. The new system utilizes a laminate consisting of uncured rubber, particular embedded in the uncured rubber, and a fabric mesh.
| 4
|
[0001] This application is a national stage entry under 35 U.S.C. §371 of International Application No. PCT/GB2014/051245, filed Apr. 22, 2014, which claims the benefit of G.B. Application 1307196.4, filed Apr. 22, 2013. The entire contents of International Application No. PCT/GB2014/051245 and G.B. Application 1307196.4 are incorporated herein by reference.
TECHNICAL FIELD
[0002] This invention relates to a vacuum pump, and in particular to the lubrication of rolling bearings used to support the impeller of a vacuum pump.
BACKGROUND
[0003] Vacuum pumps typically comprise an impeller in the form of a rotor mounted on a shaft for rotation relative to a surrounding stator. The shaft is supported by a bearing arrangement comprising two bearings located at or intermediate respective ends of the shaft. One or both of these bearings may be in the form of rolling bearings. Usually, the upper bearing is in the form of a magnetic bearing, and the lower bearing is in the form of a rolling bearing.
[0004] A typical rolling bearing comprises an inner race fixed relative to the shaft, an outer race, and, located between the races, a plurality of rolling elements for allowing relative rotation of the inner race and the outer race. To prevent mutual contacts between the rolling elements, they are often guided and evenly spaced by a cage. Adequate lubrication is essential to ensure accurate and reliable operations of rolling bearings. The main purpose of the lubricant is to establish a load-carrying film separating the bearing components in rolling and sliding contact in order to minimise friction and wear. Other purposes include the prevention of oxidation or corrosion of the bearing components, the formation of a barrier to contaminants, and the transfer of heat away from the bearing components. The lubricant is generally in the form of either oil or grease (a mixture of oil and a thickening agent).
[0005] Vacuum pumps using oil-lubricated bearings require an oil feeding system for feeding oil between the contact areas of the bearing, which enables the oil to perform cooling as well as lubrication and thereby permit the bearings to run at a faster speed. Turbo-molecular pumps have traditionally used a wicking system for supplying oil to a rolling bearing. In such a system, a felt wick partially submerged in an oil reservoir feeds oil to a conical “oil feed” nut mounted on the shaft. With rotation of the pump, oil travels along the conical surface of the nut to the bearing. The oil passes through the bearing and is returned to the reservoir.
[0006] In such oil feeding systems, a pressure differential may be generated across the oil reservoir which causes outgassing in the reservoir. In static conditions when the pump is not operating but is being initially evacuated by a primary pump outgassing can cause oil to escape from the bearing cavity and contaminate the pump. Vibrational excitation during use of the pump may additionally promote the nucleation of bubbles contributing to oil loss. Over and above contamination and loss of oil, outgassing may cause an excess of oil to be transferred to the oil feed nut which may stress the bearing.
SUMMARY
[0007] The present invention seeks to reduce the effect of outgassing in vacuum pumps.
[0008] The present invention provides vacuum pump comprising a bearing and a lubricant supply system for lubricating the bearing; the lubricant supply system comprising: a lubricant reservoir comprising a reservoir matrix for receiving a lubricant; a lubricant transfer arrangement in contact with the reservoir matrix for transferring lubricant from the reservoir matrix to the bearing, the reservoir comprising a reservoir enclosure for locating the reservoir matrix in position relative to the lubricant transfer arrangement; wherein the reservoir comprises a plurality of contact regions at which the reservoir matrix is in contact with the reservoir enclosure for locating the reservoir matrix in position relative to the lubricant transfer arrangement and a plurality of spacing regions between respective contact regions at which the reservoir matrix is spaced apart from the reservoir enclosure for receiving gas and lubricant foam caused by outgassing in the lubricant in the reservoir matrix.
[0009] Other preferred and/or optional aspects of the inventions are defined in the accompanying claims.
BRIEF DESCRIPTION OF DRAWINGS
[0010] In order that the invention may be well understood, an embodiment thereof, which is given by way of example only, will now be described with reference to the accompanying drawings.
[0011] FIG. 1 shows a section of a vacuum pump.
[0012] FIG. 2 shows a section of a lubricant supply system of the vacuum pump shown in FIG. 1 .
[0013] FIG. 3 shows a cross-section a known lubricant supply system.
[0014] FIG. 4 shows the known lubricant supply system in use.
[0015] FIG. 5 shows a radial cross-section of an improved lubricant supply system taken along line V-V of FIG. 6 .
[0016] FIG. 6 shows a section of the lubricant supply system taken along line VI-VI of FIG. 5 .
[0017] FIG. 7 shows the arrangement of FIG. 6 in use.
DETAILED DESCRIPTION
[0018] Referring to FIG. 1 , a cross-section of a vacuum pump 10 is shown comprising a pumping arrangement driven by a shaft 12 . The illustrated vacuum pump is a turbomolecular vacuum pump comprising a turbomolecular pumping mechanism 14 and a molecular drag pumping mechanism 16 . The turbomolecular pumping mechanism comprises a plurality of rotor blades 18 mounted on, or integral with, the shaft 12 . The molecular drag pumping mechanism 16 is in the form of a Holweck pumping mechanism, and comprises one or more cylinders 20 mounted on the shaft 12 . The molecular drag pumping mechanism may alternatively comprise a Siegbahn mechanism comprising rotating discs. There may be additional or alternative mechanisms such as an aerodynamic pumping mechanism downstream of the molecular drag pumping section, comprising a regenerative mechanism.
[0019] The shaft is rotated about longitudinal axis 22 by a motor 24 to drive the pumping arrangement. The shaft 12 is supported by a bearing arrangement comprising two bearings which may be positioned either at respective ends of the shaft as shown or alternatively intermediate the ends. In FIG. 1 , a rolling bearing 26 supports a first portion of the shaft 12 and a magnetic bearing 28 supports a second portion of the shaft 12 . A second rolling bearing may be used as an alternative to the magnetic bearing 28 . When a magnetic bearing is used, it may also be desirable to incorporate a back-up bearing.
[0020] The rolling bearing 26 is provided between the second end portion of the shaft 12 and a housing portion 30 of the pump 10 . With reference also to FIG. 2 , the rolling bearing 26 comprises an inner race 32 fixed relative to the shaft 12 , an outer race 34 , and a plurality of rolling elements 36 , supported by a cage 38 , for allowing relative rotation of the inner race 32 and the outer race 34 .
[0021] The rolling bearing 26 is lubricated by a lubricant supply system 40 to establish a load-carrying film separating the bearing components in rolling and sliding contact in order to minimise friction and wear. The lubricant supply system 40 comprises a liquid lubricant reservoir 42 , which surrounds an axis of rotation 22 of the shaft 12 . The reservoir 42 comprises a reservoir matrix formed in this example by a stable fibrous annular substrate surrounding a central bore 44 of the reservoir 42 , and having voids within which oil, or other liquid lubricant, is stored. The reservoir 42 comprises at least one and preferably a multiplicity of projections 46 which project into the bore 44 . The projections may be made from a similar fibrous material, such as felt, or by filaments forming brushes.
[0022] The projections are held by the reservoir 42 so that they are in contact with a tapered feed nut 48 mounted on the shaft 12 and located within the bore 44 of the reservoir. The end of the tapered nut located adjacent the bearing 26 has an external diameter which is approximately equal to the internal diameter of the cage 38 of the bearing. In this embodiment, the projections are located approximately mid way along the axial length of the reservoir 42 . However, this location is arbitrary and the axial location of the projections may vary from one vacuum pump to another. In another example, the projections or fingers may be omitted and in this case, the annular body of the reservoir matrix may be located in contact with the lubricant transfer arrangement, so that an interior surface contacts the oil feed nut 48 over at least a portion of the axial extent of the matrix. Lubricant can therefore be transferred from the interior surface of the matrix directly to the lubricant transfer arrangement. In a modification of this latter example, the reservoir matrix may extend radially inwardly to a greater extent at one axial portion, for example a middle portion, to contact the oil feed nut. The matrix may be formed by more than one component stacked one on another in layers and one of the layers may project further inwards than the layers adjacent to it in order to contact the oil feed nut.
[0023] In use of the illustrated example, the lubricant is drawn along the projections 46 and is deposited onto the feed nut 48 as it rotates. This lubricant is transferred axially along the feed nut to the cage 38 of the bearing 26 by virtue of the taper on the nut and the rotation of the nut.
[0024] FIG. 3 is a cross-section taken along line III-III in FIG. 2 looking towards the bearing 26 and shows a prior art lubricant supply system. In this system, the external surface 50 of the reservoir matrix 42 is in contact with the internal surface 52 of the housing portion 30 throughout the circumference of the surfaces. The reservoir material is to some extent resilient and its shape is at least partially formed by its location within the housing portion, which acts as a reservoir enclosure containing the matrix. In this example, the internal surface of the housing portion 30 has a circular cross-section which is uniform in the axial dimension forming a cylindrical surface. The external surface similarly has a circular cross-section of the same radius, or marginally larger, than the radius of the internal surface. The external surface is also uniform in the axial dimension forming a cylinder.
[0025] FIG. 4 is a view similar to FIG. 2 and shows the known lubricant supply system shown in FIG. 3 in use filled with a lubricant. The reservoir matrix 42 is constrained radially in the bore of the reservoir enclosure 30 and also axially by a further housing portion 54 underneath the reservoir in the illustrated orientation of the pump. During pumping, or when there is a differential pressure across the reservoir produced by initial evacuation by a primary pump, outgassing occurs in the reservoir matrix 42 causing trapped gas and microscopic bubbles 56 to “sweep” lubricant both radially inwards through the reservoir material into the bore 44 of the reservoir towards the oil feed nut 48 and axially towards the bearing 26 , as shown by the horizontal and vertical arrows, respectively. The lubricant lost from the reservoir generates a lubricant foam 58 which is highly mobile within the pump and can readily be transferred for example into regions where the presence of lubricant is undesirable thereby contaminating the pump or into the bearing causing it to be over-lubricated. The freshly nucleated bubbles increase in size as they travel towards the bore 44 and top of the matrix. An ever increasing volume of foam accumulates in the limited available volume.
[0026] FIGS. 5 and 6 show an improved lubricant supply which at least mitigates the problems caused by outgassing and the generation of lubricant foam. FIG. 5 is a view similar to FIG. 3 and shows a cross-section through the lubricant supply system taken along the line V-V in FIG. 6 . FIG. 6 is a view similar to FIGS. 2 and 4 taken along line VI-VI in FIG. 5 . A view taken along line II-II in FIG. 5 would show an arrangement which is the same as the prior art in FIG. 2 because the section is taken through the contact portions 64 , as described in more detail below.
[0027] Referring to FIGS. 5 and 6 , the lubricant supply system 60 comprises a reservoir matrix 62 for receiving and storing a lubricant, such as oil, for transfer by the lubricant transfer arrangement from the reservoir matrix to the bearing 26 . The reservoir matrix is located in position relative to the lubricant transfer arrangement by the housing portion 30 and the axial housing portion 54 , which form together a reservoir enclosure.
[0028] The reservoir comprises a plurality of contact regions 64 at which the reservoir matrix 62 is in contact with the reservoir enclosure 30 for locating the reservoir matrix in position relative to the oil feed nut 48 and a plurality of spacing regions 66 between respective contact regions at which the reservoir matrix is spaced apart from the reservoir enclosure for receiving a lubricant foam caused by outgassing in the lubricant in the reservoir matrix. In a modified arrangement, the reservoir enclosure may comprise locating means which project radially inward from the enclosure wall to contact and locate the reservoir matrix. In this arrangement, the spacing regions may be substantially continuous around the periphery of the matrix.
[0029] The spacing regions 66 provide an escape, or expansion, volume around the outer periphery of the matrix and distal from the matrix bore 44 into which trapped gas can expand or be transferred. Gas trapped in the reservoir matrix when the matrix is initially charging with oil can escape into the peripheral volume and bubbles generated during pumping can expand into the volume which provides a continuous pumping conductance at the periphery of the matrix which mitigates the effects of foaming. Since the reservoir matrix is no longer constrained by the housing portion 30 , the forces on the lubricant in the matrix are distributed both radially inwards and outwards, as shown by the horizontal arrows in FIG. 6 . Therefore, when gas escapes from the matrix it carries less lubricant with it and as a consequence, lubricant foaming is reduced. In this regard, the mean length of the escape path along which gas in the matrix has to travel in order to escape is reduced and therefore gas travelling along this shorter path accumulates less lubricant. The effect of providing an additional escape path would appear counter-intuitive since it would provide an additional means by which lubricant could be carried out of the matrix. However, to the contrary, the reduction in the mean length of the escape path reduces foaming, as illustrated in FIG. 7 which shows the lubricant supply system 60 in use.
[0030] The problems associated with the prior art lubricant supply system become worse as the radius of the reservoir increases together with the length of the escape path, particularly where the aspect ratio of radius to length increases. Therefore, the present invention has particularly utility in these types of reservoirs.
[0031] Referring to FIGS. 5 to 7 in more detail, the lubricant transfer arrangement 48 , which in this example is an oil feed nut, is located radially inward of the reservoir matrix 62 in bore 44 and has an axis of rotation 22 . The reservoir enclosure 30 is located radially outward of the reservoir matrix. The spacing regions 66 are located radially outward of the reservoir matrix around the outer periphery of the matrix. The spacing regions are separated from one another about the circumference by the contact regions 64 , which are each located between adjacent spacing regions about the circumference. The spacing regions and contact regions may be uniformly distributed about the circumference or may be irregularly distributed. A uniform spacing is however preferred since it allows gas to escape relatively consistently from all regions of the matrix.
[0032] The spacing regions are formed between an internal surface 70 of the reservoir enclosure and an external surface 72 of the reservoir matrix. In the known arrangement shown in FIG. 3 , both the internal surface of the reservoir enclosure and the external surface are cylindrical and have a circular cross-section. This arrangement does not provide a volume into which gas can escape from the matrix since the matrix is in intimate contact with the enclosure about its circumference. In the present example shown particularly in FIG. 5 , the cross-section of the reservoir enclosure remains the same but the cross-section of the matrix is hexagonal to provide six contact regions and six spacing regions between the contact regions. Whilst a hexagonal cross-section is shown in FIG. 5 , other polygonal or irregular cross-sections may be used to provide the required spacing regions for the expansion of gasses. In an alternative arrangement, the internal surface of the reservoir enclosure may have a polygonal or irregular cross-section whilst the external surface of the matrix may have a cylindrical cross-section. In further examples, one of the internal surface of the reservoir enclosure or the external surface of the reservoir matrix may comprise channels for the passage of air or ridges to define spacing regions therebetween.
[0033] As shown in FIG. 6 , the spacing regions 66 extend axially over the length of the reservoir matrix 62 . In this example, the cross-section of the matrix is uniform along the axial extent, although in other examples the cross-section may vary. The spacing regions are open at an axial end the upper of the matrix to allow gasses to be conducted away from the spacing regions. If the spacing regions were not open at at least one axial end they would form pockets which trap gas rather than letting it be conducted away from the matrix. The provision of spacing regions in gas communication with volumes away from the matrix allows gas to be readily conducted and to reduce lubricant foaming.
[0034] In use of the vacuum pump 10 and lubricant supply system 60 , the reservoir matrix 62 is initially charged with lubricant such as oil. Any gas trapped during filling of the matrix can readily escape into the spacing regions 66 , in addition to the bore 44 of the matrix, thereby reducing the propensity for lubricant foaming when the pump is in use. In operation, the motor 24 causes rotation of the turbo molecular pumping mechanism 14 and molecular drag pumping mechanism 16 about the axis of rotation 22 . In the example of a vacuum pump having these types of pumping mechanisms, pressures between about 10-3 and 10-7 mbar can be attained, and depending on the tolerances of the pump pressures as low as 10-10 mbar.
[0035] Rotation of drive shaft 12 by the motor causes rotation of the lubricant transfer arrangement, or oil feed nut, 48 . Lubricant is wicked from the reservoir matrix 62 along the finger projections 46 to the transfer arrangement and transferred to the bearing 26 . The generation of vacuum pressures in the pump, principally due to evacuation by a primary pump, generates a pressure differential across the reservoir matrix which induces bubble nucleation and outgassing in the matrix. Bubble nucleation can be accentuated by vibration caused by pump operation. Bubbles of gas are generated, in the matrix around nucleation sites, which increase in size. The spacing regions 66 located at the periphery of the matrix allow the gas bubbles to be dispersed reducing the occurrence of lubricant foaming detrimental to pump and bearing operation.
|
The present disclosure relates to a vacuum pump including a bearing and a lubricant supply system for lubricating the bearing. The lubricant supply system includes: a lubricant reservoir comprising a reservoir matrix for receiving a lubricant; a lubricant transfer arrangement in contact with the reservoir matrix for transferring lubricant from the reservoir matrix to the bearing, the lubricant reservoir including a reservoir enclosure for locating the reservoir matrix in position relative to the lubricant transfer arrangement; wherein the lubricant reservoir includes a plurality of contact regions at which the reservoir matrix is in contact with the reservoir enclosure for locating the reservoir matrix in position relative to the lubricant transfer arrangement and a plurality of spacing regions between respective contact regions at which the reservoir matrix is spaced apart from the reservoir enclosure for receiving gas and lubricant foam caused by outgassing in the lubricant in the reservoir matrix.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a U.S. National Phase Application of PCT International Application No. PCT/US2010/046897, filed Aug. 27, 2010, which claims benefit of priority from U.S. Provisional Application No. 61/237,378, filed Aug. 27, 2009. The contents of these applications are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to mounting assemblies for temporarily stowing locks, for example, bicycle U-locks and cable locks, when not in use, and for releasing the locks for ready use when needed or maintaining a portion of the lock housing during use.
BACKGROUND OF THE INVENTION
Since the invention of bicycle U-locks and cable locks, a variety of holders is have been proposed for removably carrying such a lock when the bicycle is in use, rather than parked. Such a U-lock typically comprises a semi-enclosure member or shackle having legs or fittings with configured feet, a straight crossbar having openings for reception of these feet, and a locking mechanism in the crossbar for retaining or releasing these feet. Such a cable lock typically comprises a cable having at one end a leg or fitting with a configured foot, a bar extending from the other end of the cable and having an opening for reception of this foot, and a locking mechanism in the bar for retaining or releasing this foot. For protection against theft, this tie lock assemblage ties a strut or the like of the bicycle to a post, rail or other station.
The objectives of a holder for such locks are to carry the lock securely on the bicycle frame without rattling, to position the lock inconspicuously on the bicycle frame without hindering movement of the cyclist, and yet to facilitate convenient release of the lock from the holder whenever needed. Prior art holders have not completely met these objectives.
BRIEF SUMMARY OF THE INVENTION
In one aspect, the invention provides a portable lock mounting assembly including a body defining a lock retaining mechanism and a contact surface. A strap having first and second ends is attachable to the body such that a loop facing the contact surface is defined by the strap. A cam member is supported by the body adjacent the contact surface and is pivotal between a first position wherein the cam member extends generally parallel to the contact surface and a second position wherein the cam member extends at an angle relative to the contact surface.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 shows a mounting assembly attached to a bicycle frame component and a lock member positioned in the mounting assembly.
FIG. 2 shows an exploded view of the mounting assembly.
FIGS. 3 and 4 show the mounting assembly positioned on the bicycle frame component, wherein a strap of the mounting assembly is shown in a loosened state.
FIG. 5 shows a cross-sectional view of the mounting assembly positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a loosened state.
FIG. 6 shows the mounting assembly positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a tightened state.
FIG. 7 shows a cross-sectional view of the mounting assembly positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a tightened state.
FIGS. 8 and 10 show a different mounting assembly positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a loosened state.
FIG. 9 depicts the mounting assembly of FIG. 8 in a loosened state.
FIG. 11 shows a cross-sectional view of the mounting assembly of FIG. 8 positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a loosened state.
FIG. 12 shows the mounting assembly of FIG. 8 positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a tightened state.
FIG. 13 shows a cross-sectional view of the mounting assembly of FIG. 8 positioned on the bicycle frame component, wherein the strap of the mounting assembly is shown in a tightened state.
FIG. 14 shows an underside view of the mounting assembly of FIG. 8 .
FIGS. 15 and 16 show a cross-sectional view of the mounting assembly of FIG. 8 , wherein the strap of the mounting assembly is shown in a tightened state.
FIGS. 17-24 depict exemplary steps for mounting the lock member to the mounting assembly.
DETAILED DESCRIPTION OF THE INVENTION
Although the invention is illustrated and described herein with reference to specific embodiments, the invention is not intended to be limited to the details shown. Rather, various modifications may be made in the details within the scope and range of equivalents of the claims and without departing from the invention.
Referring to FIGS. 1-7 , a mounting assembly 20 in accordance with an exemplary embodiment of the invention will be described. FIG. 1 shows mounting assembly 20 attached to a bicycle frame component 10 with a U-lock 12 supported in the mounting assembly 20 . The U-lock 12 includes a lock housing 14 and a shackle 16 . While the invention is illustrated herein with a U-lock, the invention is not limited to such and may be utilized with various portable locks, including, but not limited to, modular locks as described in PCT International Application No. PCT/US09/048,226, incorporated herein by reference. Additionally, while the mounting assembly 20 is illustrated herein attached to a bicycle frame, the invention is not limited to such, but may be utilized in various applications.
Referring to FIG. 2 , the mounting assembly 20 of the exemplary embodiment generally comprises a bracket body 22 , a strap 36 and a cam 40 . The bracket body 22 defines a lock receiving opening 24 with an end cap 26 with a slot 29 defined therein, as will be described hereinafter. The bracket body 22 includes a fixed strap support 30 and a free end strap support 32 which supports a strap buckle 34 . The cam 40 is supported on the bracket body 22 between a contact surface 23 thereof and a bracket insert 38 which defines a secondary contact surface 39 . Preferably, the bracket insert 38 has a configuration opposite the secondary contact surface 39 which is compliments the bicycle frame or other object to which the mounting assembly 20 is to be connected. In the preferred embodiment, as illustrated in FIG. 5 , the bracket insert 38 and the cam 40 are positioned within a recessed portion 25 of the body 22 . The recessed portion 25 defines a generally confined area about the contact surface 23 . The cam 40 is connected to a cam lever 42 outside of the bracket body 22 .
Referring to FIGS. 3-7 , mounting of the mounting assembly 20 will be described. The mounting assembly 20 is positioned on the frame 10 at a desired location. A strap ring 35 on one end of the strap 36 is positioned on to the fixed strap support 30 as shown in FIG. 3 . The strap 36 is wrapped around the frame 10 and the free end 37 is fed through the free end strap support 32 and about the strap buckle 34 as shown in FIGS. 4 and 5 . The strap free end 37 is pulled such that the strap 36 is firm and snug against the frame 10 . At this time, the cam 40 is positioned between the bracket body 22 and the bracket insert 38 in a neutral position such that it applies substantially no biasing force on the bracket insert. To further tighten the mounting assembly 20 to the frame 10 , the cam lever 42 is rotated as indicated by arrow A in FIG. 6 such that the cam 40 is rotated to the position illustrated in FIG. 7 . Rotation of the cam 40 causes a biasing force on the bracket insert 38 which forces the bracket insert 38 away from the bracket body 22 . Since the strap 36 is held tight by the strap supports 30 , 32 , the strap 36 stretches about the frame 10 , hence tightening the mounting assembly 20 on to the frame 10 .
Referring to FIG. 7 , in the exemplary embodiment, as the cam 40 is rotated past 90°, for example to about 97°, the tension in the strap 36 and thereby the tension of the bracket insert 38 against the cam 40 locks the cam 40 against cam stops 41 in the bracket body 22 . Preferably the angle is between approximately 91 degrees and 100 degrees.
Referring to FIGS. 8-16 , an exemplary mounting assembly 20 ′ that is an alternative embodiment of the invention will be described. The mounting assembly 20 ′ is substantially the same as in the previous embodiment, but eliminates the bracket insert and re-routes the strap 36 . In this embodiment, the strap 36 is routed through a slot 21 in the bracket body 22 ′ as illustrated in FIGS. 8 and 9 . Referring to FIGS. 10 and 11 , the strap 36 is extended across the bracket body 22 ′ and out a second slot 23 on the opposite side of the bracket body 22 ′. A pin 33 or the like is attached to the strap 36 and received in the strap support 32 to fix the fixed end of the strap 36 . In extending the strap 36 across the bracket body 22 ′, the cam 40 is between the bracket body 22 ′ and the strap 36 .
The strap 36 is wrapped around the frame 10 and the free end 37 is fed through the free end strap support 32 and about the strap buckle 34 as shown in FIGS. 10 and 11 . The strap free end 37 is pulled such that the strap 36 is firm and snug against the frame 10 . To further tighten the mounting assembly 20 ′ to the frame 10 , the cam lever 42 is rotated as indicated by arrow A in FIG. 12 such that the cam 40 is rotated to the position illustrated in FIG. 13 . Rotation of the cam 40 directly contacts the strap 36 and thereby stretches the strap 36 about the frame 10 , hence tightening the mounting assembly 20 ′ on to the frame 10 .
Referring to FIGS. 14-16 , in the exemplary embodiment, as the cam 40 is rotated past 90°, for example to about 97° the tension in the strap 36 locks the cam 40 against cam stops 41 in the bracket body 22 ′. Preferably the angle is between approximately 91 degrees and 100 degrees.
Having described exemplary embodiments of the mounting assembly 20 , 20 ′, mounting of an exemplary lock member 12 to the mounting assembly 20 , 20 ′ will be is described with reference to FIGS. 17-24 . As indicated above, the mounting assemblies of the present invention may be utilized with various locks, but are described herein for example with respect to a U-lock 12 having a locking head 14 with a projecting engagement member 15 extending therefrom. The bracket body 22 , 22 ′ may have various configurations to accommodate locks of different configurations and to mate with them in various manners.
Referring to FIGS. 17-19 , the locking head 14 is slid into the lock receiving opening 24 with the engagement member 15 aligned with the slot 29 in the end cap 26 of the bracket body 22 , 22 ′. It is noted with reference to FIG. 19 , when the cam lever 42 is rotated to the locked position, it has a contact surface 44 adjacent to the slot 29 . Once the engagement member 15 is received through the slot 29 , the locking head 14 is rotated to the desired orientation. When the locking head 14 is rotated to the desired orientation, the engagement member 15 rotates from its alignment with the slot 29 and engages the end cap 26 and locks the locking head 14 relative to the bracket body 22 , 22 ′ as illustrated in FIGS. 20 and 21 . This helps to reduce the possibility of inadvertent dislodging of the locking head 14 . The engagement member 15 also engages the contact surface 44 of the cam lever 42 such that the mounting assembly 20 , 20 ′ can not be loosened from the frame 10 . As also shown therein, the bracket body 22 , 22 ′ preferably has a slot 25 configured to align with a lock leg opening 17 in the locking head 14 . Once the locking member (for example the U-shackle) is locked to the locking head 14 , its extension through the slot 25 prevents the locking head 14 from being slid out of the mounting assembly 20 , 20 ′.
To minimize rattling and/or spinning of the locking head 14 , the mounting assembly 20 , 20 ′ may further include a tensioning assembly configured to radially tension a portion of the locking head 14 within the lock receiving opening 24 . In the illustrated embodiment, the tensioning assembly includes a locking head lever 28 pivotally supported on the bracket body 22 , 22 ′ with a caming surface 31 extending through an opening 27 in the bracket body 22 , 22 ′ (See FIG. 2 ). In the open position illustrated in FIG. 23 , the locking head lever 28 is rotated outward such that the caming surface 31 is retracted in the opening 27 and does not extend substantially into the lock receiving opening 24 . Once the locking head 14 is positioned, the locking head lever 28 is rotated as indicated by arrow B to the locked position shown in FIGS. 22 and 24 , wherein the caming surface 31 extends through the opening 27 and creates an interference fit with locking head 14 , thus holding the locking head 14 from spinning and/or rattling.
Other tensioning assemblies may also be utilized. For example, in place of the locking head lever, a strap (not shown) may be routed within the lock receiving opening such that it extends about the locking head 14 and thereafter is tensioned against the locking head 14 . Such a strap may be a portion of the strap 36 or may be a separate strap. One or more of the straps disclosed in PCT International Appln. No. PCT/US2009/048226 may be utilized as the tension assembly, however, the invention is not limited to such straps.
While preferred embodiments of the invention have been shown and described herein, it will be understood that such embodiments are provided by way of example only. Numerous variations, changes and substitutions will occur to those skilled in the art without departing from the spirit of the invention. Accordingly, it is intended that the appended claims cover all such variations as fall within the spirit and scope of the invention.
|
A portable lock mounting assembly including a body defining a lock retaining mechanism and a contact surface. A strap having first and second ends is attachable to the body such that a loop facing the contact surface is defined by the strap. A cam member is supported by the body adjacent the contact surface and is pivotal between a first position wherein the cam member extends generally parallel to the contact surface and a second position wherein the cam member extends at an angle relative to the contact surface.
| 4
|
BACKGROUND OF THE INVENTION
This invention relates to the garment field, and more particularly, to a method of applying a print design to standard hook and loop fabric (for example, Velcro®), while simultaneously attaching the hook and loop fabric to an underlying fabric or garment.
Hook and loop fabrics are old in the art. Fabric and garments having other hook and loop fabric attached thereto is also old in the art.
Garments, such as shirts, sweatshirts, pants and hats, have long since been printed with ornamental designs. Methods of printing fabric which are known in the art include, among others, screenprinting, heat transfer printing and belt printing.
In its basic form, screenprinting consists of the alternating application of laying different screens over the same area of an underlying fabric or garment and the application of different colored printing material (inks, paints, etc.) applied with pressure over each screen. Each of the screens has a print element or portion of the overall design to be placed onto the fabric or garment. When the full set of screens (one or more screens), and their different colors, have been completely applied to the fabric or garment, a complete underlying design can be seen on the fabric or garment.
Belt printing uses substantially the same steps as screenprinting, but with the added mechanization of the cut fabric or garment proceeding along on a conveyor belt to different stations of screenprinting presses.
Heat transfer printing consists of the taking of an applique (which is transfer paper having a design printed thereon and treated with a heat and pressure sensitive adhesive on the back thereof), and transferring the design element of the applique onto a fabric or garment. The applique is transferred to the fabric or garment by applying the appropriate heat and pressure, for an appropriate period of time, thereby fusing the applique to the fabric or garment so that the ornamental design is visible on the outside of the fabric or garment.
It became popular to further adorn fabrics and garments with hook and loop fabric pieces, such as Velcro®, so that removable ornamental pieces, such as figures of people or animals or writing, could be removably attached to interact with the printed-on design. It was a disadvantage of these types of systems that the hook and loop fabric pieces, onto which the detachable ornamental pieces could be placed, and which were interspersed around the fabric or garment, did not also contain any design features to allow them to blend into the surrounding or background picture. For example, if the system involved was a blue sky which incorporated different positions for a detachable element such as the sun, any position on which to place the sun would need to have a piece of the hook and loop fabric adhered or stitched over a part of the blue sky background. The hook and loop fabric would not necessarily be the same color as the blue sky background, and therefore, when no sun element was affixed to a particular hook and loop piece, that piece would be visible and disrupt the beauty of the underlying picture, it would also not be the same texture of the background picture.
Accordingly, it would be desirable to provide a method of printing the hook and loop fabric itself with the ornamental background design while maintaining the integrity of the hook and loop structure, so that removable ornamental elements could be affixed onto the design in any location to interact with that design.
Since the hook and loop fabric is different than the underlying fabric of the garment (usually cotton, polyester, a cotton-polyester blend or any other type of natural or synthetic fabric), it is also a disadvantage to stitch a hook and loop fabric to the underlying fabric or garment since different shrinkage coefficients exist for the two fabrics and the hook and loop fabric would ultimately crumple up or become detached from the garment during repeated wash cycles. Accordingly, it would also be advantageous to provide a method of resolving this attachment problem, while also enabling the hook and loop fabric to be printed.
SUMMARY OF THE INVENTION
In accordance with the invention, an improved method of simultaneously printing a hook and loop fabric and adhering the fabric to another fabric or garment is provided.
The method comprises the steps of applying a heat and pressure sensitive coating to one side of the hook and loop fabric, placing that fabric over a portion of another fabric or garment so that the hook and loop fabric touches the other fabric or garment, heating (flashing) the two fabrics to commence activation of the coating, applying a printing material onto the hook and loop fabric and compressing the two fabrics together at an appropriate temperature and pressure, and for an appropriate time interval, to complete the activation of the coating so as to adhere the fabrics together and to activate the printing material.
The resulting fabric or garment has a hook and loop fabric attached thereto in an unremovable, non-shifting manner due to adhesion of the two fabrics from the coating. The hook and loop fabric will, in addition, have an ornamental design printed thereon as a result of the application of the printing material.
Accordingly, it is an object of the invention to provide an improved method of attaching a hook and loop fabric to a base fabric or garment, wherein the hook and loop fabric contains an ornamental design printed thereon.
Still a further object of the invention is to provide a method of printing an ornamental design onto hook and loop fabric without the hook and loop fabric losing its engagement properties.
Yet another object of the invention is to provide a method of adhering and printing a hook and loop fabric to an underlying fabric or garment so that the hook and loop fabric and the underlying fabric or garment are compatible for machine washing so as to overcome the differences in shrinkage factors between the fabrics.
Still another object of the invention is to provide a one step method of printing a hook and loop fabric and adhering that fabric to an underlying fabric or garment.
Other objects of the invention will in part be obvious and will in part be apparent from the following description.
The invention accordingly comprises a method of producing a product and the resulting product, possessing the features and properties hereinafter described, and the scope of the invention will be indicated in the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a fuller understanding of the invention, reference is made to the following description taken in connection with the accompanying drawings, in which:
FIG. 1 is a schematic of a method of simultaneously printing a hook and loop fabric and adhering that fabric to an underlying fabric or garment;
FIG. 2A is a schematic of a second embodiment of a method of simultaneously printing a hook and loop fabric and adhering that fabric to an underlying fabric or garment;
FIG. 2B is a perspective view of a stack of applique sheets;
FIG. 3 is an elevational view of a garment having a hook and loop fabric adhered thereto, wherein the hook and loop fabric has an ornamental design printed thereon;
FIG. 4 is a partial elevational view of the same garment of FIG. 3, but having removable ornamental pieces affixed to the hook and loop fabric; and
FIG. 5 is a cross-sectional view taken along line 5--5 of FIG. 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, a schematic of a system for simultaneously printing a hook and loop fabric and attaching the fabric to another fabric, in accordance with the invention and generally designated at 10, is illustrated. System 10 has a spool of hook and loop fabric 20, and a spool of other fabric 30. The other fabric 30 can be cotton, polyester, rayon, lycra, or any other natural or synthetic fabric known to be applicable to the clothing trade, or any combination thereof.
Continuing with FIG. 1, system 10 also has the following stations, coating station 40, cut and apply station 50, heat station 60, color station 70 and final dryer station 90. In a preferred application, the spool of hook and loop fabric 20, located on feed reel 14, and the spool of fabric 30, located on feed reel 16, are fed through system 10 starting at coating station 40 and ending at final dryer station 90. While going through system 10, and particularly at cut and apply station 50, some pre-determined size segment of hook and loop fabric 20 is cut and placed on top of a portion of fabric 30. The combination of the portion of fabric 20 which has been cut and applied onto fabric 30, proceeds through system 10 next entering heat station 60. The fabric 20 not cut out and applied to fabric 30 is seen in FIG. 1 to be taken-up onto take-up reel 15, which exits cut and apply station 50. Ultimately, the fabric 30 having the portion of fabric 20 thereon which exits cut and apply station 50 and enters heat station 60, completes the method of the system at final dryer 90, and is taken-up onto take-up reel 17. Fabric 30 and reel 17 will then ultimately be cut into garments, as will be discussed below.
Continuing with FIG. 1, at coating station 40, a second side 24 of hook and loop fabric 20 has applied thereto a heat and pressure activated coating. It is anticipated by the invention that any known method of applying such a coating can be applicable to the subject invention. The coating used is preferably activated at between 100° Fahrenheit and 400° Fahrenheit and at normal screenprinting pressures.
After coating station 40, fabrics 20 and 30 enter cut and apply station 50. At cut and apply station 50, fabric 20 is cut pursuant to a pre-planned geometric scheme, with the cut-out geometric portion thereof allowed to come to rest upon a portion of fabric 30 which is passing through system 10 at the time of cutting. It is anticipated that any geometric shape for the cut-out portion of fabric 20 can be used in the subject invention.
Upon leaving cut and apply station 50, the combined fabric 30 now enters heat station 60. Heat station 60 is designed to provide heat in the range of 100° Fahrenheit to 125° Fahrenheit. In this temperature range, the coating applied to second side 24 of fabric 20, now located between fabric 20 and fabric 30, begins to heat. The heating, also known as flashing, of the coating and fabrics, commences the activation of the coating, which activation ultimately will result in the uniform adhesion of second side 24 of fabric 20 onto fabric 30.
With all of the elements, the cut-out portion of fabric 20, the coating and fabric 30 having been heated at heat station 60, the combined fabric enters color station 70. In color station 70, conventional screenprinting is performed in order to apply a design element to a first side 22 of hook and loop fabric 20. It is to be understood that first side 22 of fabric 20 is the side having protruding therefrom either the hook elements or the loop elements of hook and loop fabric 20. Accordingly, the design applied at color station 70 is applied at least onto the hook or loop side of fabric 20. The invention also anticipates that the design element applied at color station 70 can be applied to both fabric 20 and fabric 30 so that the design encompasses both fabrics. The preferred coloring material for system 10 is plastisol ink.
Color station 70, as shown in FIG. 1, is broken down into first color station 75, second color station 80 and additional color stations 85. In conventional screenprinting, an overall design element having five different colors, for example, will need five different color stations, one station for each color. The invention anticipates any number of coloring stations.
The only non-conventional aspect of color station 70, and its individual coloring stations 75, 80 and/or 85, consists of use of the protective mesh boards 76, 81 and 86, respectively. These mesh boards are used in the inventive process during the conventional screenprinting process, between first side 22 of fabric 20 and the screen (not shown), in order to prevent undue flattening of the hook or loop elements of fabric 20. If either the hook or loop elements of the hook and loop fabric are overflattened in the screening step, the integrity of the hook and loop fabric to receive detachable ornamental pieces 260 (FIG. 4) having hook and loop fabric thereon, will not be maintained. In particular, if for example, first side 22 of fabric 20 were the loop elements of a conventional hook and loop fabric, detachable ornamental pieces 260 would have the counterpart hook elements of the hook and loop fabric extending therefrom. As is known to be the case with these standard-type hook and loop fabrics, as for example Velcro®, they only function properly, and maintain their connectability if the loop elements are able to receive the hook elements, i.e., if they are not overly flattened. The same is true regarding the hook elements.
Continuing with FIG. 1, after exiting color station 70, the combined fabric enters final dryer 90. In final dryer 90, heat in the range of 275° Fahrenheit to 350° Fahrenheit is applied to the combined fabric so that the coating is finally cured and so that the design element applied during color station 70, is also cured. Once the fully printed and cured fabric exits dryer 90, it is received onto take-up spool 17 for later transport to a location where the fabric can be cut and sewn into garments or other goods.
Turning now to FIGS. 2A and 2B, an alternate system 110 is shown. System 110, instead of using conventional screenprinting, as with system 10, uses a conventional applique method of applying the design element onto the hook and loop fabric and the underlying garment fabric, if desired.
System 110 comprises a coating station 150, a cutting and combining station 160 and a compressing and heating station 170. Three spools of materials are used in system 110, a roll of applique material 130 (FIG. 2A) or a stack of single sheet appliques 135 (FIG. 2B), a spool of hook and loop fabric 120 and a spool of the underlying fabric 140.
In operation, system 110 applies a similar heat and pressure activated coating as was applied in system 10, to second side 124 of hook and loop fabric 120 in coating station 150. Applique material 130 is normally activated at a temperature range of between 350° Fahrenheit and 425° Fahrenheit.
While it is shown in FIG. 2A that all three materials/fabrics enter and exit coating station 150, it is anticipated that since only fabric 120 is treated in coating station 150, applique material 130 or 135 and fabric 140 could bypass coating station 150, to first enter system 110 at cutting and combining station 160.
Continuing with FIG. 2A, after exiting coating station 150, all three materials/fabrics enter cutting and combining station 160. In cutting and combining station 160 the design element located on applique role 130 and a corresponding portion of hook and loop fabric 120 are cut and placed on top of fabric 140. Since system 110 also equally anticipates the use of individual, pre-cut appliques 135, instead of the use of a spool of applique material 130, sheets 135 of FIG. 2B would enter system 110 at cutting and combining station 160. Sheets 135 are delivered by a machine (not shown) from a table 137.
Whether roll 130 or sheets 135 are used, after cutting and combining station 160, the combined fabric 180 then enters compressing and heating station 170 where a pressure and heat combination capable of both activating the coating located between second side 124 of fabric 120 and fabric 140 and activating the transfer of the design element from applique material 130 or applique sheets 135 onto first side 122 of fabric 120 is applied for a certain period of time. The completed combined fabric 180 exits compressing and heating station 170 and is received onto spool 117 for transport to a cutting and sewing location.
It is equally anticipated by the invention that hook and loop fabric 120 would have the coating material applied by an outside, independent contractor. In this event, coating station 150 would not be needed.
The invention also anticipates the replacement of fabric spools 30 and/or 140 of systems 10 and 110, respectively, by a conveyor belt system (not shown). In such a conveyor belt system, pre-cut fabric, cut into the shape of the garment, will be placed on and ride through the respective systems on the conveyor belt. All of the stations of systems 10 and 110 will be applied as previously stated.
The result of using the systems described above is a garment having uniformly and unremovably attached thereto, hook and loop fabric, wherein the hook and loop fabric has a design element thereon. It has previously been impossible to print a design element onto a hook and loop fabric so as to have the hook and loop fabric part of, or totally represent, the design feature of the garment while maintaining the total intregity of the hook and loop engagement.
As was described earlier in this specification, earlier garments having hook and loop fabric attached thereto failed to have the hook and loop fabric as part of the design on the garment. Examples of earlier uses of this type of system on a garment were as described in the background portion of this specification, where, for example, in a sunset design the different locations of the removable sun element were not able to match the coloring of the blue sky, and thereby stood out like sore thumbs.
Other uses of hook and loop fabric on garments in the prior art incorporated into an overall picture were, for example, in a picture of a football stadium or hockey rink, or other type of sporting event, where the portion of the stadium was printed on the regular garment fabric, and the playing surface was made of hook and loop fabric. In such a garment, the fan section of the picture, which appears on the standard garment fabric, would be multi-colored, while the hook and loop fabric would be either white or black, which would obviously not advance the theme of the overall picture.
By applying the system of the present invention, not only could one achieve a green and white striped football field, a white hockey surface with blue and red lines and goalie boxes, but other design features could also be printed on the hook and loop fabric. For example, football players, goal posts and referees could be placed upon the hook and loop fabric of the invention to enhance the overall picture of a football game.
Obviously, in addition to enhancing the types of garments previously made having hook and loop fabric removable elements, as stated above, other types of innovative design elements can now be applied to both hook and loop fabric and underlying garment fabric so as to achieve any underlying ornamental design for use thereon of removable decorative elements.
In addition to the above benefits, the manner of attaching the hook and loop fabric to the underlying fabric or garment prevents separation of the two materials due to washing. In particular, by using the one-step system of the invention, which calls for use of a heat and pressure sensitive coating between the hook and loop fabric and the underlying fabric or garment, a unitary structure is realized. This structure, unlike the structures resulting from previously used methods of attaching hook and loop fabrics to other fabrics (i.e., sewing), fuses the two fabrics to overcome the inherent differences normally experienced after washing these two fabrics because of their different shrinkage coefficients.
A garment having a printed hook and loop fabric thereon, and its corresponding removable decorative element are shown in FIGS. 3-5.
As seen in FIG. 3, a garment 200 has a rectangular shaped hook and loop fabric adhered thereto. It is of course anticipated that any shape of the hook and loop fabric could be used.
As seen in FIG. 5, the particular portion of the hook and loop fabric 210 applied to garment 200 by coating 215 is the loop portion 220. The corresponding hook portion 240 is applied, as shown in FIG. 5, to detachable ornamental piece 260.
It is also seen in FIGS. 3 and 4 that an ornamental design 280 is applied over both surface 205 of garment 200 and over loop portion 220 of hook and loop fabric 210. In this way, garment 200 is able to have an encompassing beautiful design 280 on both its surface 205 and on hook and loop fabric 210, is desired. In the alternative, the design could be located only on surface 220.
As seen in FIG. 4, detachable ornamental pieces 260, which interact and correspond with design 280, can be placed anywhere on the printed loop portion 220 of hook and loop fabric 210. Never before has such a garment been created. It is both ornamental and interactive, while satisfying the requirements of novelty and non-obviousness.
The system anticipates the use of a display format (not shown) comprising a preformed mock-up of the head, shoulders and chest of a person (not shown), a garment made pursuant to the invention placed thereover and sealed in some manner. It is also anticipated that the sealing mechanism will have a window therethrough for in-store application of a sample ornamental piece 260 onto the hook and loop fabric of the garment. The sample ornamental piece will be tethered to the display garment.
It will thus be seen that the objects set forth above, among those made apparent from the preceding description, are efficiently attained, and, since certain changes may be made in the above system or garment without departing from the spirit or scope of the invention, it is intended that all matter contained in the above description and shown in the accompanying drawings are to be interpreted as illustrative and not in a limiting sense.
It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.
|
An improved method of simultaneously printing a hook and loop fabric and adhering the fabric to another fabric or garment is provided. The method comprises the steps of applying a heat and pressure sensitive coating to one side of the hook and loop fabric, placing that fabric over a portion of another fabric or garment so that the hook and loop fabric touches the other fabric or garment, heating the two fabrics to commence activation of the coating, applying a printing material onto the hook and loop fabric and compressing the two fabrics together at an appropriate temperature and pressure, and for an appropriate time interval, to complete the activation of the coating so as to adhere the fabrics together and to activate the printing material. The resulting fabric or garment has a hook and loop fabric attached thereto in an unremovable, non-shifting manner due to adhesion of the two fabrics from the coating. The hook and loop fabric will, in addition, have an ornamental design printed thereon as a result of the application of the printing material.
| 8
|
This application claims priority under 35 USC § 119(e)(1) of provisional application No. 60/037,729 filed Feb. 7, 1997.
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is related to patent application Ser. No. 08/739,111, filed Oct. 25, 1996.
BACKGROUND
The present application relates to information encoding for transmission over noisy channels and storage, and more particularly to error resilient encoding.
Two common approaches to the mitigation of errors arising during the transmission of data over noisy channels exist: Automatic Retransmission Request (ARQ) and Forward Error Correction (FEC). ARQ type of mitigation typically would not be feasible in multicast or real-time applications such as video because of intolerable time delays or a lack of feedback channel. In such cases, a decoder can only decode the error corrupted bitstream, protected to an extent by error correction encoding, and must create from such bitstream. FEC provides mitigation by error correcting codes (e.g., Reed-Solomon). However, uncorrectable errors require further mitigated approaches.
In general, commonly used video compression methods have block-based motion compensation to remove temporal redundancy. Motion compensation methods encode only (macro)block motion vectors and the corresponding quantized residuals (texture); and variable length coding (VLC) of the motion vectors and residual increases coding efficiency. However, variable length coding often are highly susceptible to transmission channel errors and a decoder easily loses synchronization with the encoder when uncorrectable errors arise. The predictive coding methods, such as motion compensation, make matters much worse because the errors in one video frame quickly propagate across the entire video sequence and rapidly degrade the decoded video quality.
The typical approach of such block-based video compression methods to uncorrectable errors includes the steps of error detection (e.g., out-of-range motion vectors, invalid VLC table entry, or invalid number of residuals in a block), resynchronization of the decoder with the encoder, and error concealment by repetition of previously transmitted correct data in place of the uncorrectable data. For example, video compressed using MPEG1-2 has a resynchronization marker (start code) at the start of each slice of macroblocks (MBs) of a frame, and an uncorrectable error results in all of the data between correctly decoded resynchronization markers being discarded. This implies degradation in quality of the video stream, especially for predictive compression methods such as MPEG.
These video compression and decompression methods may be implemented on special integrated circuits or on programmable digital signal processors or microprocessors.
SUMMARY OF THE INVENTION
The present invention provides resynchronization imbedded within a video bitstream by partitioning of motion vector data and corresponding texture data so that with some uncorrectable errors the motion vector data may still be usable. The present invention also provides a method of selecting a word to use as a resynchronization marker compatible with variable length codes of the data.
This provides advantages including partial recovery over uncorrectable error in a packet of compressed video data with little additional overhead.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings are schematic for clarity.
FIG. 1 illustrates a bitstream packet syntax with first preferred embodiment resynchronization.
FIG. 2 shows known bitstream packet syntax with resynchronization.
FIG. 3 shows a resynchronization word search.
FIG. 4 shows experimental results.
FIG. 5 shows another bitstream syntax.
FIG. 6 shows object scan.
FIG. 7 shows another bitstream syntax.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Bitstream Syntax
FIG. 1 illustrates a first preferred embodiment bitstream packet syntax with motion resynchronization, and, for comparison, FIG. 2 shows a known packet syntax without the preferred embodiment motion resynchronization. In particular, both FIGS. 1 and 2 show a packet syntax for MPEG type encoded video which partitions a frame into blocks or macroblocks (MBs) and encodes most MBs by motion vectors (MV) for prediction from prior MBs plus texture data (DCT) for the (compressed) difference between predicted and actual MB pixels. Indeed, a (luminance only) frame of 288 lines with 352 pixels per line forms an 18 by 22 array of MBs with each MB a 16 by 16 array of pixels. For transmission or storage the sequence of 396 MBs of such a frame would be split into packets of convenient size. For example, with a packet size of about 1000 bytes and with an average MB encoded by about 320 bits (e.g., 20 bits for motion vector(s) and 300 bits for texture), then a packet would contain roughly 25 MBs. Consequently, such a frame would require roughly 16 packets for transmission, and a frame rate of 30 frames per second would require roughly 3.8 Mbps transmission. For low bit rate transmission, the texture data is greatly decreased, so the motion vector data becomes relatively more important.
Typically, the MBs of a frame are grouped into slices with a slice consisting of one or more consecutive MBs in a single row of a frame. Thus in the foregoing example, a slice could include from 1 to 22 MBs. Within a slice the macroblock data appears sequentially. Resynchronization may be performed using the slice start codes. For example, a simplified slice heuristically could be:
______________________________________slice(){ slice.sub.-- start.sub.-- code macroblock.sub.-- number quantizer.sub.-- scale.sub.-- code do { macroblock(i) } while (j < macroblock.sub.-- count) next.sub.-- start.sub.--code()______________________________________
where the macroblock() function provides motion vector(s) and texture data for a macroblock and macroblock -- number is the number in a frame scan of the first macroblock in the slice. This provides the syntax illustrated in FIG. 2 with motion vector and texture data interleaved on a macroblock basis.
In contrast, a preferred embodiment slice function partitions motion vector data and texture data into separate parts plus inserts a motion resynchronization word (motion -- resynch) between these data parts heuristically as follow:
______________________________________slice(){ slice.sub.-- start.sub.-- code macroblock.sub.-- number quantizer.sub.-- scale.sub.-- code do { motion.sub.-- vector(j) } while (j < macroblock.sub.-- count) motion.sub.-- resynch do { block(j) } while (j < macroblock.sub.-- count) next.sub.-- start.sub.--code()______________________________________
where the motion -- vector() and block functions provide the motion vector(s) and texture data for a macroblock. The motion -- resynch word provides additional error concealment as follows.
The motion -- resynch word is computed from the motion vector VLC tables to be a Hamming distance of at least 1 from any allowed sequence of motion vector data. The motion -- resynch word is uniquely decodable from the motion vector VLC codeword stream and gives the decoder knowledge of where to stop reading motion vector data before beginning to read texture data. The number of macroblocks in the packet is implicitly known after the decoder encounters the motion -- resynch word. In response to an error detection the decoder proceeds depending upon the error type.
(1) When an uncorrectable error is detected in the motion vector data, the decoder flags an error and replaces all of the macroblocks in the packet with skipped blocks until the next resynchronization marker. Resynchronization occurs at the next successfully read resynchronization marker. If any subsequent video packets are lost before resynchronization, those packets are replace by skipped macroblocks.
In an alternate scheme, when the decoder detects an error in the motion vector data, it may also choose to utilize the part of the motion vector data that was decoded correctly (say "N" macroblocks) and apply motion compensation. The decoder then seeks the motion marker and tries to decode the corresponding "N" macroblocks of texture data. If this texture data is decodable without any detectable errors, the decoder adds this texture data to the already motion compensated "N" blocks. If an error is detected in decoding any of the "N" macroblocks texture, the decoder only uses the motion compensation and replaces the texture data with zeros.
(2) When an error is detected in the texture data (after encountering the motion -- resynch word and and no error had been detected in the motion data) the motion vector data is used to perform the motion compensation. The texture data of the macroblocks is all replaced with zero and the decoder resynchronizes to the next resynchronization marker.
(3) If no error is detected either in the motion vector or the texture data but the resynchronization marker I not found at the end of decoding all of the macroblocks of the packet, an error is flagged and only the texture data of the packet is discarded. Motion compensation is still applied for the macroblocks as there is a higher confidence in the motion vector data because it came prior to the detected motion -- resynch word.
(4) If no errors are detected in the motion vector data or texture data in the current packet and the next resynchonization marker is found, then an additional check may be employed: the number of the first macroblock of the next packet minus the number of the first macroblock of the current packet should equal the number of macroblocks in the current packet as found by the decoding of the motion vector data up to the motion -- resynch word. If these two measures of the number of macroblocks do not agree, then discard the data of this next packet because there is a high probability of an error in the number of the first macroblock of this next packet. The chance of an error in the current packet is small since the number of motion vectors correctly decoded agreed with the number of texture data items correctly decoded and the motion -- resynch word was found in the correct place. This is in contrast to the FIG. 2 type syntax where such and error requires both packets be discarded because the location of the error occurrence and the location of the error detection usually do not coincide and neither packet can be relied on.
In short, the motion -- resynch word provides (1) more stringent checks on the validity of the motion vector data because the motion -- resynch word must be found at the end of the motion vector data and (2) an undetected error in the motion vector and texture data coupled with not finding the next resynchronization marker only requires discarding the texture data because the motion -- resynch word was correctly found.
The motion resynchronization word may be computed from the motion VLC tables using a search as described in the following section; the word is a Hamming distance at least 1 from any possible valid combination from the motion VLC tables.
Resynchronization Word Generation
The first preferred embodiment method creates resynchronization words (the motion resynchronization word of the preceding section would be an example) by a search based on the corresponding VLC tables. An optimal resynchronization word can be selected from the possible words found by the search. In particular, presume that a bitstream has a sequence of codewords, c i k (ith codeword from kth VLC table), the preferred embodiment method finds a word which differs from all possible bit patterns arising in this bitstream. A natural metric for comparison of performance of potential words is the Hamming distance between the word and the set of all possible patterns in bitstreams derivable from the VLC tables: a positive Hamming distance implies a word differing from all bit patterns in the bitstream. Thus for a given word length, R, the idea is to find among the 2 R words of length R the word(s) with the maximal Hamming distance from all possible bit patterns of length R which could arise in bitstreams derived from the VLC tables. Of course, if all words of length R have a Hanning distance 0 from the bit patterns, then R must be increased.
To find the Hamming distance between potential resynchronization words of length R and bitstream bit patterns of length R, divide the set of bit patterns into three subspaces for searching: subspace S 1 of codewords of length at least R, subspace S 2 of allowable concatenated ordered pairs of codewords with a sum of lengths at least R, and subspace S 3 of allowable concatenations of at least three codewords with each of the imbedded (interior) codewords of the concatenation having a length less than R, The search with a potential resynchronization word r proceeds as follows.
First search over subspace S 1 :
(1) Initialize a variable H to be L(r) where L() is the length of (number bits in) its argument; H will be the Hamming distance of r to the subspace S 1 at the end of the first search.
(2) The total number of shifts needed to find the Hamming distance between word r and codeword c i k in S 1 is L(c i k )-L(r)+1, so initialize a shift counter N=L(c i k )-L(r)+1.
(3) Define ç as a segment of c i k of length L(r) and starting at bit N of c i k . Then update H by
H=min(H,D(ç,r))
where D(a,b) is the Hamming distance between bit patterns a and b.
(4) Decrement N by 1 and go to step (3) if N is positive.
After repeating the foregoing steps (2)-(4) for each codeword in subspace S 1 , H is the Hamming distance of r to S 1 . and is denoted H 1 . Of course, if H becomes 0, then r is not a possible resynchronization word and the searching may be terminated.
Continue with the second search over the subspace S 2 :
(1) Initialize a variable H to be L(r); H will be the Hamming distance of r to the subspace S 2 at the end of the second search.
(2) The total number of shifts needed to find the Hamming distance between word r and two concatenated codewords c i k +c j n in S 2 is L(c i k )+L(c j n )-L(r)+1, so initialize a shift counter N=L(c i k )+L(c j n )-L(r)+1.
(3) Define ç as a length L(r) segment of c i k +c j n starting at bit N. Then update H by
H=min(H,D(ç,r))
(4) Decrement N by 1 and go to step (3) if N is positive.
After repeating the foregoing steps (2)-(4) for each ordered pair of codewords in subspace S 2 , H is the Hamming distance of r to S 2 and is denoted H 2 . Again, if H decreases to 0, then r is not a possible resynchronization word and the searching may be terminated.
Lastly, do the third search over subspace S 3 . Define a coherent block as a chosen codeword c q p from the VLC tables such that L(c q p ) is less than L(r). This is the center piece from which other codewords are concatenated to the left and right; see FIG. 3. For every coherent block in the VLC tables, proceed as:
(1) Initialize a variable H to be L(r); H will be the Hamming distance of r to the subspace S 3 at the end of the third search.
(2) The total number of shifts needed to find the Hamming distance between word r and a concatenation of three or more codeword with coherent block c q p in S 3 is L(r)-L(c q p )+1, so initialize a shift counter N=L(r)-L(c q p )+1.
(3) Partition r into three (possibly empty) portions: r 1 is the first N-1 bits, r 2 is the next L(c q p )bits, and r 3 is the remaining L(r)-L(c q p )-N+1 bits.
(4) Recursively concatenate allowable codewords on both ends of the coherent block and compute Hamming distance:
(a) form an allowed combination of codewords to the left of the coherent block until its length is at least N-1, and define ç 1 as the last N-1 bits of this combination.
(b) form an allowable combination of codewords to the right of the coherent block plus left combination from (a) until the right combination has length of at least L(r)-L(c q p )-N+1, and define ç 3 as the first L(r)-L(c q p )-N+1 bits of this right combination.
(c) update H by
H=min(H, D(ç.sub.1,r.sub.1)+D(c.sub.q.sup.p,r.sub.2)+D(ç.sub.3,r.sub.3))
(d) repeat steps (a)-(c) for all allowable left and right combinations.
(5) Decrease N by 1 and go to step (3) if N is positive.
After repeating the steps (2)-(5) for each coherent block in the VLC tables, H is the distance between r and S 3 , and is denoted H 3 .
Thus the Hamming distance between r and all possible bitstreams is min(H 1 ,H 2 ,H 3 ). So an optimal resynchronization word can be found (if one exists) by searching with increasing word length until a positive Hamming distance is found. Looking for a (longer) word with a Hamming distance to the bitstream of greater than 1 likely does not help due to the nature of burst errors. The searching method minimizes the search space by focusing in S 3 on the coherent block and not on short codewords which overlap the ends of the possible resynchronization word.
The searching strategy for finding a resynchronization word relies on a presumption that such a word exists for the given VLC tables. If the VLC tables form a set of prefix-free code tables with at
Video Object Resynchronization
Object-based video coding methods decompose video into moving objects plus a background object, so a sequence of frames is treated as a set of sequences of video object, one sequence for each object. Each frame is thus coded as a set of separately coded objects. A decoder reconstructs a frame from the decoded objects. This permits the objects to be coded at multiple resolutions, and the decoder may select certain objects to decode at higher resolution for better visual perception.
The shape, content (texture), and motion of the objects can be efficiently coded using motion compensation as previously described; and objects may be relatively small (within a few macroblocks), so avoid the first embodiment's slice() restriction to a single row of macroblocks. The preferred embodiment error concealment for this compressed data again partitions the shape, motion vector, and texture data and provides resynchronization words between each partition; this again is in contrast the known treatment of the shape, motion vector, and texture data on a macroblock basis. Thus introduce resynchronization words at the start of the data for an I frame and at the start of each of the codes for the following items for every detected object in a P frame in addition to the start of the P frame:
(I) shape (e.g., boundary contour data);
(ii) motion vector data; and
(iii) texture data (DCT or other method compressed residual data such as wavelet). Further, if control data or other data is also included, then this data can also have resynchronization words. The resynchronization words The resynchronization words are characterized by the fact that they are unique, i.e., they are different from any given sequence of coded bits of the same length because they are not in the VLC table(s) which are static table(s). For example, if a P frame had three moving objects, then the sequence would look like:
frame begin resynchronization word
contour (shape) resynchronization word
first object's contour data
motion vector resynchronization word
first object's motion vector data;
texture resynchronization word
first object's texture data
contour (shape) resynchronization word
second object's contour data
motion vector resynchronization word
second object's motion vector data;
texture resynchronization word
second object's texture data
contour (shape) resynchronization word
third object's contour data
motion vector resynchronization word
third object's motion vector data;
texture resynchronization word
third object's texture data
These resynchronization words also help the decoder detect errors.
Once the decoder detects an error in the received bitstream, it tries to find the nearest resynchronization word. Thus the decoder reestablishes synchronization at the earliest possible time with a minimal loss of coded data.
An error may be detected at the decoder if any of the following conditions is observed:
(I) an invalid codeword is found;
(ii) an invalid mode is detected while decoding;
(iii) the resynchronization word does not follow a decoded block of data;
(iv) a motion vector points outside of the frame;
(v) a decoded dct value lies outside of the permissible limits; or
(vi) the boundary contour is invalid (lies outside of the image).
If an error is detected in the boundary contour data, then the contour is discarded and is made a part of the background; this means the corresponding region of the previous frame is used. This reduces some distortion because three often is temporal correlation in the video sequence.
If an error is detected in the motion vector data, then the average motion vector for the object is applied to the entire object rather than each macroblock using its own motion vector. This relies on the fact that there is large spatial correlation in a given frame; therefore, most of the motion vectors of a given object are approximately the same. Thus the average motion vector applied to the various macroblocks of the object will be a good approximation and help reduce visual distortion significantly.
If an error is detected in the texture data, then all of the texture data is set to zero and the decoder attempts to resynchronize.
Video Object Motion Resynchronization
An explicit example of the foregoing object data partitioning for resynchronization has been experimentally examined and shows enhanced performance with a small overhead in additional bits required for coding. In particular, just motion vector data and texture data were used for P type pictures, and FIG. 5 illustrates the bitstream. The motion vector data for each macroblock consists of two parts: the number of motion vectors and the actual motion vector(s). The number of motion vectors is either 0, 1, or 4, which corresponds to no motion compensation, a single motion vector for the entire macroblock, or a motion vector for each of the four 8 by 8 blocks making up the macroblock, respectively. The number of motion vectors is coded with the following VLC table:
______________________________________ 0 11 1 0 4 10______________________________________
The motion vectors are (differentially from preceding frame) encoded with the horizontal component, and each component is coded with the following VLC table where s equals 0 for a + entry and 1 for a - entry:
______________________________________ ±16 0000 0000 0010s ±15.5 0000 0000 0011s ±15 0000 0000 010s ±14.5 0000 0000 011s ±14 0000 0000 100s ±13.5 0000 0000 10ls ±13 0000 0000 110s ±12.5 0000 0000 111s ±12 0000 0001 00s ±11.5 0000 0001 01s ±11 0000 0001 10s ±10.5 0000 0001 11s ±10 0000 0010 00s ±9.5 0000 0010 01s ±9 0000 0010 10s ±8.5 0000 0010 11s ±8 0000 0011 00s ±7.5 0000 0011 01s ±7 0000 0011 10s ±6.5 0000 0011 11s ±6 0000 0100 00s ±5.5 0000 0100 01s ±5 0000 0100 1s ±4.5 0000 0101 0s ±4 0000 0101 1s ±3.5 0000 011s ±3 0000 100s ±2.5 0000 101s ±2 0000 11s ±1.5 0001s ±1 001s ±0.5 01s 0 1______________________________________
Thus allowable bistreams will have either 2 or 8 consecutive entries from this VLC table depending upon the preceding entry from the foregoing number of vectors VLC table. The bitstream will have some fixed length codes for object items such as frame prediction type (e.g., I, P, or B) and quantization factor for the texture data, and a 17-bit resynchronization marker 0000 0000 0000 0000 1 following the texture data for packetizing the macroblock data, and a search using the preferred embodiment method of the preceding section with these two VLC tables for the motion vector data and resynchronization marker yielded roughly 10 possible minimal length (17 bits) motion resynchronization words. A particular motion resynchronization word (1010 0000 0000 0000 1) was selected and used in simulations of transmission over a noisy channel by corrupting a bitstream with random bit errors, packet loss errors, and burst errors. FIG. 4 shows the performance of the error resilient bitstream (partitioning motion vector data and texture data with the motion resynchronization word between) as compared to the usual motion vectors and texture data in a macroblock by macroblock sequence. For the simulation the bit error rate was 10 -2 and the burst length was 1 ms. FIG. 4 shows the peak signal to noise ratio (PSNR) as a function of frame number. The partitioning of the motion vector and texture data with a motion resynchronization word yielded more than a 2 dB gain.
Video Object Shape and Motion Resynchronization
For a bitstream including shape data, motion vector data, and texture data for multiple objects, a preferred embodiment coding has packets with resynchronization markers separating the data of the objects. Between each pair of resynchronization markers the data for a set of macroblocks of a single object is partitioned into shape data, motion vector data, and texture data with a shape resynchronization word between the shape data and the motion vector data and a motion resynchronization word between the motion vector data and the texture data; see FIG. 5. The motion vector data again includes the number of motion vectors plus differential motion vector components; the shape data includes the object identification data and shape codes
The size of the objects (number of macroblocks) may vary greatly, so a single packet may contain, for example, a final portion of the macroblocks of a first object, all of the macroblocks of a second objects, and an initial portion of the macroblocks of a third object. In this case, the resynchronization markers would separate the three objects' data sets and the shape and motion resynchronization words would be the boundaries for the partitioning of the data for each object into shape, motion, and texture data.
In an alternate scenario, it may be preferable to packetize each individual object separately. In this case the shape, motion and texture data of the only one object occurs between two consecutive resync markers. See FIG. 6 showing scans through macroblocks of two objects in a frame, and FIG. 7 showing the bitstream syntax. In this scheme also between two resync markers the shape and motion may occur. The advantage of this approach that the data belonging to each object is separately packetized in the bitstream.
Generally, a resynchronization marker may be inserted at fixed intervals in the bitstream, so an object's data may be split into more than one shape-motion-texture grouping. For example, a low bit rate such as 48 kbps and high compression, a resynchronization marker maya be used every 764 bits. At higher rates, use less frequent resynchronization markers.
The shape resynchronization word and the motion resynchronization word can each be generated by the preferred embodiment search method. As previously described, the resynchronization words help error detection and provide partial data use even if some of the data must be discarded; for example, shape data and motion vector data may be used without the texture data.
One possibility for improved error resilience uses reversible codes (codeword are symmetric) in the VLC tables with the shape and motion resynchronization words. This has the advantage localizing a detected error: once a decoder detects an error, the decoder may jump to the next resynchronization marker and decode backwards towards the previously detected error. Because the use of VLC often makes an error detectable only after its location has been passed by the decoder, the backwards decoding likely will not detect an error until passing the location of the forward error detection; see FIG. ?. In this case, discard the data between the locations of the forward decoded and the backwards detected errors. This provides the maximum amount of data recovery from the error.
|
Video compressed by (macro)block level motion compensation has bitstream with the motion vectors aggregated and separated form the corresponding texture data by a resynchronization word, and a method of generating resynchronization words from variable length code tables which encode the motion vectors or the texture data adjacent to a resynchronization word.
| 7
|
FIELD OF THE INVENTION
[0001] This invention relates to the production of an active nickel metal powder suitable for transformation into nickel carbonyl. Moreover, it relates to the transformation of the active powder into nickel carbonyl by reaction with carbon monoxide at atmospheric or super-atmospheric pressure, in the absence of conventional carbonylation catalysts.
BACKGROUND OF THE INVENTION
[0002] It is well known to use the Mond process for the extraction of nickel from ores, mattes, residues, or similar compounds containing nickel, in which such compounds are reduced to yield finally divided metallic nickel, which is then treated with carbon monoxide to produce nickel carbonyl that can then be decomposed to yield pure nickel. Various improvements to this process have been suggested to increase the rate of nickel carbonyl production and thus render the overall process more economical. For example, in Canadian Patent No. 322,887 it is suggested to add to the reaction chamber producing nickel carbonyl, a compound containing sulphur, selenium or tellurium in active form, such as nickel sulphide, nickel selenide or nickel telluride and carrying out the carbonylation reaction in the absence of oxygen. The preferred additive is nickel sulphide and it is added so that the amount of active sulphur in the reaction chamber lies between 0.2% and 5% by weight. It, therefore, acts as a catalyst to promote the carbonylation reaction.
[0003] In U.S. Pat. No. 4,045,541 another improvement is disclosed according to which a metal, such as iron, copper or cobalt, which forms sulphides more easily than nickel at 200° C., is admixed with the material comprising elemental nickel, such as nickel oxide, which is then subjected to carbonylation and sulphidation.
[0004] British Patent No. 649,988 discloses a process for the manufacture of nickel carbonyl by reacting an aqueous solution of a nickel salt, such as nickel chloride or nickel sulphate, with an alkaline reacting substance, producing a nickel compound which is treated in aqueous solution or suspension with carbon monoxide under super-atmospheric pressure of at least 50 atmospheres and at elevated temperatures of at least 70° C., and in the presence of a minor amount of nickel sulphide or cyanide as a catalyst.
[0005] All the above prior art processes require the presence of various additives or carbonylation catalysts and/or the use of super-atmospheric pressure and elevated temperature to achieve satisfactory rates of nickel carbonyl production.
[0006] There is thus a need for a simplified production of nickel carbonyl from nickel salts.
OBJECTS AND SUMMARY OF THE INVENTION
[0007] It is an object of the present invention to produce active nickel powder by reducing feed materials containing nickel chloride and/or other reducible nickel salts, such that the active powder is capable of reaction with a gas containing carbon monoxide to yield nickel carbonyl. It is a further object of the present invention to produce active nickel powder by reducing feed materials containing one or more reducible nickel salts with a reducing gas containing both hydrogen and hydrogen chloride such that the active powder is capable of reaction with a gas containing carbon monoxide to yield nickel carbonyl. It is yet a further object of the present invention to transform the produced active nickel powder into nickel carbonyl at rapid and commercial rates without addition of carbonylation catalysts or promoters, such as used in the prior art.
[0008] Other objectives and advantages of the present invention will become apparent from the following description thereof.
[0009] In essence, it has been found that an active nickel powder can be made by reducing a feed material containing one or more reducible nickel salts, optionally comprising nickel chloride, having a surface area in excess of 1 m 2 /g, with a reducing gas containing preferably at least 20 volume per cent hydrogen, at a temperature between about 300° C. and 600° C., by either (a) including nickel chloride in the feed material such that the weight ratio of chloride to total nickel is greater than 0.1, or (b) adding hydrogen chloride directly to the reducing gas. The resulting activated nickel powder can then be reacted with a gas containing CO at atmospheric pressure at temperatures of 20° C. to 100° C. to produce nickel carbonyl {Ni(CO) 4 }, with high yield, preferably close to 100%. The active nickel powder can also be reacted with a gas containing CO at super-atmospheric pressure and elevated temperature, if desired. The carbonylation reaction with a gas containing CO is simple and effective, requiring no catalysts or other promoters.
[0010] When other reducible nickel salts, for example nickel carbonate, nickel hydroxide or nickel sulphate are treated in the same manner, namely by reduction with a gas containing H 2 at 300° C.-600° C., the nickel powder produced is essentially inactive. However, surprisingly, when such reducible nickel salts are admixed with nickel chloride or treated with HCl gas such that the weight ratio of chloride to total nickel is greater than 0.1 and the reducible nickel salts have a surface area in excess of 1 m 2 /g, the entire admixture reduces to an active nickel powder. For example, nickel extraction from reduced nickel carbonate is typically about 10 wt % after five hours but nickel extraction from an admixtures of NiCO 3 and NiCl 2 or from NiCO 3 with 1-5 volume per cent hydrogen chloride directly added to reduction gas-, are in the range of 95-100%. Extractions obtained with admixtures including NiSO 4 are usually slightly lower, but still in a very appreciable range of 85-90%, probably due to the formation of some nickel sulphide, which does not carbonylate.
[0011] When reference is made to reducible nickel salts and nickel chloride, it is to be understood that these salts can be either in the anhydrous form or in the form of hydrates, such as NiCl 2 .6H 2 O. Moreover, when reference is made to reducible nickel salts, they can also be combined with other nickel compounds, such as nickel hydroxide, as in the compound called zaratite—2Ni(OH) 2 .NiCO 3 .4H 2 O.
[0012] The starting feed material to be reduced to nickel powder should have a high surface area in excess of about 1 m 2 /g, and preferably between 35 and 100 m 2 /g.
[0013] Those skilled in the art will appreciate that the feed material containing nickel chloride and one or more reducible nickel salts, in which the weight ratio of chloride to total nickel is greater than 0.1 and the reducible nickel salts have a surface area in excess of 1 m 2 /g, can be made by mixing together the dry components, or by wet mixing in the presence of water, reducible nickel salts and other soluble metal chloride salts (for example CrCl 3 , FeCl 3 , FeCl 2 ) and then removing the water by drying, or by adding hydrochloric acid to an excess of reducible nickel salts and then removing the water by drying, or by adding alkali (for example sodium carbonate ) to a solution of reducible nickel salts, which includes nickel chloride, and then removing the water by drying. Those skilled in the art will recognize that mixing the soluble components of the feed material in water will allow nickel chloride to be formed by metathesis (exchange of anions). For example, mixing nickel carbonate and chromium chloride produced some nickel chloride and chromium carbonate in the admixture after drying. Drying of the wet feed material can be an integral part of reduction with gas containing at least 20 volume % hydrogen or it can be done as a separate step prior to reduction. It has been found that the beneficial effect of the hydrogen chloride gas given off during reduction of a feed material containing both reducible nickel salts and reducible metal chlorides (for example NiCl 2 ) can also be obtained by adding hydrogen chloride gas directly to the reducing gas preferably in an amount equivalent of that produced by reducing nickel chloride as described above. It has been found that when hydrogen chloride gas is added directly to the reducing gas in this way it is not necessary to add nickel chloride to the feed material to make active nickel although the present invention also contemplates the addition of nickel chloride.
[0014] Active nickel powder produced in accordance with the present invention can be maintained indefinitely under inert gas, such as argon. A useful feature of this powder is that if the active nickel powder loses, or partly loses its activity due to storage in the absence of oxygen, it can be re-activated by exposing it to a gas containing H 2 at a temperature above about 150° C. If the active nickel powder loses its activity due to storage in the presence of oxygen, it can be conveniently re-activated by exposing it to a gas containing H 2 at a temperature of about 150° C. to 600° C. This is an important advantage of the present invention since it enables the carbonylation reaction to be performed completely separately and even at a different location from the reduction reaction that produces the active nickel powder.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a graph showing nickel extraction from active nickel powder produced by reduction of nickel chloride hydrate;
[0016] FIG. 2 is a graph showing nickel extraction from active nickel powder where treatments were made on various materials containing NiCl 2 at different temperatures;
[0017] FIG. 3 is a graph showing nickel extraction from nickel powder produced by reduction of nickel carbonate only with no nickel chloride present;
[0018] FIG. 4 is a graph showing nickel extraction from active nickel powder produced by reduction of an admixture of and nickel carbonate and nickel chloride.
[0019] FIG. 5 is a graph showing nickel extraction at super-atmospheric pressure and elevated temperature from active nickel powder of the present invention (F) as compared to regular nickel powder of the prior art (G).
[0020] FIG. 6 is a graph showing the nickel extraction from active nickel powder produced by reduction of nickel carbonate with a reducing gas to which hydrogen chloride gas has been directly added.
[0021] FIG. 7 is a graph showing nickel extraction from active nickel powder (A) produced by reduction of an admixture of nickel carbonate and chromium chloride produced by first wet mixing the nickel carbonate and chromium chloride and then drying the wet mixture at 110° C. to remove water, and nickel extraction from nickel powder (B) produced by reduction of a dry admixture of dry nickel carbonate and dry chromium chloride.
[0022] FIG. 8 is a graph showing nickel extraction from active nickel powder (A) produced by reduction of an admixture of nickel carbonate and nickel chloride produced by first wet mixing the nickel carbonate and nickel chloride and then drying the wet mixture. The graph also shows carbonylation extraction of active nickel after additions of 1 wt % of CrCl 3 (B), FeCl 2 (C) and FeCl 3 (D) metal chlorides to the wet admixture of nickel carbonate and nickel chloride.
DETAILED DESCRIPTION OF THE INVENTION
[0023] Examples of preferred, but non-limiting, embodiments will now be described with reference to the appended drawings. In these examples, tests were carried out by first reducing a pre-dried small sample (25 mg) of finely divided (1) nickel chloride and of (2) nickel carbonate and (3) nickel carbonate in admixture with nickel chloride. This feed was reduced in hydrogen at 500° C., the resulting active nickel powder was then further cooled to 200° C. and the reactive gas switched from hydrogen to carbon monoxide at a flow rate of 10 ml/min. The sample was then further cooled to 50° C. Weight loss was monitored over time using appropriate computercontrolled measurement. The weight loss was confirmed with TGA (thermogravimetric analysis) measurements, and the residue was dissolved in acid and analysed for nickel to give a complete mass balance. The obtained nickel metal powder reacted with CO to form volatile nickel carbonyl gas, which was removed and decomposed at high temperature into a pure nickel product as is known in the art.
[0024] Whenever use herein, the term “about” can afford a deviation of ±20% of the absolute value being described or claimed, without departing from the scope of this invention.
EXAMPLE 1
[0025] In this example, NiCl 2 .6H 2 O was pre-dried at 170° C. in air. This feed was reduced in hydrogen at 500° C. and the resulting nickel powder was then further cooled to 200° C. The reactive gas was switched from hydrogen to carbon monoxide at a flow rate of 10 ml/min and the nickel powder was then further cooled to 50° C. Carbonylation extraction of the nickel powder was carried out in CO gas at 50° C. Nickel extraction of 99.6% was obtained in 45 minutes as illustrated by the curve in the graph of FIG. 1 and by curve B in the graph of FIG. 2 .
[0026] The same procedure as above was repeated with a sample of NiCl 2 pre-dried at 300° C. in N 2 . Nickel extraction of essentially 100% was obtained in about 30 minutes as illustrated by curve A in the graph of FIG. 2 .
[0027] The same procedure was repeated with another sample of NiCl 2 pre-dried at 170° C. in air. Nickel extraction of essentially 100% was obtained in about one hour as illustrated by curve C in the graph of FIG. 3 .
[0028] The same procedure was repeated but using a temperature of 600° C.-800° C. for reduction in hydrogen. In this case, essentially full extraction was reached after about 2.5 hours, as illustrated by curve D in the graph of FIG. 2 . This shows that temperatures higher than 600° C. actually slow down the extraction and there is no practical reason to use them. The present invention is, however, not limited to temperatures below 600° C.
[0029] The same procedure was repeated using anhydrous NiCl 2 without pre-drying. In this case, only about 90% of extraction was achieved after about 5 hrs, as illustrated by curve E in the graph of FIG. 2 .
[0030] The above experiments indicate that changes in drying temperature, hydrogen reduction temperature, and in the composition of the nickel chloride may lead to variations in extraction rates and the time required to achieve the desired extraction.
EXAMPLE 2 (COUNTER EXAMPLE)
[0031] In this example, the feed production procedure described in example 1 was repeated but using NiCO 3 only without nickel chloride addition as the starting material. This feed was reduced to nickel powder as described above and then carbonylation extraction of the nickel powder was carried out in CO gas at 50° C.
[0032] As shown by the curve in the graph of FIG. 3 , a very low extraction of less than 20% was achieved after about 6 hours. It is obvious, therefore, that reduction of NiCO 3 alone did not produce an active nickel powder.
EXAMPLE 3
[0033] The procedure of Example 2 was repeated but with replacement of the starting material with a mixture of NiCO 3 and NiCl 2 in a proportion of 3:1. This feed was reduced to nickel powder as described above and carbonylation extraction of the nickel powder was carried out in flowing CO gas at 50° C. Essentially 100% of the nickel was extracted in less than one hour as shown by the curve in the graph of FIG. 4 .
[0034] Other amounts of mixture blends of nickel carbonate and nickel chloride were tested and satisfactory results were obtained starting with about 5% by weight of NiCl 2 in the mixture. Increasing the proportion of NiCl 2 resulted in a more complete extraction of nickel and increasing the surface area of the mixed solids resulted in a faster extraction of nickel. Thus, the presence of NiCl 2 in admixture with other nickel salts, including possible other compounds that may be present during production of such salts (for example sodium chloride, calcium chloride, magnesium chloride, sodium carbonate, nickel sulphate and calcium sulphate), produces a satisfactory and rapid conversion of the total nickel present in such mixtures into active nickel.
[0035] Larger scale atmospheric carbonylation tests, using feed quantities up to 500 g, have also been carried out and gave similar results as those described in the above examples. However, in this larger equipment extractions from active nickel typically required times of 3 to 6 hours, which was considerably less time than required for extraction from regular nickel powder.
EXAMPLE 4
[0036] A 300 g sample of active nickel powder produced in accordance with the present invention was subjected to pressure carbonylation with CO gas in a small vertical reactor at 300 psi (20 atm) and 85° C. Essentially 100% of the nickel was extracted in less than 10 hours, as shown by curve F in FIG. 5 .
[0037] For comparison, a 300 g sample of non-activated nickel powder was treated in the same manner with CO gas at 300 psi and 85° C. Extraction of nickel from non-activated nickel powder required over 20 hours, as shown by curve G in the FIG. 5 .
[0038] As previously mentioned, it is already known in the art that nickel can be extracted by carnonylation with CO gas at super-atmospheric pressures and at elevated temperatures above 70° C. The present example shows that when such known carbonylation is carried out using the active nickel powder of the present invention, a considerable reduction in the time required for nickel extraction is achieved.
EXAMPLE 5
[0039] In this example, the feed production procedure described in example 2 was repeated. This feed was reduced to nickel powder in 20 minutes at 500° C. but 1-2 volume per cent HCl gas was added to the hydrogen used for reduction. Carbonylation extraction of the resulting active nickel powder was carried out in flowing CO gas at 50° C. As shown by the curve in the graph of FIG. 6 , 98% of the active nickel was extracted in less than three hours.
EXAMPLE 6
[0040] In this example nickel chloride was not added to the feeds which were prepared by both the wet-mix and the dry-mix methods. For the wet-mix, an admixtures of water, nickel carbonate and chromium chloride was stirred together and then dried 110° C. to remove all the free water. Both wet and dry admixtures were reduced in hydrogen gas at 450° C. Carbonylation extractions of the resulting nickel powders were carried out in CO gas at 50° C.
[0041] As shown by the curves in the graph of FIG. 7 , 97.6% (H) of the nickel was extracted in less than one hour from wet mixed feed compared to only 10% (I) of the nickel extracted from the dry mixed feed in the same period. As described above the wet mixing is thought to allow the formation of nickel chloride in the wet admixture by metathesis reaction in solution (exchange of anions).
EXAMPLE 7
[0042] A feed material was made by wet mixing nickel carbonate and nickel chloride electrolyte such that the chloride to total nickel weight ratio was 0.2 and this was divided into four samples. As shown by the curves in the graph of FIG. 8 , additions of 1 weight % chromic chloride (J), ferric chloride (L) and ferrous chloride (M) were separately made to three samples. The fourth sample (K) was the same feed as the three other samples but without additive. Feeds were reduced in hydrogen at 500° C. and the resulting nickel powder was then further cooled to 200° C. The reactive gas was switched from hydrogen to carbon monoxide at a flow rate of 10 ml/min and the nickel powder was then further cooled to 50° C. Carbonylation extraction of the nickel powder was carried out in CO gas at 50° C. Iron chlorides slowed the nickel extraction slightly but chromium did not.
[0043] It should be noted that the invention is not limited to the specific embodiment and examples described above, but that various modifications obvious to those skilled in the art can be made without departing from the invention and the following claims.
|
Active nickel powder is produced by reducing a feed material, containing one or more reducible nickel salts, such that when nickel chloride is present, the weight ratio of chloride to total nickel is greater than 0.1 and the reducible nickel salts have a surface area in excess of 1 m 2 /g, with a reducing gas containing preferably at least 20 volume per cent hydrogen, at a temperature preferably between 300° C. and 600° C., and when nickel chloride is not present, by adding hydrogen chloride directly to the reducing gas. The resulting active nickel powder can be rapidly converted into nickel carbonyl by reaction with a gas containing carbon monoxide preferably at atmospheric or super-atmospheric pressure, in the absence of conventional carbonylation catalysts.
| 2
|
BACKGROUND OF THE INVENTION
The present invention relates to a method and apparatus for controlling the air-fuel ratio of internal combustion engines, or more in particular to a method and apparatus for air-fuel ratio control in which the air-fuel ratio is controlled to an optimum value associated with the optimum fuel consumption rate by feedback control.
Generally, the air-fuel ratio is set to a stoichiometric ratio or a leaner value than that with emphasis placed on the fuel consumption rate under general running conditions, that is, to about 13 or a value with the highest output while the acceleration pedal is depressed to the full such as when ascending a slope, and to a value considering the stability when idling.
In the conventional air-fuel control under general running conditions, the carburetor is subjected to open-loop control and some loss of the fuel consumption rate is caused by variations between internal combustion engines, the secular variation of the internal combustion engine involved and variations between carburetors. An electronically-controlled fuel injection system for measuring the intake air amount of the internal combustion engine with an air flow sensor or the like, computing the required fuel amount with a computer or the like and injecting the fuel from fuel injectors according to the computation practically uses a closed loop control for deciding the direction of the stoichiometric ratio (about 15) from the oxygen sensor provided in the exhaust pipe and for correcting the fuel amount. Also, a closed loop control for the carburetor in which the air amount of the air bleed is corrected by determining the direction of the stoichiometric ratio by the oxygen sensor finds partial applications. These closed loop controls are capable of correcting the variations of the air-fuel ratio, but result in the loss of fuel consumption rate since the stoichiometric ratio is not a value associated with the best fuel consumption rate.
A conventional method has been suggested for controlling the fuel consumption rate without the above-mentioned loss. In such a control method, the air bypassing an air amount sensor and the throttle valve is made to dither at regular intervals of time between rich and lean sides of the air-fuel ratio, the direction of the air-fuel ratio associated with an improved fuel consumption rate is determined, and the air-fuel ratio is corrected by an auxiliary air valve bypassing the air amount sensor. In this method, the engine is run once at each of the relatively rich and lean levels of the air-fuel ratio, so that the engine speed Ner for the rich air-fuel ratio is compared with the engine speed Nel for the lean air-fuel ratio, and if Ner is larger than Nel, the bypass air amount is reduced, while if Ner is smaller than Nel, the bypass air amount is increased.
In determining the change of output from the engine speed which is changed by various factors, however, the above-mentioned conventional method of control is incapable of determining whether the engine speed is changed by the change of the air-fuel ratio or operation of the acceleration pedal or by ascending or descending a slope, with the result that the control may be effected in the direction reverse to the improvement of fuel consumption rate, thus deteriorating the fuel consumption rate. Further, the air passing through the air amount sensor may change and also may not change in cases when the air is applied through a bypass of the air amount sensor and the throttle valve and when the air is not applied therethrough, and it could not be assumed that a fuel flow rate is always constant. As a result, it may occur that the best fuel consumption rate is not achieved but a loss is caused.
SUMMARY OF THE INVENTION
In view of the above-mentioned disadvantage of the conventional systems, an object of the present invention is to provide a method and apparatus for controlling the air-fuel ratio in which while controlling the air-fuel ratio by detecting the change of engine speed under operating conditions associated with at least two different air-fuel ratios, the internal combustion engine is always controlled to be operated with the optimum fuel consumption rate.
According to the present invention, there is provided a method and apparatus for controlling the air-fuel ratio, in which the air supply amount in a bypass of an air supply path is changed between at least two different air-fuel ratios near an optimum air-fuel ratio, the engine is operated for a predetermined length of time alternately between the two air-fuel ratios in such a manner that the fuel flow rate for the leaner of the two air-fuel ratios is the same as that for the richer one thereof, signals representing the rotational speed of the internal combustion engine, torque or other operating conditions related thereto are detected at a plurality of operating points when the engine is operated at these different air-fuel ratios, the signals thus detected are compared at the operating points thereby to decide whether the optimum air-fuel ratio is rich or lean as compared with the air-fuel ratio associated with the optimum fuel consumption rate, and the amount of fuel is regulated thereby to correct the air-fuel ratio on the basis of the result of the decision.
According to the present invention, in controlling the air-fuel ratio of internal combustion engines by detecting the change of engine speed under the operating conditions for at least two different air-fuel ratios, through correction of the change of the fuel flow rate between the lean step with an electromagnetic valve open and the rich step with the electromagnetic valve closed the internal combustion engine can be controlled to operate always at the optimum fuel consumption rate.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram showing an apparatus for controlling the air fuel ratio of an internal combustion engine according to an embodiment of the present invention.
FIG. 2 is a block diagram showing a computing circuit of FIG. 1.
FIG. 3 is a flowchart showing the processing operation of the computing circuit.
FIG. 4 is a detailed flowchart of the learning map correction amount computing step shown in FIG. 3.
FIG. 5 is a diagram showing the map in the RAM of FIG. 2.
FIG. 6 is a detailed flowchart of the dither correction amount computing step shown in FIG. 3.
FIG. 7 is a diagram showing the secular variation of the processing operation shown in FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
An embodiment according to the present invention is shown in FIG. 1. The air-fuel control system shown in FIG. 1 comprises an internal combustion engine 1, a rotational angle sensor 2 constructed integrally with a distributor, an intake pipe 3 placed downstream of the throttle valve 4, the throttle valve 4 interlocked operatively with the acceleration pedal, and an air flow sensor 6. The air flow sensor 6 is for detecting the air flow rate in such a manner that the opening of a baffle plate in the air path is changed with a flow rate of air and the output voltage generated by the sensor changes with the opening of the baffle plate. The air-fuel ratio control system shown in FIG. 1 also comprises an air-introducing downstream pipe 5 connecting the air flow sensor 6 and the throttle valve 4, an air cleaner 8, an air introducing upstream pipe 7 connecting the air cleaner 8 and the air flow sensor 6, a pressure sensor 9 for detecting the pressure of the intake pipe, a bypass air electromagnetic valve 12 installed to bypass the air amount sensor 6 and the throttle valve 4, a bypass downstream introducing pipe 10 for connecting the bypass air electromagnetic valve 12 and the intake pipe 3, a bypass upstream introducing pipe 11 connecting the bypass air electromagnetic valve 12 and the air introducing upstream pipe 7, and a computer 13. In response to the signals from the air amount sensor 6 and the rotational angle sensor 2, the computing circuit 13 computes the injection amount of the injection valve 14 for time being as a pulse duration and generates an output signal to be supplied to the electromagnetic injection valve 14 for intermittently injecting the fuel maintained at a predetermined pressure according to the pulse duration.
The computer 13 will be described in detail with reference to FIG. 2. Numeral 100 designates a microprocessor (CPU) for computing the pulse duration for the injector, and numeral 101 designates an engine speed counter unit for measuring the engine speed in response to the signal from the engine rotational angle sensor 2. The engine speed counter unit 101 applies an interruption command signal to the interruption control section 102 in synchronism with the engine rotations. In response to this signal, the interruption control section 102 applies an interruption signal to the microprocessor 100 through a common bus 150. Numeral 103 designates a digital input port for transmitting to the microprocessor 100 a digital signal such as a starter signal from the starter switch 16 for turning on and off the operation of the starter (not shown). Numeral 104 designates an analog input port including an analog multiplexer and an A/D converter and has the function to cause the signals from the air-flow sensor 6, the pressure sensor 9 and the cooling water temperature sensor 15 to be subjected to A/D conversion and read into the microprocessor 100. The output data of the units 101, 102, 103 and 104 are applied to the microprocessor 100 through the common bus 150. Numeral 105 designates a power supply circuit for supplying power to the RAM 107 described later. Numeral 17 designates a battery and numeral 18 a key switch. The power supply circuit 105 is connected directly to the battery 17 but not through the key switch 18. The RAM 107 is thus impressed with the power supply all the time regardless of the position of key switch 18. Numeral 106 also designates a power supply circuit, which is connected through the key switch 18 to the battery 17. The power supply circuit 106 is for supplying power to the parts other than RAM 107. The RAM 107 is a temporary memory unit used temporarily while the computer 13 is programmed for operation and provides a nonvolatile memory supplied with power always regardless of the key switch 18 so that the data stored therein is not erased even when the engine operation is stopped by turning off of the key switch 18. The learning map correction amount ΔT is also stored in this RAM 107. Numeral 108 designates a read-only memory (ROM) for storing various constants and a program. Numeral 109 designates a fuel injection time control counter including a register and provides a down counter for converting a digital signal representing the open time of the fuel injector 14, namely, the fuel injection amount computed at the microprocessor (CPU) 100 into a pulse signal of time duration representing the actual open time of the fuel injector 14. Numeral 110 designates a power amplifier section for driving the fuel injector 14. Numeral 111 designates a timer for measuring the elapsed time and applying it to the CPU 100.
The rotational speed counter unit 101 is for measuring the engine rotational speed by measuring the time of each engine rotation and supplies an interruption command signal to the interruption control section 102 at the end of the measurement. In response to this signal, the interruption control section 102 generates an interruption signal and causes the microprocessor 100 to execute the interruption processing routine for computing the fuel injection amount.
The processes of the processing operation at the computer 13 is shown in the flowchart of FIG. 3. When the key switch 18 and the starter switch 16 are turned on thereby to start the engine 1, the process is started from the step S1. At step S2, the condition of the electromagnetic valve and the counter of injection number n are initialized, i.e. the electromagnetic valve is closed and the injection number n is reduced to zero. The step S3 computes the engine condition correction factor K1 in response to the starter switch 16 and the engine cooling water temperature sensor 15 and stores the result of computation into the RAM 107. At step S4, the learning map correction amount ΔT described later is computed and the result is stored in RAM 107.
FIG. 4 shows detailed flowchart of the step S4 for computing the learning map correction amount ΔT. At step S400, it is decided whether or not the feedback is established for controlling the engine to the best fuel consumption rate, that is, whether or not the cooling water temperature is higher than 70° C. and the starter switch is turned off. If the feedback condition is not established, the process of step S4 is completed and the process is passed to step S3. If the feedback condition is established, on the other hand, the process proceeds to step S401 for deciding whether or not the injection count n has reached the set number D. Until the set number D is reached, the correction amount ΔT is not computed but the process of step S4 is completed and passed to step S402.
Referring to FIGS. 2 and 3, normally, the processing operation of the main routine including steps S3 to S4 are repeatedly executed according to the control program. In response to an injection interruption signal from the interruption control 102, the microprocessor 100 immediately suspends the processing operation of the main routine and is transferred to process the interruption processing routine of the step S100. The step S101 fetches the number of pulses N for each crank angle of 360 degrees representing the engine rotational speed Ne from the rotational speed counter 101, fetches the intake air amount signal and the intake pressure signal from the analog input port 104, and computes and stores in the RAM 107 the engine rotational speed Ne, the intake air amount Qa and the intake pressure Pm. At step S102, the basic pulse duration Tm is computed to attain the stoichiometric air-fuel ratio (about 15) from the present rotational speed Ne and the intake air amount Qa. Step S103 decides whether or not the feedback condition is established in a manner similar to step S400, and if the feedback condition is not established, the process is passed to the step S104 for computing the final output pulse duration Ti of the injection valve from the equation below.
Ti=K.sub.1 ×Tm
Then at step S105, since the feedback is not involved, the close signal of the bypass air electromagnetic valve is applied to the electromagnetic valve control section 112. At step S106, the injection number n is set to zero. If the feedback condition is established at step S103, in contrast, the step S103 branches to "Yes," and at step S107, the learning correction amount ΔT (p,r) corresponding to the engine rotational speed Ne and the intake pressure Pm is read from the map as shown in FIG. 5 in RAM 107.
The memory shown in FIG. 5 is made up of a nonvolatile memory in the computer for dividing the rotational speed Ne and the intake pressure Pm at predetermined intervals and stores ΔT (p,r). Referring to FIG. 3, step 108 is for computing the dither correction amount K 2 for maintaining constant the fuel flow rate per hour regardless of the operation of the electromagnetic valve in the case where the operation of the bypass air electromagnetic valve causes the amount of air flowing in the air amount sensor 6 to change so that the basic pulse duration Tm is changed thereby to cause an unstable amount of fuel injected.
Let us consider the manner in which the intake air amount Qa is changed by the operation of the electromagnetic valve 12. In the case where the opening of the throttle valve 4 is constant, the intake air amount Qa is determined by the pressures Pb and Pm shown in FIG. 1. When the pressure Pm is below the critical level, the velocity of air passing through the throttle valve 4 is equal to the velocity of sound, and therefore regardless of the operation of the electromagnetic valve 12, the amount of air passing through the air amount sensor 6 is maintained constant, so that the basic pulse duration Tm remains unchanged.
As the pressure Pm approaches Pb, the effect of the electromagnetic valve increases. The change of air amount passing through the air amount sensor 6 due to the opening or closing of the electromagnetic valve is negligible as compared with the change of the bypass air passing through the electromagnetic valve 12. Nevertheless, this slight change of air amount passing through the air amount sensor 6 is important, since without changing the bypass air amount with a fixed fuel flow rate, it is impossible to control the fuel consumption rate in the true sense of the word.
FIG. 6 shows a detailed flowchart of the step S108 FIG. 3. Step S1081 decides whether or not n=0, namely, whether or not the electromagnetic valve is in initial stage of switching and is open. If n=0 and the electromagnetic valve is open, the step S1081 branches to "Yes," so that the dither correction amount K 2 is determined at step S1082.
The dither correction amount K 2 will be explained with reference to the time chart of FIG. 7. If the present total number of injections is 48, the average value of the basic pulse (Tm r-1, Tm l-1) and the average value of rotational speed (Ne r-1, Ne l-1) in the immediately preceding closed state of the electromagnetic valve (32 to 48 in the number of times of injections) and in the second preceding open state thereof (16 to 32 in the number of times of injections) are used to compute the value K 2 from the equation below, which is stored in RAM 107. ##EQU1## When n is not zero or the electromagnetic valve 12 is closed at step S1081, the process branches to "No" to step S1083 where if the electromagnetic valve is open, the processing operation of K 2 is completed. If the electromagnetic valve is closed, on the other hand, the value K 2 is set to 1.0 at step S1084 without dither correction by K 2 . In this way, when the electromagnetic valve is open, the decreased fuel flow rate is computed from the preceding engine conditions, so that without storing the correction factor K 2 for all the engine operating conditions, it is possible to determine an accurate correction factor by a simple computation.
Returning to FIG. 3, the step S109 computes the output pulse duration Ti fed back by the equation below.
Ti=K.sub.2 ×Tm+ΔT(p,r)
At step S110, the number of injections n is changed to n+1 for count up, after which the step S111 sets the output pulse duration of the injection valve 14 at the counter 109. The process then proceeds to step S112 for returning to the main routine.
When the number n reaches D at step S401 in FIG. 4 (namely, D=16, or 16 injections in the time chart of FIG. 7), the number of clock pulses determined in the second half of the dither period, namely, the number of clock pulses C shown in FIG. 7 is compared for the four preceding rotational periods including the present period. The number of clock pulses is counted for the second half of the dither period for the reason that the change of the air-fuel ratio due to the bypass air electromagnetic valve 12 has fully affected the rotational speed. Step S402 checks to see whether the electromagnetic valve is presently open or closed, and if it is closed, the process is passed to step S403 where the numbers of clock pulses C l-1 , C r-1 , C l and C r for the four rotational periods are compared with each other, where C r is the number of clock pulses for the present rich step, C l is the number of clock pulses for the immediately preceding lean step (electromagnetic valve open), C r-1 is the number of clock pulses for the second preceding rich step (electromagnetic valve closed) and C l-1 is the number of clock pulses for the third preceding lean step.
Step S403 decides whether or not the relation C l-1 >C r-1 <C l >C r holds as a result of the comparison mentioned above, and if this relation holds, the process branches to "Yes" to the step S408. This indicates that when the rotational speed increases at a rich step and decreases at a lean step, an increased fuel amount increases the rotational speed, thus improving the fuel consumption rate. Steps S407 and S408 compute the pulse duration learning correction amount ΔT(p,r) The correction amount ΔT(p,r) corresponding to the present rotational speed Ne and the intake pressure Pm is read from the corresponding address of the map formed in the nonvolatile memory region in the computing circuit, and ΔT is added or subtracted, so that the value ΔT(p,r) after this computation is written to the corresponding address of the memory anew.
In the case where the relation C l-1 >C r-1 <C l >C r does not hold at step S403, the process is passed to step S404. The condition C l-1 <C r-1 >C l <C r of step S404 is established when the engine is run at the air-fuel ratio richer than the air-fuel ratio associated with the best fuel consumption rate. In that case, the process is passed to step S407 where Δt is subtracted from the memory correction amount ΔT(p,r) corresponding to the operating conditions involved and the result is stored. Specifically, the injection amount is reduced by the amount corresponding to Δt in pulse duration to approach the optimum fuel amount. If the relation C l-1 >C r-1 <C l >C r or C l-1 <C r-1 >C l <C r does not hold, the learning map correction amount ΔT is not corrected.
If the step S402 decides that the electromagnetic valve is open or a lean step is involved, the process is passed to step S405, and if the relation C r-1 <C l-1 >C r <C l holds the process proceeds to step S408 for adding Δt to the correction amount ΔT (p,r) and storing the result thereof. If the relation C r-1 <C l-1 >C r <C l does not hold at step S405, the process branches to "No," followed by the step S406 for deciding whether or not the relation C r-1 >C l-1<C r >C l holds. If this relation holds, the process branches to "Yes" so that Δt is substracted from the correction amount ΔT(p,r) and the result is stored. In the event that this relation does not hold, by contrast, the process branches to "No," in which case the correction amount ΔT(p,r) is not corrected. Upon completion of the correction of the correction amount ΔT(p,r) the process is passed to step S409 where the count n of the number of injections is set to zero, followed by step S410 where if the electromagnetic valve is open thus far, a close signal is applied to the electromagnetic valve control section 112, and vice versa. The computation of the learning map correction is now over, followed by the process of step S3.
The aforementioned control operation permits the air-fuel ratio to be controlled to the level associated with the optimum fuel consumption rate by correction of the air-fuel ratio if it is displaced from the level associated with the optimum fuel consumption rate under steady engine operation. Also, since the optimum correction amount ΔT(p,r) for each operating condition is stored, each operating condition is controlled to optimum state. The flow rate in the bypass air electromagnetic valve 12 is selected in such a manner as to satisfy both the drivability and the ability of detecting the change of the rotational speed, while the fuel correction amount Δt is selected to be 1/2 or less or the change of the air-fuel ratio by the bypass air electromagnetic valve 12.
In the aforementioned embodiment, the dither correction amount K 2 is determined from the ratio of fuel flow rate between the immediately preceding dither state and the second preceding dither state. Instead of this method, the value K 2 based on the engine rotational speed and the intake pressure may be stored in advance in ROM.
Further, the ratio of fuel flow rate ##EQU2## may be replaced by ##EQU3## involving only the pulse durations.
|
In an air-fuel ratio control system the air-fuel ratio is changed by changing the auxiliary air supply amount in a bypass path with respect to a main path for supplying air to the engine in the vicinity of an optimum air-fuel ratio. Signals representing the operating conditions such as rotational speed of the engine operated at the resulting different air-fuel ratios are detected at a plurality of operating points. The signals thus detected are compared and the fuel injection amount is regulated thereby to correct the air-fuel ratio so that the fuel consumption rate may become optimum.
| 5
|
BACKGROUND OF THE INVENTION
The invention relates to a device for the transfer of harness elements from a conveying member in a drawing-in machine for warp yarns onto carrying members of a weaving machine, with an ejector for removing the harness elements from the conveying member.
EP 500 848 has already disclosed such a device, in which the carrying members, designed as carrying rails, have an oblique entry flank directed downwards. Ejectors push the harness elements from carrying pins of a conveying member up onto these entry flanks, so that the harness elements slide along these entry flanks onto the carrying rails. The carrying rails are retained or supported against gravity by holding bolts which are capable of being moved in and out and which are fastened to a transport system. In their moved-in position, these holding bolts position the carrying rails. The holding bolts are moved out in order to allow the harness elements to pass at the relevant point.
A disadvantage of the known device mentioned is to be seen in that, in order to allow the harness elements to pass, the guidance or support of the carrying rails is temporarily removed precisely when the harness element passes over from the carrying pins of the conveying member onto the carrying rail. This puts exact alignment of the carrying pins and carrying rails at risk. This adverse circumstance can, admittedly, be eased by arranging the said guide of the carrying rails as far as possible from the conveying member, but, even then, the exact alignment of the carrying pins and carrying rails is impaired.
SUMMARY OF THE INVENTION
The invention, provides a device in which the carrying members are aligned as exactly as possible at the moment when the harness elements are transferred onto them.
This is achieved in that the carrying members or carrying rails are guided by a guide roller which is arranged very near the end of the carrying member at the conveying member and which has guides for the carrying member which guide the latter in two orthogonal directions, that is to say laterally and in the direction of gravity, during the transfer of the harness elements. The guide roller has a recess which, starting from the circumference, extends towards the axis and serves, on the one hand, for providing space for the lock-transfer of the end eyes of the harness elements and, on the other hand, for providing an engagement surface for the forward movement of the harness elements on the carrying member by means of the guide roller. In this case, the guide roller, together with the recess, forms a transfer lock for the harness elements.
The advantages achieved by means of the invention are to be seen, in particular, in that the carrying member is guided in an exact and defined manner at the moment when the harness elements are transferred from the conveying member, guidance for the lock-transfer of the harness elements being partially cancelled only when the harness element has already been taken up by the carrying member. In this case, the carrying members are always guided laterally by the guide roller, whatever the position of the latter. Another advantage is to be seen in that the guide roller executes a simple rotational movement and, at the same time, propels the harness elements some distance forwards. The guide roller may be designed for any number of adjacent carrying members. While a single harness element is being propelled forwards by the guide roller, the latter additionally holds back harness elements which have already been transported, so that these cannot be pushed towards the conveying member again.
BRIEF DESCRIPTION OF THE DRAWING
The invention is explained in more detail below by means of an example and with reference to the accompanying figures:
FIG. 1 is a schematic sectional view of the device according to the invention.
FIG. 2 shows part of the device on an enlarged scale.
FIG. 3 shows a view of the device in a first operating phase, the said view having been pivoted through 90° in relation to FIG. 1 .
FIGS. 4 and 5 show the device in two further operating phases.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a section through part of a guide roller 1 for a plurality of carrying members 2 , 3 , 4 , which are arranged next to one another at equal intervals. The guide roller 1 is mounted on a shaft 5 rotatably about an axis 6 in a way not illustrated in any more detail, but known per se, and is connected to a drive 7 . The guide roller 1 has lateral guides 8 , 9 for guiding the carrying member 4 in the direction of an arrow 10 and guides 11 for guidance in the direction of an arrow 12 , and therefore for guidance in two orthogonal directions. The guides 8 , 9 are interrupted or widened in the region of a recess 13 and therefore do not form a closed circular ring. A harness element 14 , which is located on the carrying member 4 , is depicted in the recess 13 . A region delimited by an arc of a circle 15 shows a section through the guide roller 1 , this section in turn, being located in the region of the guides 8 , 9 , 11 , although, in this case, the carrying member 2 , which is guided by these guides 8 , 9 , 11 , is depicted.
FIG. 2 once again shows, on an enlarged scale, the carrying member 2 together with the guides 8 , 9 , 11 of the guide roller 1 .
FIG. 3 shows, from another viewing angle, the arrangement of the guide rollers in or in front of a drawing-in machine for warp yarns. Since the harness elements 16 , illustrated diagrammatically here, have an eye 17 , 18 at the top and bottom in each case, two carrying rails 19 , 20 are also provided as carrying member. The drawing-in machine has, as part of a conveying member 21 , 21 ′ for each harness element, two holding bolts 22 , 23 , a plurality of which are arranged next to one another, for example, on a rotating chain in each case, as is known, for example, from EP 500 848 already mentioned. Moreover, the drawing-in machine preferably has two ejectors 24 , 25 , which are each illustrated here in the initial position 26 , 27 and in the end position 28 , 29 . These ejectors are capable of executing a lifting movement out of the initial position into the end position. However, such ejectors 24 , 25 are known per se and therefore the way in which they are driven is not described in any more detail either. A guide roller 30 , 31 is also provided for each carrying rail 19 , 20 . The said guide rollers are illustrated in section here, the section running in a plane which is illustrated in FIG. 1 by a broken line 32 and, in principle, passes through the center of the harness elements. Thus, the recess 33 , 33 ′, which corresponds to the recess 13 (FIG. 1) and which, starting from the circumference 34 , 34 ′, extends towards the axis 35 , is also rendered clearly visible. The recess 33 causes the guide 36 , corresponding to the guide 11 (FIG. 1 ), to extend approximately over three quarters of the circumference. This proportion is greater for the lateral guides 37 , 38 , which correspond to the guides 8 , 9 (FIG. 1 ). The guide roller is arranged very near the end 46 , 47 of the carrying rails 19 , 20 or of the carrying member and so as to be adjacent to the conveying member 21 , 21 ′.
FIG. 4 again shows the same elements as FIG. 3 . These elements are therefore also given the same reference symbols. However, the guide rollers 30 , 31 and the harness element 16 have assumed a different position. The harness element 16 has been grasped by guide surfaces 39 , 40 in the recesses 33 , 33 ′ and moved on the carrying rails 19 , 20 . The ejectors 24 , 25 are still in their end positions 28 , 29 .
FIG. 5 shows, yet again, the same elements as FIG. 3 . Here, the harness element 16 is illustrated as having been transported even further.
The device operates as follows: A harness element 16 , such as, for example, a heald or drop wire, is guided in a way known per se, on two holding bolts 22 , 23 , in front of the carrying rails 19 , 20 by synchronously rotating conveying members 21 , 21 ′. The ejectors 24 , 25 then move out of the initial positions 26 , 27 into the end positions 28 , 29 , the end eyes 17 , 18 of the harness element 16 being stripped from the holding bolts 22 , 23 in the direction of an arrow 45 and being pushed onto the carrying rails 19 , 20 . During this time, the carrying rails 19 , 20 are guided laterally by the guides 37 , 38 , 37 ′ 38 ′ and vertically by the guide 36 , 36 ′. The harness element 16 is then grasped by the guide rollers 30 , 31 , which rotate in the direction of the arrows 41 , 42 . Since the channel defined by the guides 8 , 9 , 11 (FIG. 1) and 36 , 37 , 38 and 36 ′, 37 ′ 38 ′ is as narrow as a carrying rail 19 , 20 , but narrower than an end eye 17 , 18 , a boundary 43 , 44 of the recess 33 , 33 ′ forms a guide surface 39 , 40 (FIG. 4 ), along which the end eyes 17 , 18 slide and, at the same time, are moved further on the carrying rail 19 , 20 . In this case, the guidance of the carrying rails 19 , 20 by the guides 36 , 36 ′ is lost for a short time in the region of the position as shown in FIG. 4, but this is not a disadvantage, since the transfer of the harness element 16 onto the carrying rails 19 , 20 has already taken place. The lateral guidance of the carrying rails by the guides 8 , 9 (FIG. 1) and 37 , 38 and 37 ′, 38 ′ is always maintained. In the position shown in FIG. 5, guidance is once again effective on all sides. From then on, the guide roller 30 , 31 , via the circumference 34 , 34 ′, supports the harness elements against backward movement.
The rotational movement of the guide roller may be continuous or controlled in a specific manner by means of control and monitoring elements. In the case of continuous movement, the position of the recesses 13 , 33 give rise to periods of time in which the ejectors 24 , 25 can eject the harness element 16 . However, the movement of the guide roller may also be governed by the conveying member 21 , so that the guide roller waits in a position according to FIG. 3 until the ejectors 24 , 25 have performed their task. The guide roller then executes a complete revolution as quickly as possible, in order to return to the position according to FIG. 3 . In this case, the guide roller may be driven by means of a DC motor or a stepping motor. Corresponding rotary transducers have to be provided for monitoring the position. In any event, however, the drive 7 is operatively coordinated with the drive of the ejectors 24 , 25 , as can be gathered from the manner of operation described.
|
A device is used for the transfer of harness elements ( 21 ) from a conveying member ( 21 ) in a drawing-in machine for warp yarns onto carrying members of a weaving machine, that has an ejector for removing the harness elements from the conveying member. In order to provide a device in which the carrying members are aligned as exactly as possible at the moment when the harness elements are transferred onto them, there is provided a guide roller for the harness elements which is mounted rotatably about an axis and which has guides for the carrying member which guide the carrying members in two orthogonal directions.
| 3
|
BACKGROUND OF THE INVENTION
The present invention relates to a pressure-control injector for injecting fuel with a double valve.
The fuel injection systems commonly used for direct injection and internal combustion engines nowadays contain a high-pressure collecting chamber (common rail). In addition to a high pressure collecting chamber the injection system includes injectors which project into a combustion chamber of an internal combustion engine to be supplied with fuel. Upon injection the demand for the fuel quantity to be injected and the starter injection is exceptionally important and must take into consideration the ignition leg. Moreover, the injectors represent mechanically loaded components whose fatigued strength at favorable manufacturing costs must not fall below the service life of the internal combustion engine.
Reference numerals EP 0 657 642 A2 and DE 197 01 879 A1 each disclose a fuel injection device for combustion engines. More specifically, each of these documents describes a fuel injection device that includes a high pressure pump which is assigned to a high pressure accumulating chamber (common rail) that is to be filled with fuel. A high pressure accumulating chamber is connected via injection lines with injection valves projecting into the combustion chamber of the internal combustion engine. The opening or closing movements are controlled respectively by an electrically control valve. The control portion is formed as a 3/2 way valve, which is connected with the injection line or a release line to a high pressure channel opened to an injection opening of the injection valve. A hydraulic working chamber or a pressure release chamber fillable with high pressure fuel is provided on a control member of the control part. The working chamber is controllable for adjustment of the set position of the control member of a release channel. As the case may be, during a pause an injection a connection between the injection valve and the release chamber can be created. Both these devices have a considerable overall height.
SUMMARY OF THE INVENTION
Accordingly, it is an object of present invention to provide a pressure-control injector for injecting fuel with a double valve, which avoids the disadvantages of the prior art.
In contrast to the devices described above, the present invention provides a 3/2-way valve which has a very compact construction and can be produced in a cost effective manner due to the use of ball-shaped bodies. The ball-shaped bodies arranged as ball valves opposite to one another represent simple standard parts, which based on the geometry, allow an optimal pressure distribution of the surface to receive the pressure. In addition, the solution proposed in the present invention makes possible the production of a simply constructed 3/2 valve without the need for relative movements of a seat surface.
The positioning of the balls lying opposite to one another on and supported by a common guide, bring about a self-centering of the balls in their respective ball sockets in a simple manner. Another manufacturing advantage associated with the valve configuration is that the ball sockets lye freely on or on top of the faces of the guide, and by the respective pressure forces take care of the centering itself with reference to a center line of the injector. The ball sockets are composed of a soft metal or a soft metal alloy to facilitate a secure support and to ensure an optimal fitting to the ball surface geometry. Thus, with the configuration of the injector in accordance with the present invention adjusting plate is avoided in the life of the injector, and a centering of the ball sockets and the balls received therein relative to the guide and thereby to the line of symmetry of the injector is realized. The guide which has the ball sockets.
The guide which has the ball sockets on its upper and lower sides is provided with free spaces which permit a longitudinal flow of the pressurized fuel upon pressure release of the control chamber by regulation of a 2/2 valve. A pressure release of the nozzle chamber of the injection nozzle takes place through a pressure release of the nozzle inlet and the pressure chamber connected thereby via the ball valve on the control chamber side to which upon closing of the common rail the nozzle inlet line releases various oil.
With the use of a high pressure receiving chamber line which is angled at 90°, its connection to the injector body is lateral, and the height of the inventive injector is favorably affected or in other words minimized.
The novel features which are considered as characteristic for the present invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together with additional objects and advantages thereof, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view showing a longitudinal cross-section through a housing of an injector with ball valves located opposite to one another and supported on a guide and ball sockets for receiving the ball valves, in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
An injector for injecting a high pressure fuel in a combustion chamber of the internal combustion engine shown in FIG. 1 has an injector housing 2 with an inlet 5 coming from a high pressure collecting chamber open beneath a dividing seam 35 . For space saving purposes the inlet 3 from the high pressure collecting chamber is formed as a bore extending at an angle of 90°, so that inside the injector housing 2 beneath a guide 19 a hollow chamber 28 can be located in order to create an injector 1 with particularly compact dimensions.
A bore 4 is provided in the injector housing 2 and branches off from the inlet 3 to the high pressure collecting chamber. The bore 4 opens into a control chamber 6 via an inlet throttle 5 . These features make possible that in a control chamber 6 a constant and adequate control volume is maintained under high pressure. The control chamber 6 which actuates the vertical movement of the guide 19 is associated with a 2/2-way valve. The 2-2/way valve can be a hydraulic/mechanical regulating unit, a piezo actuator, or a magnetic valve, as is not specifically shown in FIG. 1 .
By means of this not shown element which makes possible the advantageous and short response and control time features which are even more important with high rotational speed of the internal combustion engine, a sealing body 8 is pressure-unloaded with a corresponding control. Thereby the sealing body 8 shown here as a ball slides up on its sealing seat 9 and releases an outlet throttle 10 which is located behind a release opening 11 provided above the control chamber 6 . The control chamber 6 is balanced by regulation of the 2/2-way valve 7 .
By balancing of the control chamber 6 a control chamber piston 12 located opposite to the release opening 11 descends into the control chamber 6 . The pole 17 of the ball valve 16 on the control chamber side which lies on a contact point 15 of the control chamber piston 12 moves upwardly and closes off the waste oil line 14 which branches transversely relative to the control chamber piston 12 in the injector housing 2 . The control chamber piston 12 is formed with a diameter which exceeds the valve diameter 25 on the ball 24 of the oppositely disposed ball valve 23 .
The ball valve 16 provided on the control chamber side as well as the ball valve 23 provided on the high pressure collecting chamber side are received in a hollow chamber provided in the injector housing 2 . The hollow chamber is partially filled by a guide 19 , wherein ball sockets 18 are provided at oppositely located faces of the guide. The ball sockets 18 are freely movable relative to the faces of the guide 18 and preferably composed of a soft, metallic material or a soft metallic alloy. In addition of the ball sockets 18 , a rounded portion 26 or 27 is formed, each of which corresponds to the ball 17 or 24 received in the ball sockets 18 .
Based on this construction of the ball sockets 18 composed of soft metal an exact fit of the radius of curvature of the outer surfaces of the balls 17 or 23 with the socket rounded portions 26 , 27 in the respective ball socket 18 is realized. In connection with this, the construction of the ball sockets 18 enables the balls 17 or 24 to be sufficiently centered to the socket rounded portions 26 , 27 of the ball sockets 18 . Furthermore, the selected configuration provides for a self-centering of the ball socket 18 in the balls 17 and 23 relative to the line of symmetry of the injector housing 2 . From a manufacturing point of view, the arrangement of the ball sockets on the faces of the guide 19 offers advantages, since the sufficient operational position of the guide is independent from a form-locking connection of the ball sockets 18 with the guide 19 during the operation of the inventive injector.
The guide 19 is provided near a guide area 34 with free surfaces or spaces 20 . The guide area 24 serves for guiding the guide 19 free from play in a vertical direction in the hollow chamber in the injector housing 2 . The free spaces 20 permit a longitudinal flow of the pressurized fuel along the free spaces 20 of the guide 19 and introduction of the pressurized fuel through the transverse bore in a longitudinal bore 22 , which represents the nozzle inlet to the nozzle chamber to the injection nozzle needle. The above-described longitudinal flow occurs upon pressure release of the control chamber 6 in the above described longitudinal flow occurs upon pressure release of the control chamber 6 in the above described manner, or in other words by controlling the actuator elements an opening of the oppositely located valves, of the high pressure receiving chamber 3 .
Due to the angled configuration of the inlet 3 to the ball valve 23 on the inlet side, a sealing spring 30 in the hollow chamber 28 can be positioned directly under the inlet 3 from the high pressure collecting chamber in the injection housing 2 . The sealing spring 30 in the hollow chamber 23 abuts against a disc-shape member 29 and lies with its opposite ends on a ball shaped pressure member 31 . An end of the pressure member 31 receives a pin 33 of the nozzle needle 32 , so that the sealing force of the sealing spring 30 on the nozzle needle 32 can be transferred, with the sealing spring 30 pressed in its sealing seat in the area of the injector opening. By regulating of the 2/2 control valves 7 and therefore the pressure release of the control chamber 6 , the control chamber piston 12 descends into the control chamber 6 . The ball 17 of the ball valve 16 on the control chamber side descends into its sealing seat in the injector housing 2 and closes the waste oil line 14 . At the same time the ball 24 of the ball valve 23 located on the lower surface of the guide 19 descends and opens the inlet from the high pressure accumulating chamber. High pressure fuel flows over the inlet 3 into the hollow chamber of the injector housing 2 , passes over the free space 20 of the guide 19 and enters into the nozzle inlet 22 through the transverse bore 21 . The nozzle inlet 22 drains into a nozzle chamber (not shown in FIG. 1 which surrounds the injector nozzle in front of its injector seat). Its position the waste oil line 14 opposite the high pressure is closed by the ball 17 when it descends into its seat in the injector housing 2 .
The ball 24 on the inlet side ball valve 23 is pressed with its valve diameter 25 into its seat in the injector housing upon closing of the inlet 3 from the high pressure collecting chamber. This is performed by an increase of the pressure in the control chamber 6 via the bore and the inlet throttle 5 . Since the diameter 13 of the control chamber piston 12 is larger than the valve diameter 25 of the ball valve 23 , a downward vertical movement of the guide 19 and the hollow chamber within the injector housing 2 occurs, so that the inlet 3 from the high pressure receiving chamber can be closed. At the same time, the ball 17 of the control chamber side ball valve 16 opens the waste oil line 14 . Thus, the nozzle inlet 22 and therefore the nozzle chamber of the injection nozzle can be released by the transverse bore 21 and the upper portion of the hollow chamber of the injector housing 2 , so that the pressure fuel can run back into the tank via the waste oil line 14 .
The main idea of the present invention therefore resides in two ball-shaped ball valves 16 and 23 , each located in a socket 18 of the surface of a guide 19 , wherein the valves self center opposite the seat in the injector housing 2 . This permits a simple manufacture of the component since the tolerances can be favorably chosen and since the self centering can be automatically adjusted, based on the prevailing pressure during operation in both areas of the hollow chamber within the injector housing 2 containing the guide 19 . Therefore this reason a seat surface need not be movable relative to the guide. In addition, the seat surface can be stationary in the injector housing 2 since with the selected geometry of the counter parts, that is the balls 17 and 23 , an adaptation to the final structural conditions of the seat surfaces of the injector housing 2 can be precisely determined. Thus, a seal seat without leakage can be achieved with a favorable selected tolerance in the injector housing 3 .
It will be understood that each of the elements described above, or two or more together, may also find a useful application in other types of constructions differing from the types described above.
While the invention has been illustrated and described as embodied in pressure-control injector for injecting fuel with a double valve, it is not intended to be limited to the details shown, since various modifications and structural changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can, by applying current knowledge, readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention.
|
A fuel injector for injecting pressure fuel in a combustion chamber of an internal combustion engine has an injector housing, an inlet connectable with a high pressure collecting chamber, a nozzle inlet line, a 2/2-way valve for opening and closing the nozzle inlet line, a control chamber in which a pressure change occurs, at least one first ball valve positioned at a side of the control chamber, at least one second ball valve positioned at a side of the inlet, and a guide element movable in the housing, the first and second ball valve being positioned opposite to one another and associated with the movable guide element.
| 5
|
RELATED APPLICATIONS
[0001] This application is a divisional application of U.S. application Ser. No. 11/856,521, filed Sep. 17, 2007, entitled “SOLAR ARRAY SUPPORT METHODS AND SYSTEMS” which is a continuation of U.S. application Ser. No. 10/606,204, filed Jun. 25, 2003, now U.S. Pat. No. 7,285,719, issued Oct. 23, 2007, entitled “SOLAR ARRAY SUPPORT METHODS AND SYSTEMS” which claims priority to provisional application Ser. No. 60/459,711, filed Apr. 2, 2003, entitled “SOLAR SCULPTURE” ENERGY AND UTILITY ARRAY, which is incorporated herein by reference.
FIELD
[0002] The present invention is related to the field of solar energy capture.
BACKGROUND
[0003] Present systems for supporting solar panels tend to be bulky and expensive. Given the size and weight of such systems, implementation of solar panel arrays in remote locations is difficult and expensive. When large equipment is required, installation of a solar panel array in an environmentally sensitive area without significant impact on surrounding habitat becomes very difficult. Typically, such support systems do not allow for secondary uses of the solar panel arrays.
SUMMARY
[0004] The present invention, in an illustrative embodiment, includes a system for supporting a solar panel array. The system includes two pairs of vertical columns, where each pair includes a tall column and a short column. The pairs are placed a distance apart, and a first support cable is secured between the short columns and a second support cable is secured between the tall columns. A guy wire or other anchoring devices may be attached to the columns to provide lateral support to the columns against the tension created by suspending the support cables between the spaced columns. The system further includes a solar panel receiver adapted to be secured to the two support cables. The solar panel receiver may be adapted to receive any type of solar panel or several panels. The receiver may include a maintenance catwalk or other access providing design element.
[0005] In another illustrative embodiment, the present invention includes a system for providing both shelter and electricity. The system may again include columns, support cables, and one or more solar panel receivers as in the illustrative solar panel array support system noted above.
[0006] The system further includes a number of solar panels secured to or received by the solar panel receiver. The columns may be sized to allow an activity to occur beneath the solar panel receivers. For example, if the desired activity is that of providing a shaded parking lot, the columns may have a height allowing vehicles to be parked beneath the solar panel receivers, and the columns may be spaced apart to create a sheltered area sized to correspond to the desired area of the parking lot.
[0007] In yet another illustrative embodiment, the present invention includes a system for supporting a solar panel array, the system comprising four anchor points, with a first support cable suspended between a first pair of anchor points, and a second support cable suspended between a second pair of anchor points. The system further includes a solar panel receiver adapted to be supported by the first and second support cables, the solar panel receiver also adapted to receive one or more solar panels.
[0008] In a further embodiment, the present invention includes methods of supporting a solar panel array. The methods include the step of using cables to support solar panel receivers adapted to receive one or more solar panels. In yet another embodiment, the present invention includes a method of creating a sheltered space which makes use of a solar panel array that creates electricity, where the method also includes using the electricity to cool an area beneath the array.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a perspective view of a solar panel array supported in accordance to an illustrative embodiment;
[0010] FIG. 2 is a longitudinal section view of a solar panel array supported in accordance to an illustrative embodiment;
[0011] FIG. 3 is a horizontal section view of a solar panel array supported in accordance to an illustrative embodiment;
[0012] FIG. 4 is a perspective rear view of an illustrative solar panel array;
[0013] FIG. 5 is a perspective side view of an illustrative solar panel array;
[0014] FIG. 6 is a rear perspective view of an illustrative pod showing the use of several struts and cords to create a rigid member;
[0015] FIG. 7 is a section view of an illustrative pod including several optional features;
[0016] FIG. 8 is a front perspective view of several solar panel receivers linked together;
[0017] FIG. 9 is a front elevation view of several solar panel receivers linked together;
[0018] FIG. 10 is a front and side perspective view of an illustrative solar panel array including a center support member;
[0019] FIG. 11 is a section view showing an illustrative solar panel array including a center support member;
[0020] FIG. 12 is a front elevation view of an illustrative solar panel array suspended across a valley;
[0021] FIG. 13 is an overhead plan view of an illustrative solar panel array suspended across a valley.
DETAILED DESCRIPTION
[0022] The following detailed description should be read with reference to the drawings. The drawings, which are not necessarily to scale, depict illustrative embodiments and are not intended to limit the scope of the invention.
[0023] FIG. 1 is a perspective view of a solar panel array supported in accordance with an illustrative embodiment. A solar panel array 10 is illustrated as including a number of solar panel receivers 12 . Pairs of short columns 14 a , 14 b and tall columns 16 a , 16 b are aligned with one another. The pairs of columns 14 a , 16 a and 14 b , 16 b may also be connected by a stability cable 18 that runs along the edges of the array 10 . The solar panel receivers 12 are held above a surface 20 at a height 22 defined by the columns 14 a , 14 b , 16 a , 16 b. A first cable 24 is suspended between the short columns 14 a , 14 b , and a second cable 26 is suspended between the tall columns 16 a , 16 b . The solar panel receivers 12 are designed to be supported by the cables 24 , 26 , so that the overall design is a lightweight, flexible and strong solar panel array 10 that leaves plenty of usable, sheltered space below. Anchor lines 28 and anchors 30 may be used to provide further support and to enable the use of lightweight columns 14 a , 14 b , 16 a , 16 b.
[0024] The surface 20 may be, for example, a generally flat area of ground, a picnic area in a park, a parking lot, or a playground. The height 22 may be chosen to allow for a desired activity to occur beneath the array 10 . For example, if a parking lot is beneath the array 10 , the height 22 may be sufficient to allow typical cars and light trucks to be parked underneath the array 10 , or the height may be higher to allow commercial trucks to be parked beneath the array 10 . If a playground is beneath the array 10 , the array 10 may have a height 22 chosen to allow installation of desired playground equipment.
[0025] Any suitable material and/or structure may be used for the columns 14 a , 14 b , 16 a , 16 b including, for example, concrete or metal, or a simple pole or a more complicated trussed column. In some embodiments a footing may be placed beneath the base of each of the columns 14 a , 14 b , 16 a , 16 b to provide stability on relatively soft ground. The cables 18 , 24 , 26 and anchor lines 28 may be made of any material and design as well including, for example, metals, composites, and/or polymeric fibers. In one embodiment the primary material used in the columns 14 a , 14 b , 16 a , 16 b , the cables 24 , 26 and the anchor lines 28 is steel. Because the primary support technology for the array 10 is the cables 24 , 26 under tension, the design is both visually and literally lightweight.
[0026] While FIG. 1 illustrates an embodiment wherein the columns 14 a , 14 b , 16 a , 16 b are either “short” or “tall”, in other embodiments the columns may all be of the same height. No particular angle of elevation is required by the present invention, however, it is contemplated that, depending upon the latitude, time of year, and perhaps other factors, certain angles may be more effective in capturing incident sunlight.
[0027] FIG. 2 is a longitudinal section view of a solar panel array supported in accordance with an illustrative embodiment. The array 10 illustrates the relative spacing of rows of the array 10 , and helps to show how the stability cable 18 connects the columns 14 , 16 of the array 10 . The stability cable 18 may be coupled to an anchor member as well, though this is not shown in FIG. 2 . It can be seen that the relative heights of the columns 14 , 16 help to define the angle that the solar panel receivers 12 have with respect to the incident sunlight. In some embodiments, the columns 14 , 16 or the solar panel receivers 12 may include a mechanism allowing for adjustment of the angle of the solar panel receivers 12 . To do so, for example, the length of the columns 14 , 16 may be adjusted, or the solar panel receivers 12 may include a mechanism for changing the angle of individual panels or entire receivers 12 . For example, with the changing of seasons, the height of the sun in the sky may vary sufficiently to affect the efficiency of the solar panel receivers 12 , and so it may be desirable to vary the angle of the receivers 12 . Also, as the sun moves during the day it may be desirable to change the angle of the receivers 12 to improve light reception.
[0028] FIG. 3 is a horizontal section view of a solar panel array supported in accordance with an illustrative embodiment. As illustrated, the array 10 is supported by short columns 14 a , 14 b , tall columns 16 a , 16 b , and cables 24 , 26 . Anchor lines 28 and anchors 30 are provided to improve stability and allow the use of lightweight columns 14 a , 14 b , 16 a , 16 b . The solar panel receivers 12 are illustrated as pairs of individual units 32 having gaps 34 between each unit 32 . The gaps 34 allow for air movement, reducing the amount of wind resistance of the array 10 . The gaps 34 also allow for relative movement of the units 32 since the cables 24 , 26 are somewhat flexible.
[0029] FIG. 4 is a perspective rear view of an illustrative solar panel array. It can be seen that the stability cables 18 are coupled in various configurations along the length of the array 10 , linking the short columns 14 and tall columns 16 to create a linked structure. The array 10 also includes various anchor cables 28 and anchor points 30 , including at the end of the array 10 that may help anchor the stability cables 18 .
[0030] FIG. 5 is a perspective side view of an illustrative solar panel array 10 which is similar to that shown in FIGS. 1-4 . It can be appreciated from the several views of FIGS. 1-5 that the illustrative array 10 provides a readily usable shelter that is amenable to a variety of activities.
[0031] FIGS. 6 and 7 illustrate a pod which may be used as a solar panel receiver. The “pods” illustrated herein are intended to provide an example of a solar panel receiver that may be used with the present invention. The solar panel receiver may, of course, have a variety of other structures to perform its function of holding one or more solar panels while being adapted to couple to support cables as illustrated herein.
[0032] FIG. 6 is a rear perspective view of an illustrative pod showing the use of several struts and cords to create a rigid member. The pod 40 is shown with several solar panels 42 which may be, for example, photovoltaic panels. A maintenance walkway 44 is included as an optional feature of the pod 40 . Several curved struts 46 extend vertically along the back of the pod 40 , with several horizontal struts 48 coupled by moment connections to the curved struts 46 . By using moment connections, the overall structure becomes a rigid yet lightweight frame for receiving the solar panels 42 . A center strut 50 extends out of the back of the pod 40 , and is connected to a truss cable 52 which provides another lightweight yet highly supportive aspect of the structure. The center strut 50 and truss cable 52 allow a lightweight curved strut 46 to be used, lending support to the center of the curved strut 46 .
[0033] In another embodiment, rather than creating electricity with photovoltaic panels, the present invention may also be used to support solar panels that collect solar thermal energy. The solar thermal collectors could be mounted on the solar panel receivers illustrated herein, and thermal energy could be collected by the use of a heat transfer medium pumped through flexible tubing. In one such embodiment, glycol may be used as a mobile heat transfer medium, though any suitable material may be used.
[0034] FIG. 7 is a section view of an illustrative pod including several optional features. The pod 40 is shown with solar panels 42 in place. The optional maintenance walkway 44 is again shown on the lower portion of the curved member 46 . The center strut 50 and truss cable 52 again provide support to the curved member 46 . The pod 40 may include, for example, a mister 54 that can be used to provide evaporative cooling to the sheltered area beneath a solar array using the pod 40 . The pod 40 may also include a light 56 or security camera, for example. In one embodiment, a solar array may be used to provide a parking shelter, with the solar array storing electricity during the day using, for example, fuel cells or batteries, and then discharging the stored electricity by lighting the shelter created by the solar array during the evening.
[0035] Two cable receivers 58 , 60 are also illustrated. While shown in the form of a simple opening that a cable may pass through, the cable receivers 58 , 60 may take on a number of other forms. For example, the cable receivers 58 , 60 may include a mechanism for releasably locking onto a cable. It can be appreciated from FIGS. 6 and 7 that the illustrative pod 40 is designed so that rain is readily directed off of the solar panels, as the water will run down the curve of the pod 40 . In other embodiments, the pod 40 may be more or less flat, rather than having the curvature shown, or may have a different curvature than that shown.
[0036] FIG. 8 is a perspective front view of several solar panel receivers linked together. A first solar panel receiver 70 , a second solar panel receiver 72 , and a third solar panel receiver 74 are supported by an upper support cable 76 and a lower support cable 78 . An optional maintenance walkway 80 is illustrated as well. Also included is a flexible electric cable 82 that allows for transmission of electrical power from each of the solar panel receivers 70 , 72 , 74 when solar energy is captured. The flexible electric cable 82 may also serve to distribute power to devices such as security cameras or lighting that may be provided beneath the solar panel receivers 70 , 72 , 74 .
[0037] FIG. 9 is a front elevation view of several solar panel receivers linked together. Again, the solar panel receivers 70 , 72 , 74 are shown supported by an upper support cable 76 and a lower support cable 78 , and include an optional maintenance walkway 80 . Two flexible electric cables 82 a , 82 b are illustrated in FIG. 9 , and may serve the same purposes as that noted above with respect to FIG. 8 . It is clearly shown in FIG. 9 that there is a gap 84 between the solar panel receivers 70 , 72 , 74 . The gap 84 allows the solar panel receivers 70 , 72 , 74 to move independently, rendering the overall array less rigid and more likely to withstand high winds. The gap 84 also prevents neighboring solar panel receivers (i.e. 70 and 72 or 74 and 74 ) from damaging one another in windy conditions.
[0038] Depending on the desired output of the array, the flexible electric cables 82 a , 82 b may be coupled to a substation for gathering produced power and providing an output. For example, the electricity gathered is inherently direct current power, an array as illustrated herein may be easily used to charge batteries or fuel cells. The power may also be used with an electrolyzer to produce hydrogen and oxygen, with the hydrogen available for use as a fuel.
[0039] FIG. 10 is a perspective front and side view of an illustrative solar panel array including a center support member. The illustrative array 100 includes a number of alternating short columns 102 and tall columns 104 , with support cables 106 , 108 suspended from the columns 102 , 104 . Anchor lines 110 and anchors 112 provide additional support, and the array 100 supports a number of solar panel receivers 114 . The further addition in FIG. 10 is the inclusion of a center support 116 , which allows for a longer span to be covered between the outer columns 102 , 104 , reducing the need to place additional anchors 112 . Further, because the center support 116 does not have to provide stability against lateral movement, and only needs to provide vertical support, the center support 116 may be of an even lighter weight construction than the outer columns 102 , 104 .
[0040] FIG. 11 is a section view showing an illustrative solar panel array including a center support member. Again, the array 100 is supported by the use of a short column 102 , a tall column 104 , a lower support cable 106 and an upper support cable 108 . The array 100 is stabilized in part by the use of anchor lines 110 and anchors 112 , and a number of solar panel receivers 114 are supported. The center column 116 provides a central support, but is not required to add to the lateral stability of the array 100 , because there are portions of the array pulling equally on both sides of the center column 116 .
[0041] FIG. 12 is a front elevation view of an illustrative solar panel array suspended across a valley. An array 120 is suspended across a valley 122 by the use of four anchors 124 that enable two support cables 126 , 128 to be suspended across the valley 122 . A number of solar panel receivers 130 are supported by the support cables 126 , 128 . By suspending the array 120 across the valley 122 , a desired height 132 above the valley floor can be achieved by the array. The height 132 may be sufficient to allow wildlife to pass below.
[0042] A number of potential environmental benefits of this type of structure can be identified, including that the structure provides a quiet and safe energy production array, the structure provides shade and/or shelter, and the structure can be installed without requiring a large amount of heavy machinery. The use of an array over eroding ground may encourage foliage growth in highly exposed locations, slowing erosion.
[0043] FIG. 13 is an overhead plan view of an illustrative solar panel array suspended across a valley. It can be seen that the array 120 is designed to match the shape of the valley 122 . In particular, the array 120 includes a number of individual lines of solar panel receivers 130 . By varying the number of solar panel receivers 130 suspended by each pair of support cables, a relatively short line 134 can match a relatively narrow place in the valley 122 , while longer lines 136 , 138 span a wider portion of the valley 122 .
[0044] Those skilled in the art will recognize that the present invention may be manifested in a variety of forms other than the specific embodiments described and contemplated herein.
[0045] Accordingly, departures in form and detail may be made without departing from the scope and spirit of the present invention as described in the appended claims.
|
Systems and methods for disposing and supporting a solar panel array are disclosed. In one embodiment, a system for supporting a solar panel array includes the use of support columns and cables suspended between the support columns, with the solar panels received by solar panel receivers that are adapted to couple to the cables. The solar panel array may then be used to provide power as well as shelter. Cooling, lighting, security, or other devices may be added to the solar panel array.
| 7
|
This invention relates to an adjustable door latch striker and especially to a striker adapted to be mounted to the jamb of a door and automatically adjustable relative to a door mounted latch upon the closing of the door.
BACKGROUND OF THE INVENTION
It is known in the art to provide elongated mounting holes on a jamb mounted striker to allow it to be adjusted and aligned relative to a door mounted latch. The striker is first loosely mounted by the elongated holes and roughly aligned with the door latch. The door is then closed partially to check the alignment, the striker is realigned and tested again in a series of successive approximations before finally secured. It is necessary to adjust the striker assembly in both a fore and aft direction relative to the vehicle and hinge axis of the door and in a direction normal to the fore and aft direction or transverse of the vehicle to obtain alignment of the striker and latch.
It is known to obtain the fore and aft adjustment of the striker through the use of a manually rotatable threaded member interposed between a mounting member mounted to the door jamb and a member supporting the striker. This is the subject of a pending application Ser. No. 334,786, now U.S. Pat. No. 4,451,071 John E. Iafret et al, filed Dec. 28, 1981, and assigned to the assignee of the present application and to TRW, Inc.
SUMMARY OF THE INVENTION
The striker of the present invention includes such fore and aft adjustment and also automatic adjustment in a direction normal to the fore and aft adjustment, thus providing complete adjustability and alignability.
The embodiment disclosed is for use with a glove box door movable about a hinge axis relative to a door jamb. The striker includes a mounting member fixed directly to the door jamb; a body member which includes a striker element adapted to be engaged by the door mounted latch on closure of the door to retain the door in closed position; and an intermediate track member which mounts the body member and is mounted to the mounting member. The track member is automatically adjustable relative to the mounting member and the body member is manually adjustable relative to the track member.
The striker and door latch include interacting camming surfaces which matingly engage as the door is closed to shift the body member and track member as a unit relative to the mounting member to thereby align the striker with the latch in a direction normal to the fore and aft direction.
It is, therefore, an object of the invention to provide a striker element which is automatically adjustable with respect to a door latch after the striker element has been mounted to the door jamb.
It is another object of the invention to provide such an adjustable striker element in which the striker is automatically alignable with the latch upon closing of the door. It is a further object of the invention to provide such an adjustable and alignable striker in which no further tightening or adjusting of the striker is necessary after its alignment. It is a still further object of the invention to provide such a striker which will automatically realign itself if misaligned after attachment.
These and other objects of the invention will become apparent from the following written description and drawings in which:
FIG. 1 is an exploded perspective view of a glove box door and adjustable latch striker according to this invention.
FIG. 2 is a front view of the striker.
FIG. 3 is a plan view of the striker from the perspective of line 3--3 of FIG. 2.
FIG. 4 is a sectional view of the striker from the perspective of line 4--4 of FIG. 2.
FIG. 5 is a view of a portion of FIG. 3 with an adjusting screw removed.
FIG. 6 is a bottom view of the striker from the perspective of line 6--6 of FIG. 2.
FIG. 7 is an enlarged view of a portion of FIG. 3.
FIG. 8 is a partial section along the line 8--8 of FIG. 3.
FIG. 9 is a partial section along the line 9--9 of FIG. 3, and
FIG. 10 is a perspective view of part of the striker.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring first to FIG. 1, a striker assembly designated generally 10 is shown situated within the peripheral door frame or jamb 12 of a glove box 14 in the instrument panel or dashboard 16 of a vehicle or the like. A cover or door 18 sized to cover the opening of jamb 12 is joined to the bottom edge of door jamb 12 by a hinge 20 and bolts 22. Hinge 20 mounts door 18 to jamb 12 for rotative movement about the axis of hinge 20 between open and closed positions. In closed position, door 18 engages resilient bumpers 24. In the open position, a cable assembly 26 attached at one end by bolt 28 to a side of door 18 and having a stop 30 at the other end received through hole 32 maintains door 18 in position. A latch mechanism designated generally 34 is held to door 18 by clip 36. Latch mechanism 34 has a pair of resilient ears 38 which slide together and apart and which engage a striker element of striker assembly 10 to hold door 18 in a closed position. Striker assembly 10 is mounted by bolts, one of which is shown at 40, to the top edge of door jamb 12 as will be described below.
Referring to FIGS. 2 and 3, striker assembly 10 is comprised of three basic members or sub-structures of molded plastic. The first sub-structure is a mounting member designated generally at 42, the second sub-structure is a housing or body member designated generally at 44 and the third sub-structure is an intermediate track member designated generally at 46 which joins mounting member 42 to body member 44. The interconnection and cooperation of these three sub-structures allows striker assembly 10 to be adjusted in two directions, both parallel to and perpendicular to the hinge axis of hinge 20, thus allowing complete adjustment and alignment after mounting member 42 has been affixed to the upper edge of door jamb 12.
Referring to FIG. 3, mounting member 42 has a generally rectangular shape with an integral upwardly extending peripheral strengthening rib 48 on the top face thereof which is inset along the front and rear to define parallel front and rear flanges 50 and 52. The bottom face of mounting member 42 is entirely flat except for a centrally located upwardly offset stepped recess 54, FIGS. 4 and 8, having a relatively deeper central portion 56 and covered by a centrally located boss 58 on the top face of mounting member 42. A flanged mounting hole 60 is located at each end of mounting member 42. Flange 52 is serrated by teeth 62.
Track member 46 has a generally rectangular base 64 with flat top and bottom faces, as best seen in FIG. 10. An upstanding flange 72 at the front edge of base 64 supports two spaced lateral tabs 74 which overlie front flange 50 of mounting member 42. Extending slightly inwardly from flange 72 beneath each tab 74 is a small bearing rib 76, best seen in FIG. 3, of generally triangular cross-section which bears against the edge of flange 50. Parallel to flange 72 are two coplanar resilient fingers 78 cantilevered from the rear edge of the top face of base 64 and separated by an intermediate, upstanding tab 80, as seen in FIG. 10. A shallow horizontal rib 82 on each finger 78 overlies rear flange 52, as best seen in FIG. 8. Each rib 82 has a downwardly sloped top surface 84. Beneath each rib 82 is a pair of serrations or teeth 86 which engage teeth 62 on the edge of flange 52 of mounting member 42, FIG. 7. A first track on track member 46 is thus defined by the top face of base 64, tabs 74 on flange 72, and ribs 82 on fingers 78.
Referring to FIG. 2, a wall 87 extends downwardly on each side of base 64. Each wall 87 includes a lateral tab 88 spaced from the bottom face of base 64, best seen in FIGS. 6 and 10 and defining a second track on track member 46.
Base 64 also includes a central slot 90, which, as seen in FIG. 5, has an enlarged center portion 92 and a pair of opposed bearing ribs 94. Slot 90 receives an adjusting screw 96 further described below. The walls 87 also include a pair of clearance notches 98 best seen in FIG. 6, to facilitate the mounting of mounting member 42, described below. A screw access hole 100 passes through flange 72, FIGS. 3, 4 and 5, and ribbed extensions 102, FIGS. 4 and 9, extend between flange 72 and base 64 for added strength. Tabs 74 and 88 and ribs 82 all are arranged so as not to project over or beyond one another, so it is possible to match them all with aligned access slots through base 64 to obviate the need for sliding mold cores.
Referring to FIG. 2, body member 44 has a general box shape with a horizontally extending top wall 112, a pair of downwardly extending side walls 114 and horizontally extending bottom wall 116. An extension 118 on one side wall 114 may serve as a base for the attachment of an electrical connector body, and a box shaped extension 120 on the other side wall 114 may serve as a housing for a trunk release switch, not shown. A cylindrical housing 122 interposed between top wall 112 and bottom wall 116 may contain a conventional glove box light switch 124, best seen in FIG. 4. Top wall 112 extends slightly beyond side walls 114 and the edges 126 thereof are received between base 64 and tabs 88. Molded into the center of the top surface of wall 112 is a rectangular recess 128 ribbed to matingly engage screw 96, with a colinear, shallow semi-cylindrical groove 130 extending beyond each end thereof, best visible in FIG. 5. A scale 132 is also molded into the top surface of wall 112 parallel and adjacent to recess 128, which serves in the adjustment process, described below. As best seen in FIG. 6, the front edge of each side wall 114 includes a rearwardly and inwardly sloped jaw 134 which together comprise the camming surfaces of the striker element. The greatest separation of jaws 134 is larger than the separation of the fully extended resilient ears 38 on latch member 34 and the smallest separation is slightly greater that the separation of the ears 38 when fully compressed.
The assembly of the three substructures may be understood by referring to FIGS. 2, 3, 8 and 9. Initially, track member 46 is assembled to body member 44 by sliding the side edges 126 under tabs 88 until track member 46 is located with slot 90 generally overlying recess 128. Next, the slotted head 136 of adjusting screw 96 is inserted within hole 100 and the screw dropped into recess 128, with the high lead thread 138 of the screw engaging the ribs of the recess 128. This engagement prevents relative sliding between members 46 and 44. Next, mounting member 42 is positioned generally centrally to track member 46 with rear flange 50 contained beneath tabs 74 and with the edge of flange 52 resting against the sloped top surfaces 84 of ribs 82. Downward pressure on member 42 forces the edge of flange 52 past sloped surfaces 84 and below ribs 82 as resilient fingers 78 bend outwardly to bring teeth 86 into mating engagement with teeth 62 to releasably secure members 42 and 44 with respect to each other. Adjusting screw 96 is captured between mounting member 42 and body member 44 and held flat by the engagement of stepped recess 54 with adjusting screw 96, best seen in FIG. 4. Deeper control portion 58 of recess 54 is, as seen in FIGS. 4 and 9, deeper and wider than thread 138 for a purpose described below.
To mount striker assembly 10, an initial rough fore and aft adjustment of track member 46 and mounting member 42 relative to body member 44 is done by turning adjusting screw 96 to move track member 46 to a predetermined position on scale 132. Next, mounting member 42 is mounted by bolts 40 extending through holes 60 into predrilled holes at the top edge of door jamb 12. Access to bolts 40 is available because of the clearance notches 98.
Next, door 18 is closed to engage resilient ears 38 of latch mechanism 34 with sloped jaws 134 on housing member 44. This forces members 44 and 46 to slide relative to member 42 as the teeth 86 on resilient fingers 78 ratchet relative to the teeth 62 of flange 52 as can be seen by the dash lines of FIG. 3. This movement is made possible by the clearance of thread 138, but screw 96 is still held flat, as seen in FIG. 4, to simultaneously maintain the fore and aft adjustment. The cross-car adjustment transverse of the vehicle parallel to the axis of hinge 20 is automatic, and requires no further tightening of screws or adjustment after the closing of the door. In addition, should housing member 44 become misaligned, it will automatically be realigned upon reclosing of door 18. If, after initial closing, it appears that door 18 still rattles or has not latched completely, then adjusting screw 96 may be turned fore and aft to adjust housing member 44 so that resilient ears 38 just engage the back of jaws 134 with door 18 compressing resilient bumpers 24. This fore and aft adjustment may be done at any time.
Additional features which may be incorporated with the striker assembly 10 are the provision of glove box illumination, by compression of button 124 upon door closing. Other buttons and electrical connections may be provided on extensions 118 and 120, as described, without affecting the adjustment.
Thus an adjustable latch striker has been provided in which various subassemblies are cooperatively connected to provide striker adjustment both fore and aft and laterally of the vehicle.
|
An adjustable striker assembly includes a mounting member on a door frame and a track member mounted thereto for sliding movement in a direction parallel to the door hinge. Cooperating resilient toothed fingers and teeth on the mounting member and track member releasably maintain them in any adjusted position. A body member, slidable relative to the track member and mounting member, includes a striker element engageable by a door latch. During door closing, the latch-striker engagement ratchets the body member and track member relative to the mounting member to automatically correct any misalignment. An adjusting screw between the mounting member and body member is adjustable to adjust the body member and striker element relative to the track member.
| 4
|
This is a continuation application of U.S. application Ser. No. 09/363,017 filed Jul. 29, 1999, now U.S. Pat. No. 6,116,453, which is a continuation of Ser. No. 08/793,751 filed Jun. 11, 1997, now U.S. Pat. No. 5,964,367, which is a 371 of application filed Sep. 12, 1995 as the National Phase of PCT/EP95/03586, now U.S. Pat. No. 5,964,367, which is a continuation-in-part of U.S. application Ser. No. 08/283,695 filed Aug. 1, 1994, now U.S. Pat. No. 5,593,060, which is a continuation application of U.S. application Ser. No. 08/049,722, filed Apr. 20, 1993, now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to a cylindrical, blow-molded lidded barrel (wide-mouthed drum) with a barrel lid and tension-ring closure, in which in the closed position, the tension ring, which is U-shaped in cross section, engages with its upper leg over the outside upper edge of the lid and engages with its lower leg under an outside edge of the barrel that runs basically horizontally or slightly obliquely downward in the opening area of the body of the barrel.
Such a lidded barrel is known from, e.g., DE-B-41 08 606. In the case of this barrel, however, the tension-ring closure is arranged some distance below the upper edge of the lid or the opening of the barrel, so that handling such a filled, e.g., 220-liter lidded barrel with a shipping weight of about 230 kg is possible only using special barrel-gripping tools. This type of a lidded barrel was developed by Mauser in 1975 and distributed worldwide under the designation “standard lidded barrel”; it is well-suited for handling solid, particulate or pasty contents, but such a barrel is not readily suited for use with liquids.
In the case of lidded barrels, the sealing action of the barrel lid on the barrel mouth is produced by bringing about axial prestressing on the lid seal via the tension ring leg bevels at the upper edge of the lid and at the outer border of the barrel body (or indentation) as the tension ring is clamped or closed.
On lidded barrels that are approved for use in, e.g., the chemical industry, certain requirements with respect to their storage and transport safety are set; compliance with these requirements is tested and examined in special acceptance tests (e.g., dropping on its side, jacket dropping, diagonal dropping on the edge of the lid, static internal pressure test, i.a.). In the case of known existing plastic lidded barrels, even when barrels are dropped from heights of about 1.20 m—e.g., from the bed of a truck—leaks occur, especially in the case of liquids, or complete detachment of the barrel lid can even occur.
The drawbacks of previously known lidded barrels consist of, especially,
a) when there is axial internal pressure on the barrel lid (surge pressure when a barrel filled with water is dropped on its jacket or when there is hydraulic internal pressure in a closed barrel),
b) when a closed barrel that is filled with water slams flat against a side wall (jacket dropping), and
c) when a closed barrel that is filled with water drops diagonally onto the edge of the lid, various reactions occur:
the barrel lid is pressed axially outward, the tension ring is pulled axially outward, the tension ring (together with lid and barrel mouth area) is flattened at the central impact point, the tension ring is heavily buckled laterally at the impact point and its U-shape is flared at both buckling points, the lid edge tries to slide out from under the upper tension ring leg, prestressing on the seal is reduced and the locking system begins leaking.
The stresses that occur with the deformations must be absorbed in each case by the U-shaped tension ring. In this connection, the legs are pressed outward (flared) in the buckling areas. If the stress on the legs is too high, it leads to permanent deformations, prestressing on the seal is reduced at those points, and significant flaring results in leaks or leaking of the barrel.
An attempt is thus to be made to reduce the deformation of the tension ring, especially the flaring in the U-area, by structural measures, especially in the barrel mouth area, at the barrel lid and/or tension ring, while at the same time continuing to ensure good handling, i.e., easy closing of the tension ring.
SUMMARY OF THE INVENTION
The object of this invention is to indicate a lidded barrel made of plastic with a barrel lid and tension-ring closure which, owing to the special way in which the individual components are matched to one another, makes it possible to use the same barrel-gripping tool (parrot's beak) or which, in the filled state, can be manipulated with the same barrel-gripping tool, as usually used universally for modern plastic L-ring bung barrels or normal steel-bung barrels. In this case, the lidded barrel is to be especially suitable for using liquids, i.e., it remains liquidtight even when it falls or is dropped from considerable heights.
This object is achieved according to the invention in that
directly behind the outer lid edge, which is overlapped by the upper leg of the tension-ring closure and which is shaped in cross section like a downward-facing U, in which the lid seal is inserted or foamed-in, the barrel lid has an essentially V-shaped engaging groove which has a flat groove floor and which is drawn in peripherally downward into the barrel body, between a reduced-diameter central lid disk and the lid edge, the inside boundary of the engaging groove is formed by a ring part which slopes conically upward and to which is connected the flat lid disk with at least one bunghole that is recessed laterally in a bung housing, the lower leg of the tension-spring closure engages tightly below (about 15 mm) the upper barrel edge in an indentation in the upper barrel wall, whose upper boundary represents the essentially horizontal barrel edge or slightly oblique attachment surface for the tension ring and whose outline, as it moves downward toward the transition to the fully cylindrical part of the barrel wall, is essentially designed to be increasingly flat-conical, and the transition from the conical area to the fully cylindrical part of the barrel body is arranged at a distance of 80 mm to 140 mm, preferably about 120 mm, from the upper front edge of the barrel mouth edge, and the upper barrel edge of the barrel mouth is designed solidly as an outer support for a lid seal and has a width (thickness) of approximately double the wall thickness of the barrel body.
This special design of the upper outer area of the lidded barrel according to the invention makes it possible, on the one hand, to use or apply barrel-gripping tools that are generally employed for bung barrels; on the other hand, the lidded barrel according to the invention also has considerably improved liquid sealing properties in the case where it is filled with liquid, e.g., in the case where barrels are dropped from considerable heights (about 1.8 m) or in the case of the previously described acceptance tests.
In a variant embodiment of the invention, it is provided that the conical outline of the barrel wall inside the indentation below the horizontal attachment surface for the lower leg of the tension-ring closure be made at an acute angle of between 15° and 30°, preferably about 18° to 20°, at the transition in the fully cylindrical part of the barrel body to the longitudinal axis of the barrel. As a result, the barrel-gripping device can, as usual, be brought in first against the cylindrical barrel body in the usual way and then raised upward, passing into the indentation until the lower barrel-gripping claw strikes the lower leg of the tension ring which rests on the horizontal attachment surface of the edge of the barrel and the upper barrel-gripping claw automatically pivots inward and tilts owing to the resistance that, is produced, and the lidded barrel is tightly grasped and can be transported.
To ensure a secure fit of the lower tension-ring leg as well as the barrel-gripping claw that is applied thereto, it is provided according to the invention that the radial depth of the indentation, measured by the extension line of the fully cylindrical part of the barrel body, be between 12 mm and 25 mm, preferably about 17 mm. In this case, the slightly oblique barrel edge, which is used as attachment surface for the lower leg of the tension ring and which simultaneously represents the upper boundary of the indentation, is made at a distance of about 10 to 20 mm, preferably about 15 mm, from the upper barrel edge in the outside wall of the barrel body. A solid outer support for the tension ring and for the barrel-gripping device that is put on is further achieved in that the solid barrel mouth edge, with its upward-pointing smooth area that has the shape of a partial circle and is used as a sealing surface for the lid seal, is produced during the blow-molding process by squeezing the thermoplastically deformable plastic of the barrel wall with the aid of a mold slide, and outside on the solid barrel edge, a peripherally smaller flange edge with a radial extension of about 3 to 5 mm is formed, thus increasing the width of the horizontal support surface for the lower leg of the tension ring.
Since the lidded barrel according to the invention in its light design for a capacity of 35 US gallons has a barrel (body) weight of only about 5.2 kg and for a capacity of 55 US gallons has a barrel (body) weight of only about 8.2 kg, as well as an opening width of the upper barrel mouth that is about 15% larger than a usual bulgy lidded barrel of the above-mentioned type, it is very well suited for granulate-like or pasty contents, for which mainly fiber drums are now used.
In the USA, fiber drums, optionally with liners, are also widely used for liquids. Because of its excellent gas and liquid sealing properties as well as the ability to drain residue almost completely (with the lid on) via the residue-drain lid bung, the lightweight lidded barrel according to the invention is also highly suitable for using liquids instead of the previously usual fiber drums.
Other advantages of the lidded barrel according to the invention consist in the fact that it has dimensions that are identical to the greatest extent possible to those of a corresponding plastic L-ring bung barrel or steel bung barrel, and it can thus be handled with the same barrel-gripping tools (parrot's beak). These lidded barrels can also be handled on pallets together with bung barrels without the losses of space due to big-bellied lidded barrels and differing heights that otherwise usually occur. The filling of the lidded barrels is done via the 2-inch bung using the same filling systems as for bung barrels since the dimensions and arrangements of the lid bung correspond exactly to the relevant dimensions of the bung barrel.
Reconditioning of the lidded barrels for reuse or multiple use is considerably simpler and more efficient in comparison with bung barrels, and also later disposal causes no problems whatsoever since the plastic of the barrel body and barrel lid as well as the tension ring, whether it is made of steel or of plastic, can be recycled without residue.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention as well as other advantageous embodiment variants are explained in greater detail and described below based on the embodiments diagrammatically presented in the drawings. Here:
FIG. 1 shows a lidded barrel with a base ring according to the invention, in side view,
FIG. 2 shows another embodiment of the lidded barrel according to the invention,
FIG. 3 shows a configuration comparison between a usual bulgy lidded barrel and a cylindrical lidded barrel according to the invention,
FIG. 4 shows a sectional view through the left edge area of a lidded barrel according to the invention (US version),
FIG. 5 shows a sectional view through the left upper edge area of a lidded barrel according to the invention,
FIG. 6 shows a sectional view through the right upper edge area of a lidded barrel with barrel-gripping claws that are put on according to the invention,
FIG. 6 a shows a profile of the upper barrel edge seen in FIG. 6 and represents the delineations of various portions of the upper barrel edge,
FIG. 7 shows an enlarged sectional view through the right upper edge area of a lidded barrel according to the invention,
FIG. 8 shows another lidded barrel (without base ring) according to the invention in side view with a partial sectional view (European version),
FIG. 9 shows an enlarged view of the upper barrel area of the lidded barrel according to FIG. 8 ,
FIG. 10 shows an upper left barrel area in a partial sectional view,
FIG. 11 shows the upper left barrel area according to FIG. 10 in a complete sectional view,
FIG. 12 shows an upper right barrel area in a sectional view,
FIG. 13 shows an upper left barrel area in a sectional view of another embodiment (US version) and
FIG. 14 shows an upper left barrel area in a sectional view of another embodiment (US version).
DETAILED DESCRIPTION OF THE INVENTION
In FIG. 1 , a lidded barrel with a capacity of 55 US gallons here, according to the invention, which is provided with a barrel lid 12 put on and a tension-ring closure 14 in place, is referred to by reference number 10 . About 80% of barrel body 20 is designed as fully cylindrical, while about 10% respectively of the barrel height upward toward barrel opening edge 28 and downward toward barrel bottom 34 is drawn in with a slight conical taper. In fully cylindrical part 26 of barrel body 20 , two comparatively broad rounded barrel body roller cages 38 are arranged at one-third and two-thirds of the barrel height. In the conically tapered transition area between fully cylindrical part 26 of barrel body 20 and flat barrel bottom 34 , a solid bottom roller cage 36 that ends flush with barrel bottom 34 is provided. Bottom roller cage 36 has a trapezoidal cross section below with a thinner bridge connection to barrel body 20 and an outside diameter that is almost identical to that of tension ring 14 , which is put on in the closed state and imparts to lidded barrel 10 excellent stability, especially when several barrels are stacked on top of one another, and a high degree of stiffness or resistance to indentation or crushing (buckling work in plastic) of the lower barrel edge when a filled lidded barrel is rolled at an oblique angle.
The barrel with a capacity of 55 US gallons has a maximum diameter of about 578 mm and a height of about 898 mm (height/diameter ratio about 1.55). A first modified barrel design with identical diameter dimensions, but a somewhat smaller volume of 52.5 US gallons, has a height/diameter ratio of about 1.49, and the barrel height with a tension ring mounted is about 860 mm. This barrel thus is of precisely the same height as the usual lidded barrels that are found in the USA, and it can therefore be handled on a pallet with the latter. A second modified barrel design with identical diameter dimensions, but a comparatively smaller volume of only 36 US gallons, has a height/diameter ratio of only 1.06, and the barrel height with a tension ring mounted is about 610 mm. This barrel (the so-called “stubby drum”) appears as high as it is wide and is provided especially for granulate-like or powder-like products, such as pigments, and to remove them from the barrel, the pigments are “scooped out” by hand with a scoop. Owing to the small height (about one arm's length) of the barrel, it is also possible to remove residue from the lower barrel area without having to bend double to reach into the barrel or to inhale dust particles.
In FIG. 2 , a slender lidded barrel 10 with a volume of 35 US gallons is depicted as a preferred embodiment. This lidded barrel has a height of about 860 mm and a maximum diameter of barrel body roller cages 38 of about 475 mm. The height/diameter ratio of this barrel is about 1.82. A modified barrel design with the identical diameter dimensions, but a smaller volume of 30 US gallons has, on the other hand, a height-diameter ratio of about 1.57, and the barrel height with a tension ring mounted is about 745 mm. The two barrel types of identical diameter (according to FIGS. 1 and 2 ) with only different heights can be produced in an advantageous way in a single alternating blow mold. To this end, only a suitable extension ring piece in the blow mold needs to be used (taller barrel) or removed (shorter barrel).
The particular feature of this embodiment variant thus consists in the fact that it has almost the same dimensions as the fiber drums that are usually used today in the USA and can be manipulated and handled with the same barrel-gripping tools as the usual fiber drums or bung barrels. In addition, the novel lidded barrels in a light design can be produced more economically than comparable fiber drums and subsequently cause no disposal problems whatsoever since they are completely recyclable. The tension ring can be a usual sheet-steel closure ring, but it can also be made entirely of plastic.
When using the lidded barrel according to the invention to hold liquids, barrel lid 12 is equipped with at least one bung opening, preferably with two lateral bung openings that can be sealed and are arranged on opposite sides from one another; larger bung 42 has a 2-inch (about 50.8 mm) opening, and smaller bung 44 has a ¾-inch (about 19.1 mm) opening. From FIG. 2 , it is also clear that the conical outline of the barrel wall inside indentation 22 below horizontal attachment surface 18 for the lower leg of tension-ring closure 14 is made at an acute angle a of between 15° and 30°, preferably about 18° to 20°, at transition 24 to fully cylindrical part 26 of barrel body 20 . This configuration ensures a high degree of resistance to stacking stresses.
In FIG. 3 , a previously commonly used bulgy standard lidded barrel or its barrel body 46 is drawn in the left half of the drawing in dotted configuration for comparison with barrel body 20 according to the invention. From this, the improved stability of the more slender lidded barrel according to the invention is clear. Furthermore, it is evident that in the case of the bulgy barrel body, the fully cylindrical part is only about one-third (⅓) of the entire height of the barrel body, while fully cylindrical part 26 in the case of the barrel body according to the invention constitutes more than three-fourths (¾) of the entire height of the barrel body. As an advantageous result, especially also due to sturdy bottom roller cage 36 , the barrels can be more easily handled on pallets, while simultaneously having improved stability and better rolling-off capability when the barrel is tilted.
In FIG. 4 , the left edge area of a lidded barrel 12 according to the invention is shown in cross-sectional view. A lid seal 30 is inserted or foamed-in into downward-facing U-shaped lid edge 16 . An approximately 25 mm deep engaging groove 32 is made between lid edge 16 and central flat lid disk 80 that is arranged almost flush at the same height. Engaging groove 32 has a flat groove floor 48 , which evenly extends radially inward at least 10 mm, and preferably about 15 mm. An obliquely conical ring part 52 rises from groove floor 48 as a connecting piece to upper flat lid disk 80 .
On the lower side of barrel lid 12 , two approximately 20 mm long (axial) ring flanges 54 , 56 that extend down below engaging groove 32 are made in the outside edge area. Ring flanges 54 , 56 are about 20 mm apart and are used to increase the stiffness of barrel lid 12 . Also visible is 2-inch bung 42 that is arranged in a sunken bung housing 50 . Of special importance is an intermediate piece or connecting piece 58 which is formed between U-shaped lid edge 16 and groove floor 48 and which, starting from lid edge 16 , is bent or angled inward. With barrel lid 12 put in place, this bent connecting piece 58 or outer axial ring piece 54 comes to rest with the inside wall of barrel body 20 opposite outer indentation 22 and increases the stacking capacity of the lid or lidded barrel because of the mutual support.
In FIG. 5 , a corresponding partial section through the left upper edge area of a barrel lid 12 according to the invention is shown, but laterally outside a bung or bung housing. Here, radial ribs 60 that rest on the inside against U-shaped lid edge 16 are arranged above angled connecting piece 58 . Radial ribs 60 are provided in large numbers with a small lateral spacing of about 5 mm to 10 mm.
Furthermore, in this embodiment of barrel lid 12 , a second upward-facing peripheral V-shaped groove 62 with a preferably rounded groove floor in the outside area of flat lid disk 80 is provided facing radially inward behind engaging groove 32 . This groove 62 is interrupted only by the recessed bung housing and improves the elasticity of the lid against internal overpressure and the surge pressure that occurs when a barrel falls.
Further, FIG. 6 shows the upper right edge area of a lidded barrel according to the invention with barrel-gripping claws 64 , 66 applied. For the light barrel design, it is necessary that, in particular, the barrel lid and the barrel opening area be matched exactly to one another. Part of this is that, i.a., to ensure secure attachment of lower barrel-gripping claw 66 , the radial depth of indentation 22 , measured from the extension line of the fully cylindrical part of the barrel body, is between 12 mm and 25 mm, preferably about 17 mm. The width of the horizontal support surface for the lower leg of tension ring 14 or the attachment surface for barrel-gripping claw 66 is also increased by virtue of the fact that solid barrel opening edge 28 is produced during the blow-molding process by squeezing the thermoplastically deformable plastic of the barrel wall with the aid of a mold slide, so that a small peripheral flange edge 40 extending radially outward about 3 to 5 mm is formed on the outside at the bottom at barrel edge 28 .
As seen in FIG. 6 , the upper barrel edge includes a first wall portion 27 extending substantially radially outwardly from the barrel sidewall, and a second wall portion 29 having a lower section 31 adjacent the first wall portion 27 with at least an inner edge 27 a of the first wall portion 27 extending radially inwardly of the entire second wall portion 29 . The upper barrel edge 28 also includes an exterior rib 40 which projects radially outwardly beyond an outward extent of the first and second wall portions, the rib having both an upper surface and a lower surface and terminating in a free end surface connecting the two.
FIG. 6 a has the identical profile of the upper barrel edge 28 of FIG. 6 and presents the delineations of the first wall portion 27 , the second wall portion 29 and the exterior rib 40 . As depicted in FIG. 6 a , the second wall portion 29 constitutes that portion of the upper barrel edge 28 that is above an uppermost portion of the rib 40 . As also seen in FIG. 6 a , the first wall portion 27 constitutes that portion of the upper barrel edge 28 that is: (a) above a level of the radially innermost portion of the barrel's upper sidewall, (b) below the second wall portion 29 and (c) radially inward of the rib 40 to which the first wall portion 27 is connected.
In FIG. 6 , it is further evident that the area of solid barrel opening edge 28 that points upward with a height of about 8 mm upward has a smooth, partially circular cross section as a sealing surface for lid seal 30 . A special design of the mold slide in the blow mold ensures that this sealing surface of squeezed solid barrel opening edge 28 that points upward and is exactly opposite lid seal 30 remains free of folds and seams of the squeezed plastic. These folds and seams are shifted outward and are advantageously arranged in outer flange edge 40 , where they no longer pose a problem. To improve the engagement area of upper barrel-gripping claw 64 , a considerable number of radial ribs 60 can be provided above bent connecting piece 58 behind U-shaped lid edge 16 .
To illustrate important features according to the invention, FIG. 7 shows once more in detailed representation the upper right barrel area of a lidded barrel. Quite important structural features consist especially in the fact that:
Above on the lid edge, an approximately 6 mm to 12 mm, preferably 8 mm wide, slightly obliquely adapted support surface 84 (identified by arrow) is formed for the upper leg of tension ring closure 14 . Thus, when, for example, a barrel is dropped, the lid edge cannot move outward in the buckling areas under the tension ring, and the stress on the lid seal will not be relieved.
Because of flange edge 40 which projects or overhangs outward at the lower outside edge of the barrel body opening, an enlarged support surface 18 of at least 10 mm is provided for the lower slightly oblique leg of tension ring 14 . The support surface is (in the radial direction) preferably even 15 mm (arrow 86 ) wide. This is also advantageous for reliably gripping the barrel with the lower claw of the barrel-gripping tool (parrot's beak). Groove floor 48 of outer peripheral engaging groove 32 is arranged at the same height as or even a little below the lower leg of tension ring 14 . As a result, the upper claws of the barrel-gripping device engage far down into engaging groove 32 and reliably secure the lidded barrel.
The barrel body edge, which is overlapped by tension ring 14 , is basically designed as a T that projects upward with a horizontal arm 88 and a vertical arm 90 that is arranged approximately in the center and pointing upward, and the surface of vertical arm 90 that is pointing upward is rounded in the shape of a partial circle (radius 4.5 mm) and represents the sealing surface of the barrel body edge that comes into contact with lid seal 30 . A partial piece of horizontal arm 88 that points outward is represented by flange edge 40 , which projects radially outward. The partial piece of the horizontal arm that points inward connects to the barrel body wall that runs downward. The cut point or cut surface of the cut-off slug piece (waste piece from the blow-molding process) is located in the transition area from the partial piece that points inward to the barrel wall that runs downward. The cut edge can run perpendicular or, as represented, slightly obliquely downward and toward the inside. Directly below the cut edge, there is a contact area 92 of the barrel inner wall with the outside surface of the barrel lid or the extension of outer lid ring arm 54 . In contact area 92 is the narrowest diameter of the barrel body opening, which is about 2 to 4 mm smaller here than at the cut edge of the slug piece. When the cover is mounted, outer lid ring arm 54 passes into the barrel interior and radial centering and bracing of the lid on the inner wall of the barrel takes place in contact area 92 below the cut surface of the slug piece. If a number of barrel bodies are distorted in a slightly oval shape, e.g,. by shrinkage stresses, a centering adaptation is made in the barrel opening area, thus ensuring a uniform positioning and an exact fit of the sealing surface of upward-pointing vertical arm 90 to lid seal 30 . Such centering cannot be achieved with conventional barrel lids, which do not project part-way into the barrel interior and make contact there with the barrel inner wall. It is just this kind of centering that makes it possible to adapt the width of vertical arm 90 (8 mm wide, about 9 mm high) to the inner width (about 10 mm) of the downward-facing U-shaped lid edge precisely enough to ensure that, on the outside and inside of vertical arm 90 , exact lateral spacing gaps 96 , 98 (identified by arrows) 1 mm wide are left. This ensures that vertical arm 90 with the smooth, arched sealing surface always hits in the center on sealing ring 30 .
The lidded barrel according to the invention is further distinguished in that the maximum outside diameter of barrel lid 12 is equal in size to the outside diameter of flange edge 40 that projects radially outward (both connect flush to one another), and the distance between the face of the outer downward-facing leg and the downward-opening U-shaped lid edge for the upward-facing lateral face of flange edge 40 that projects radially outward at the barrel opening edge with a lid put on and with the tension ring closure closed is only about 1 mm. For this purpose, it is ensured that when the stack load is applied, lid seal 30 needs to give only by this 1 mm, and then the outer leg of the lid edge will come into contact with flange edge 40 that projects outside and will be supported on it in such a way that overstressing of seal 30 will be avoided.
Another lidded barrel according to the invention (European version) without a base ring and with a capacity of 220 liters is depicted in FIG. 8 , which with barrel lid 12 put on and tension ring closure 14 in place has a barrel weight of only about 8 kg. The plastic of the barrel body consists of high-molecular-weight polyethylene (HD-PE). In this embodiment the disk-shaped upper plate of barrel lid 12 projects over U-shaped lid edge 16 which is open downward or the upper leg of tension ring 14 that engages over the latter. The excess height is about two to five times the wall thickness or thickness of the barrel lid, preferably about 10 mm. This is used to improve long-term stacking properties owing to a defined inner pressure buildup. In a modified embodiment, the lidded barrel can be equipped at the bottom with a base ring or bottom roller cage, which then is aligned in a plane with the bottom or is flush with it.
FIG. 9 provides a better view of barrel lid 12 with two lateral bungs 42 , 44 that are recessed in bung cavities 50 , 50 ′. (Left) 2-inch bung 42 is provided for filling as well as for the removal of the contents by means of a suction pipe. Further, said bung 42 is designed as a residue-drain bung owing to the adjacent incline of the lid upper plate. Smaller ¾ inch bung 44 can be opened to vent the barrel during filling or removal processes.
As an additional, quite essential feature, it can be seen here that below V-shaped engaging groove 32 on the inside of barrel lid 12 , two peripheral ring lands 54 , 56 , which are spaced a certain distance apart, are made. Outer ring land 54 rests on the inner barrel wall. Ring lands 54 , 56 are spaced approximately 10 mm to 30 mm, preferably about 20 mm, apart and extend over a length of about 20 mm into the barrel in the axial direction. The particular feature of this embodiment variant of a lidded barrel now consists in the fact that it is has almost exactly the same dimensions as a suitably closed L-ring bung barrel, which is usual and in use at present in the chemical industry in Europe, so that the novel lidded barrel can be handled on pallets together with ordinary bung barrels and can be manipulated and handled with the same barrel-gripping tools as ordinary bung barrels. The novel lidded barrels in a light design can further be produced economically and later cause no disposal problems whatsoever since they are completely recyclable. Also, here, tension ring 14 can be an ordinary sheet-steel closure ring, but it can also be made entirely of plastic.
In FIG. 10 , barrel lid 12 is shown in a sectional view next to 2-inch bung 42 . On both sides of bung housing 50 , the upper plate of barrel lid 12 is designed tilted downward toward the lid edge. On the outside, incline 68 extends as far as the projection or the beginning of inner ring land 56 or as far as the inner flat edge of engaging groove 32 .
Thus, when the lidded barrel is tilted slightly when inverted (turned over), the very last drop of liquid will flow out to lowest point 78 at the upper edge of inner ring land 56 or at the outer edge of the 2-inch bung or will run out through the bunghole from the inside of the barrel.
In order also to make it possible for residual liquid to flow out from the outer lid area or from the space between two ring lands 54 and 56 , it is provided according to the invention that a bore 76 (or a wider crosswise opening) be introduced at least in inner ring land 56 directly in front of discharge bung 42 . It is also advantageous to provide a suitable bore in outer ring land 54 at the same spot to make it possible for residual liquid from the space between the inside barrel wall and outside ring land 54 . It is advisable to provide an inside-type indentation 74 , viewed from the inside, directly in front of bung 42 , into which bore 76 , which is in ring land 56 and which leads to the bunghole, empties. In engaging groove 32 , this inner outlet trough appears as a projection 72 that extends upward like a ridge obliquely to the bung.
As FIG. 11 shows, bores 76 run through ring lands 54 and 56 obliquely to the bung and with a steeper inclination to the bung than incline 68 , so that lowest point 78 is produced on the outer edge of the bunghole. This can be achieved so easily because flat groove floor 48 of engaging groove 32 is deeper than the bottom of bung housing 50 . Groove floor 48 is approximately one to two wall thicknesses (about 30 mm to 10 mm) of the barrel lid deeper than the bottom of the bung housing.
In FIG. 12 , the right edge area of a lidded barrel according to the invention is further shown in cross-section. As the other drawing figures also show, lid seal 30 is introduced into U-shaped lid edge 16 that is open downward. Engaging groove 32 , which is about 20 mm to 40 mm deep, is placed between lid edge 16 and the central flat lid disk, which is designed to be higher. Engaging groove 32 has flat groove floor 48 , which extends horizontally about 15 mm radially inward. From groove floor 48 , obliquely conical ring part 52 rises (except in the bung housing area) as a connecting piece to the upper flat lid disk.
On the lower side of barrel lid 12 , two ring flanges 54 , 56 , which are recessed about 20 mm (axially) in the barrel body, are made in the outside area. Also visible is the ¾-inch bung 44 arranged in recessed bung housing 50 ′. Basically, the residue-drain lid incline could also be placed here.
In FIG. 13 , another embodiment of a lidded barrel according to the invention (US version) is presented. In this connection, discharge bung 42 ′ in the embodiment usually found in the USA is designed with bung plug 70 which seals at the top at the bung connection piece—in contrast to the embodiment of the bung plug usually found in Europe, which comes to rest with its sealing ring and is sealed in the bung connection piece below the screw threading at a retracted conical sealing surface.
The last embodiment, depicted in FIG. 14 , is distinguished from the embodiment shown in FIG. 13 essentially in that the upper plate or central flat lid disk 80 of the barrel lid is designed flush with the lid edge or flush with the upper leg of the tension ring. In this case, consequently, incline 68 of the flattened lid area runs correspondingly flatter laterally beside the discharge bung.
For the light barrel design according to the invention, it is necessary that, in particular, the barrel lid and the barrel opening area be matched exactly to one another. The special design of upper barrel edge 28 is significant. Part of this is that, to ensure secure attachment of lower barrel-gripping claw 66 , the radial depth of indentation 22 , measured from the extension line of the fully cylindrical part of the barrel body, is between 12 mm and 25 mm, preferably about 17 mm. The width of the slightly oblique attachment surface for the lower leg of tension ring 14 or the attachment surface for barrel-gripping claw 66 is also increased by virtue of the fact that solid barrel opening edge 28 is produced during the blow-molding process by squeezing the thermoplastically deformable plastic of the barrel wall with the aid of a mold slide in such a way that a small peripheral flange edge 40 that extends radially outward about 5 mm is formed on the outside down at barrel edge 28 .
Barrel mouth edge 28 is designed as an inverted “L,” which forms an angle of about 70° to 85°, preferably about 76°, between its long leg (=barrel wall) that points downward and its basically horizontal short leg that points outward. The short leg that points outward is designed to be slightly obliquely conical on its lower side, i.e., it tapers outward. The oblique surface is used as attachment surface for the lower leg of the tension ring which, with the lid seal in the closed state, presses the lid on the upper barrel wall by means of the oblique attachment surface. The short “L”-leg is provided on its upper side with a bead-like projection, which has a smooth semicircular sealing surface above. This beadlike projection engages in the U-shaped lid edge and seals against the lid seal. The outer edge of the U-shaped lid edge that points downward ends almost flush with flange edge 40 of barrel opening edge 28 that points radially outward, so that the lid seal will not be overstressed even in the case of overstacking.
The semicircular area of solid barrel opening edge 28 that points upward has a height of at least 10 mm and forms the sealing surface for lid seal 30 . A special design of the mold slide in the blow mold ensures that the sealing surface of squeezed solid barrel mouth edge 28 that points upward remains free of folds and seams of the squeezed plastic.
To achieve the advantageous properties of the lidded barrel according to the invention, considerable numbers of details and subtleties that are matched to one another are important, which in combination with one another constitute the essence of this lidded barrel.
|
This invention relates to a cylindrical, blow-molded lidded barrel (wide-mouthed drum) with a barrel lid and tension-ring closure. Previously known lidded barrels have comparatively little ability to withstand falls and are therefore not well-suited for handling liquids. Owing to the special configuration of the barrel lid and the barrel mouth edges as well as by a special matching of the individual components to one another, the lidded barrel according to the invention can be manipulated in the filled state with the same barrel-gripping tool (parrot's beak), ans is universally employed and in industrial use for modern plastic L-ring bung barrels or normal steel bung barrels. By improving the strength of the lidded barrel when it is dropped, the barrel is also made especially well-suited for handling liquids since it remains liquidtight even when dumped or dropped from great heights.
| 1
|
BACKGROUND OF THE INVENTION
[0001] The present invention relates generally to outdoor enclosures for electronic components and, more particularly, to an outdoor enclosure for electronic components that uses passive heating and cooling to control the temperature of the enclosure.
[0002] When telecommunications equipment is deployed in outdoor locations, a cabinet or enclosure protects the electronics from weather and environmental contaminants. The reliability of electronic components decreases significantly if they are subjected to high temperature extremes, especially if the temperature swings or cycles are frequent. The temperature swings may be due to heat generated by the electronics (i.e., more heat is produced at peak times), natural temperature variations, and solar loading. To protect the electronics equipment, various methods are used to control the internal temperature of the electronics enclosure.
[0003] Ventilated cabinets are sometimes used to cool electronics equipment inside an enclosure or cabinet. Ventilated cabinets use natural or forced convection to draw ambient air through the cabinet to cool the equipment inside the cabinet. Ventilated cabinets are relatively inexpensive and require little maintenance. However, the electronics inside the ventilated cabinet are exposed to the air flow, which may contain environmental contaminants, such as moisture, nitrates, hydrocarbons, sulfur dioxide, nitrogen oxides, hydrogen sulfides, chlorine, ozone, salt, and the like.
[0004] Sealed cabinets provide an alternative to ventilated cabinets where environmental contamination is a concern. Sealed cabinets use heating and cooling systems to maintain the electronics in the cabinet within the desired temperature range without exposing the electronics to potentially harmful contaminants. The heating and cooling systems include fans, air conditioners, and heaters, which consume space in the cabinet and add considerably to the cost of the cabinet. Additionally, such components require periodic maintenance to maintain them in proper operating condition.
[0005] Passive cooling methods for cooling electronics enclosures are also known. Passive cooling relies on conduction and radiation to passively cool the electronics equipment inside an enclosure without fans, air conditioners, or heat exchangers. Passive cooling of electronics enclosures is less expensive than active cooling systems, reduces energy consumption, and minimizes noise. Additionally, because there are fewer components to fail, passive cooling systems are generally more reliable and robust than active cooling systems.
[0006] Passive cooling systems for electronics enclosures dissipate heat generated by the electronics through natural convection and radiation. However, if the enclosure is placed in direct sunlight, the solar load on the cabinet may be as many more times that of the heating load of the electronics. In order to dissipate heat generated by the solar load using passive methods, a phase change material (PCM) is typically used. Phase change materials are materials that change state (e.g., from solid to liquid and vice versa) as the temperature changes. The temperature at which the PCM changes state is referred to as the phase change temperature. As heat builds up in the enclosure, the PCM begins to change from solid to liquid when the temperature inside the enclosure reaches the phase change temperature. While the phase change is occurring, the PCM continues to absorb heat while the temperature remains the same. The temperature does not begin to increase again until the PCM has changed phase. The amount of heat, or energy, required to change the PCM from one phase to another is called the latent heat of the PCM. Conversely, when the solar load is removed and the temperature inside the enclosure begins to cool, the temperature of the PCM also reduces and it changes back to a solid state.
BRIEF SUMMARY OF THE INVENTION
[0007] The present invention relates generally to a passively-cooled electronics enclosure for use outdoors. The electronics enclosure comprises an electronics cabinet or housing, a mounting bracket for mounting the electronics housing to a support structure, and a heat absorption module. The electronics housing may be directly mounted to the mounting bracket or, alternatively, may be mounted to the heat absorption module which, in turn, mounts to the mounting bracket. Thus, the electronics housing may be used with or without the heat absorption module. When the electronics enclosure is deployed in a location where it is not exposed to direct sunlight, it may be used without a heat absorption module. Conversely, when the electronics enclosure is deployed in a location where it is subjected to solar loading, the heat absorption module may be used to passively cool the electronics housing.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] [0008]FIG. 1 is an exploded perspective view of the modular electronics enclosure of the present invention.
[0009] [0009]FIG. 2 is a perspective view of the modular electronics enclosure assembled without the heat absorption module.
[0010] [0010]FIG. 3 is a perspective view of the modular electronics enclosure assembled with the heat absorption module.
[0011] [0011]FIG. 4 is an exploded perspective view illustrating a second embodiment of the modular electronics enclosure of the present invention.
[0012] [0012]FIG. 5 is a partial perspective view of the heat absorption module with a portion cutaway to illustrate the construction of the heat absorption module.
DETAILED DESCRIPTION OF THE INVENTION
[0013] Referring now to the drawings, the electronics enclosure of the present invention is shown therein and indicated generally by the numeral 10 . The electronics enclosure 10 comprises three main components: a housing 12 , a heat absorption module 40 , and a mounting bracket 70 . The housing 12 is designed to mount directly to the mounting bracket 70 or, alternatively, to the heat absorption module 40 . The heat absorption module 40 , when used, mounts to the mounting bracket 70 .
[0014] The housing 12 comprises a main body 14 and an access door 26 . Main body 14 comprises a substantially rectangular box made of a sheet metal or other heat conductive material. The main body 14 includes a top 16 , bottom 18 , sides 20 , 22 , and back 24 . A hinge 28 pivotally mounts the door 26 to one side 20 or 22 of the housing 12 . Door 26 includes a handle 30 for opening and closing the door 26 . Handle 30 may incorporate a conventional latch or locking mechanism to provide security. A door seal (not shown) may be provided to prevent moisture or other contaminants from entering the housing 12 . The back 24 of the housing 12 includes a series of mounting holes 32 used for mounting the housing 12 to a support structure. The number of mounting holes 32 is not material to the invention. In the exemplary embodiment shown in the drawings, there are four mounting holes 32 disposed adjacent the four corners of the housing 12 . As will be hereinafter described, the mounting holes 32 receive mounting studs 80 on the mounting bracket 70 .
[0015] The heat absorption module 40 is a sealed enclosure made of metal or other heat conductive material. In the exemplary embodiment shown in FIG. 1, the heat absorption module 40 comprises a front plate 42 , back plate 44 , top 46 , bottom 48 , and sides 50 , 52 . The front plate 42 , back plate 44 , top 46 , bottom 48 , and sides 50 , 52 are secured together by welding to form a sealed enclosure. A fill hole 54 and vent hole 56 are formed in the top 46 of the heat absorption module 40 . The fill hole 54 is used to fill the heat absorption module 40 with a phase change material (PCM). The PCM is heated to change it to a liquid state and then poured into the heat absorption module 40 . Vent hole 56 allows air to escape from within the heat absorption module 40 during filling. After filling, the fill hole 54 and vent hole 56 are sealed by plugs 58 .
[0016] The front plate 42 and back plate 44 of the heat absorption module 40 extend beyond the sides 50 , 52 in the exemplary embodiment shown in FIG. 1. Both the front plate 42 and back plate 44 include a series of mounting holes 60 , 62 . The mounting holes 62 in the back plate 44 receive mounting studs 80 on the mounting bracket 70 , as will be hereinafter described. The mounting holes 60 on the front plate 42 receive a bolt used to fasten the housing 12 to the heat absorption module 40 .
[0017] Mounting bracket 70 is a formed metal sheet having side portions 72 , 74 and a recessed central portion 76 . The central portion 76 includes a series of mounting holes 78 to receive bolts, lag screws, or other mounting hardware. Mounting studs 80 project from the side portions 72 , 74 . When the housing 12 is mounted directly to the mounting bracket 70 , the mounting studs 80 are received in the mounting holes 32 in the back 24 of the housing 12 . When the heat absorption module 40 is used, the mounting studs 80 are received in the mounting holes 62 in the back plate 44 of the heat absorption module 40 . In either case, the housing 12 or heat absorption module 40 is secured in place by nuts 88 that thread onto the mounting studs 80 . When the heat absorption module 40 is required, the housing 12 can be mounted to the heat absorption module 40 by carriage bolts 82 and nuts 84 , or other mounting hardware. In the exemplary embodiment of FIG. 1, the bolts 82 pass through the opening 60 in the front wall 42 of heat absorption module 40 and the opening 32 in the back 24 of housing 12 . The nuts 84 thread onto the end of the carriage bolts 82 to secure housing 12 to the heat absorption module 40 .
[0018] [0018]FIG. 4 illustrates a second embodiment on the modular electronics enclosure 10 of the present invention. The second embodiment of the electronics enclosure 10 uses many of the same components as the first embodiment. Therefore, the reference numerals used to describe the first embodiment will also be used in the description of the second embodiment to indicate the similar components.
[0019] The second embodiment includes a housing 12 , a heat absorption module 40 , and a mounting bracket 70 . The housing 12 is essentially the same as the first embodiment; whereas the heat absorption module 40 and mounting bracket 70 are slightly modified. In the second embodiment, the sides 50 , 52 of the heat absorption module 40 are flush with the lateral edges of the front wall 42 and back wall 44 . The opening 60 in the front wall 42 are connected to the openings 62 in the back wall 44 by sleeves 48 (FIG. 5). The sleeves 48 define a sealed passage through the interior of the heat absorption module 40 for the mounting hardware (e.g., carriage bolt 82 ) to pass through the heat absorption module 40 . The mounting bracket 70 has openings 86 in place of the mounting studs 80 of the first embodiment. The openings 86 in the mounting bracket 70 align with the openings 60 , 62 in the heat absorption module 40 and the openings 32 in the housing 12 . A single carriage bolt 82 and nut 84 can therefore be used at each corner of the enclosure to secure the entire assembly together. The carriage bolt 82 is inserted from the rear of the mounting bracket 70 as shown in FIG. 4 and passes through the sleeve 48 in the heat absorption module 40 . The exposed end of the carriage bolt 82 , on which the nut 84 is threaded, is contained inside the housing 12 .
[0020] The mounting bracket 70 in the second embodiment may include mating elements to align and support the heat absorption module 40 or housing 12 . The mating elements may comprise, for example, locating pins 90 on the mounting bracket 70 that insert into locating holes 92 in either the back wall 44 of the heat absorption module 40 or the back wall 24 of the housing 12 . The heat absorption module 40 likewise may include locating pins 94 that insert into locating holes 92 in the back wall 24 of the housing 12 . The locating pins 90 , 94 help support the components before the carriage bolts 82 are inserted. Those skilled in the art will recognize that the locating pins 90 , 94 and locating holes 92 could be reversed or that other forms of mating elements that interlock with one another could be used.
[0021] When the heat absorption module 40 is used, heat generated by the electronics inside the housing 12 or by the solar load is absorbed by the housing 12 and passed through conduction to the heat absorption module 40 . While below its phase change temperature, the PCM will absorb and remove heat from the housing 12 as the temperature inside the housing 12 increases. After reaching the phase change temperature, the PCM will continue absorbing heat from the housing 12 , but the temperature of the housing 12 and PCM will remain substantially constant until the PCM changes phase. A PCM can be selected which has a phase change temperature that corresponds to the maximum allowable temperature of the electronics enclosure 10 . Therefore, until the PCM completely changes phase, the maximum allowable temperature inside the housing 12 will not be exceeded.
[0022] In order not to exceed the maximum allowable temperature inside the housing 12 , the heat absorption module 40 must be able to absorb the energy of the solar load on the enclosure 10 without completely changing phase. Therefore, enough PCM must be used to absorb the solar load for as long as it is present. Since the solar load occurs only during the day, the PCM can absorb the energy during the daylight hours and pass the heat back to the housing 12 through conduction to be dissipated at night. Therefore, the amount of PCM used may be computed based on the latent heat of the PCM and the maximum solar load that could be absorbed by the enclosure 10 over one day.
[0023] Since the enclosure 10 can dissipate the heat generated by the electronics without the heat absorption module 40 , the heat absorption module 40 is not required. The present invention allows the heat absorption module 40 to be deployed when needed and to be omitted when the enclosure 10 is not subjected to solar loading. Using the present invention, the same housing 12 and mounting bracket 70 can be used in applications where solar loading is present, as well as applications when no solar loading is present. Thus, only one housing 12 and one mounting bracket 70 is required. The use of the same parts for both shaded and unshaded applications requires fewer parts to be stocked and simplifies ordering. The additional size, weight, and expense of the heat absorption module 40 is only added when needed. In addition, the present invention allows an enclosure 10 initially deployed without the heat absorption module 40 to be easily upgraded to include a heat absorption module 40 at a later time.
|
An electronics enclosure includes a mounting bracket adapted to mount to a support structure, a heat absorption module adapted to mount to the mounting bracket, and a housing to contain electronic equipment. The housing is adapted to mount alternatively to either the mounting bracket or the heat absorption module dependent upon solar loading conditions.
| 7
|
PRIORITY
[0001] This application claims priority to and the benefit as a divisional application of U.S. patent application entitled, “MEDICAL FLUID THERAPY FLOW CONTROL SYSTEMS AND METHODS”, Ser. No. 10/738,446, filed Dec. 16, 2003.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to medical systems and more particularly to medical fluid treatment therapies.
[0003] Due to disease, injury or other causes, a person's renal system can fail. In renal failure of any cause, there are several physiological derangements. The balance of water, minerals and the excretion of daily metabolic load are reduced or no longer possible in renal failure. During renal failure, toxic end products of nitrogen metabolism (e.g., urea, creatinine, uric acid, and others) can accumulate in blood and tissues.
[0004] Kidney failure and reduced kidney function have been treated with dialysis. Dialysis removes waste, toxins and excess water from the body that would otherwise have been removed by normal functioning kidneys. Dialysis treatment for replacement of kidney functions is critical to many people because the treatment is life sustaining. One who has failed kidneys could not continue to live without replacing at least the filtration functions of the kidneys.
[0005] Hemodialysis (“HD”), hemofiltration (“HF”), hemodiafiltration (“HDF”) and peritoneal dialysis (“PD”) are types of dialysis therapies generally used to treat loss of kidney function. Peritoneal dialysis utilizes a sterile dialysis solution, or “dialysate”, which is infused into a patient's peritoneal cavity and into contact with the patient's peritoneal membrane. Waste, toxins and excess water pass from the patient's bloodstream through the peritoneal membrane and into the dialysate. The transfer of waste, toxins, and excess water from the bloodstream into the dialysate occurs due to diffusion and osmosis during a dwell period as an osmotic agent in the dialysate creates an osmotic gradient across the membrane. The spent dialysate is later drained from the patient's peritoneal cavity to remove the waste, toxins and excess water from the patient.
[0006] Hemodialysis treatment removes waste, toxins and excess water directly from the patient's blood. The patient is connected to a hemodialysis machine and the patient's blood is pumped through the machine. Needles or catheters are inserted into the patient's veins and arteries to create a blood flow path to and from the hemodialysis machine. As blood passes through a dialyzer in the hemodialysis machine, the dialyzer removes the waste, toxins and excess water from the patient's blood and returns the cleansed blood back to the patient. A large amount of dialysate, for example about ninety to one hundred twenty liters, is used by most hemodialysis machines to dialyze the blood during a single hemodialysis therapy. Spent dialysate is discarded. Hemodialysis treatment lasts several hours and is generally performed in a treatment center about three times per week.
[0007] Hemofiltration is an effective convection-based blood cleansing technique. Blood access can be venovenous or arteriovenous. As blood flows through the hemofilter, a transmembrane pressure gradient between the blood compartment and the ultrafiltrate compartment causes plasma water to be filtered across the highly permeable membrane. As the water crosses the membrane, it convects small and large molecules across the membrane and thus cleanses the blood. A large amount of plasma water is eliminated by filtration. Therefore, in order to keep the body water balanced, fluid must be substituted continuously by a balanced electrolyte solution (replacement or substitution fluid) infused intravenously. This substitution fluid can be infused either into the arterial blood line leading to the hemofilter (predilution), into the venous blood line leaving the hemofilter (postdilution) or both. Another type of therapy, hemodiafiltration, combines the diffusion and convective cleansing modes of hemodialysis and hemofiltration.
[0008] A patient's hematocrit, which is the percentage of red blood cells in the blood, is about thirty-two to thirty-six percent by volume, leaving the amount of fluid in the blood to range from about sixty-four to sixty-eight percent. In a typical HDF and HF therapy, blood flow can be about 300 ml/min, wherein about 100 ml/min of the fluid is being removed through the filter, leaving a relatively smaller percentage of the blood as fluid to exit the hemofilter and to thereafter receive an amount of dialysate.
[0009] Postdilution is a more efficient blood clearance mode than predilution HF or HDF. In some instances, postdilution HF or HDF can be fifty percent more efficient than predilution HF or HDF. With postdilution clearance, however, blood exits the body and enters the filter before the extracorporeal circuit receives therapy fluid or dialysate. Because the hemodialyzer or hemofilter can remove a good portion of the liquid from the patient's blood, postdilution clearance can hemoconcentrate or clot the blood filter. Predilution clearance, on the other hand, infuses fresh therapy fluid into the extracorporeal circuit before the filter and therefore at least substantially reduces the possibility that blood will clot in the hemofilter or hemodialyzer.
[0010] With predilution HF or HDF, the dialysate is fed into the extracorporeal circuit prior to the hemofilter. Some of that fluid is then immediately removed by the filter, rendering the therapy less effective than postdilution therapy. Blood leaving the filter, however, has the same percentage liquid, e.g., sixty-four to sixty-eight percent, as the blood leaving the patient, reducing the chances of clotting or aggregating blood platelets because the blood has too high a percentage of solids.
[0011] It is therefore desirable to provide a hemofiltration and/or a hemodiafiltration system that can perform both predilution or postdilution clearance modes.
[0012] It is also desirable to provide an HF and/or an HDF system that provides a priming function, bolus infusion function and/or a blood rinseback function. System priming occurs at the beginning of therapy to remove air from the line, which would be harmful if delivered to the patient. The prime purges the air with a sterile or substantially sterile electrolyte solution.
[0013] At certain times during HF or HDF therapy it is necessary to deliver a bolus or relatively large volume of fluid to the patient. It may happen during therapy that too much blood is removed from the patient too quickly. The patient's vascular space contains only five to six liters of blood. Removing too much blood too quickly can possibly lower the pressure in the vascular space. The patient's heart rate will quicken and the vascular system will contract in an attempt to compensate for the loss in blood pressure, however, such measures may not be enough to prevent the patient from becoming hypotensive. In such a case, providing a bolus or volume of fluid to the patient is one effective procedure for increasing the blood pressure in the vascular system.
[0014] It is further desirable to have an HF or HDF system that can provide a blood rinseback at the end of therapy. At the end of therapy there is typically blood that remains in the extracorporeal circuit. It is desirable to return as much of that blood as possible to the patient. To do so, the blood therapy system needs to have the ability to pass a volume of fluid through the blood circuit sufficient to push the blood remaining therein back to the patient.
[0015] Both the bolus feature and the rinseback feature present challenges to the machine manufacturer. For instance, if the machine uses a fluid balancing system or match flow equalizer that removes an equal amount of fluid from the patient for each amount of fluid delivered to the patient, that balancing system must be accounted for to enable a positive net fluid volume to be delivered to the patient. Second, since the fluid is delivered directly to the extracorporeal circuit, the bolus or rinseback fluid needs to be sterile or of an injectable quality.
[0016] Removing ultrafiltrate (“UF”) from the patient is a precise operation in which a specific amount of fluid needs to be removed from the patient over the course of therapy. The amount of fluid removed from the patient therefore needs to be carefully monitored. In that regard, problems arise if the device or devices controlling the UF rate or volume output fails, e.g., if a valve fails. In such a case, uncontrolled flow from the patient can occur causing an overfiltration of the patient. It is therefore desirable to have an ultrafiltration flow control device that fails in such a way that fluid flow is blocked and uncontrolled UF removal does not occur.
[0017] Certain HF and HDF machines generate the fluid used during therapy at the time and place that the therapy takes place. Those machines are referred to as “on-line” machines because they make and provide the solution on-line. On-line machines use micro or ultrafilters to sterilize the solution or make it of an injectable quality before the solution is delivered to the patient's extracorporeal circuit. The filters over time accumulate bacteria and endotoxin along the outer filtering surfaces of the membranes located inside the filters. It is therefore desirable to have a method and apparatus that cleans or at least reduces the amount of bacteria and endotoxin that accumulate and reside along the membranes of the filters used to create dialysate on-line.
SUMMARY OF THE INVENTION
[0018] The present invention provides systems and methods for improving medical fluid delivery systems, such as hemodialysis (“HD”), hemofiltration (“HF”) and hemodiafiltration (“HDF”) systems. The present invention includes a multitude of aspects relating to medical fluid flow. In one aspect, systems and methods for selectively performing pre- and postdilution HF and HDF clearance modes are provided. In another aspect, systems and methods for providing priming, bolus and rinseback fluid volumes during/after HF and HDF therapies are provided. In a further primary aspect, improved systems and methods for removing ultrafiltrate from the patient are provided. In still a further aspect, the present invention provides an improved filtration configuration and method.
[0019] In one aspect of the present invention, an HF or HDF system is provided that performs pre- and/or postdilution clearance modes, e.g., concurrently or simultaneously. The system efficiently uses flow components to perform both pre- and postdilution clearance modes. For example, the system does not require an extra pump or an additional pump segment to be located in the substitution fluid line, wherein such additional components would have to be integrated into the machine to react appropriately to alarms and operator settings, etc.
[0020] The pre/postdilution feature of the present invention instead uses a “Y” connector located at the output of the system's substitution line. A first leg of the “Y” connector extends to the postdilution drip chamber. A first check valve is placed on the first leg to prevent blood from backing into the first leg or substitution fluid infusion line. The second leg of the “Y” can be used for multiple purposes, such as for a connection to the predilution drip chamber or the arterial line to prime the extracorporeal circuit. In the present invention, the second leg is used to deliver dialysate, prefilter, to the blood line. A second check valve is accordingly placed on the second leg to prevent blood from backing into the substitution line.
[0021] Two substitution line pinch clamps are provided, one for each leg output of the “Y” connector. In one embodiment, when pre- and postdilution are desired during the same therapy, the arterial line is primed. When the patient or nurse is ready to connect the dialysate lines to the dialyzer, the second leg of the “Y” connector is connected fluidly to an arterial drip chamber located upstream from the blood pump. The first leg of the “Y” connector is connected fluidly to the venous drip chamber. The electrically or pneumatically actuated substitution line pinch clamps placed on each of the first and second legs extending from the “Y” connector control the amount of substitution fluid used for predilution and postdilution infusion.
[0022] In one embodiment, the operator sets a total target substitution fluid volume that the patient is to receive. In addition, the operator inputs a percentage pre-versus postdilution setting, for example, by setting a specific predilution volume or flowrate or postdilution volume or flowrate or enters a percent predilution versus a percent postdilution. Upon starting therapy, the single substitution pump runs continuously, while the clamps alternate to achieve the desired pre- and postdilution percentage. For example, if the total substitution flowrate is 150 milliliters/minute (“ml/min”) and a fifty ml/min substitution predilution flowrate is desired, the postdilution clamp could be closed while the predilution clamp is opened for, e.g., five seconds, followed by the predilution clamp being closed and the postdilution clamp being opened for ten seconds. The result is a continuously running flow of fluid into one of the arterial or venous drip chambers, for example, to perform postdilution therapy a majority of the time for its improved clearance ability, while performing predilution therapy enough of the time to prevent blood clotting and hypotension.
[0023] The system is provided with suitable alarms and assurances, such as a sensor that senses if one or both the clamps is in the wrong position, e.g., both clamps being closed at the same time. In such a case, the machine sends an appropriate alarm and takes an appropriate evasive action. There are many alternative technologies to sense clamp position, such as via a microswitch, Reed switch, Hall effect switch, optical sensing, ultrasonic sensing, pressure transducer and the like.
[0024] In another aspect of the present invention, an HF/HDF system is provided that performs special fluid delivery functions, such as a prime, a bolus function and a blood rinseback using fluid components in an efficient arrangement. Those function can be commenced manually or automatically, e.g., upon receipt of a signal from a suitable biosensor. In one embodiment, a two-way isolate valve is placed in the post dialyzer therapy fluid or dialysate circuit. The isolate valve is electrically or pneumatically controlled by the machine controller to perform one of a plurality of functions at a desired time in therapy.
[0025] In one implementation, the isolate valve is used to perform a bolus infusion, e.g., to stabilize the patient who has low blood pressure or is hypotensive. The bolus amount can be predetermined or entered at the time it is needed. Upon an operator input or suitable signal from a sensor, a bypass valve in the upstream dialysate line is closed or de-energized so that normal flow to the dialyzer is stopped and so that an ultrafiltrate flowmeter is turned off. The isolate valve located downstream of the dialyzer is also closed, so that the dialyzer is isolated between the bypass and isolate valves. Transmembrane pressure (“TMP”) alarm limits, operable during normal therapy, are disabled while the dialyzer is isolated. A purge valve located upstream from the bypass valve is opened, allowing post dialyzer fluid sent previously to drain to be drawn through the purge valve to match the flow of fluid to the patient that flows through the balancing chambers or flow equalizer. The volume of fluid flowing to the patient flows through at least one filter, out of a substitution port, is pumped via the substitution pump to the venous drip chamber and through the venous access line to the patient. After the bolus amount is delivered, the purge valve is closed and the patient's blood pressure is allowed to stabilize. Next, the isolate valve is opened, the TMP limits are reset and normal therapy is resumed.
[0026] The above apparatus is also suitable to perform a substitution fluid rinseback at the end of therapy to rinse blood remaining in the extracorporeal circuit back to the patient. Here, the operator begins the procedure by pressing a “Rinseback” button and perhaps a “Verify” confirmation input. The rinseback feature, like the bolus volume, can be initiated automatically. An amount of rinseback solution can be preset or set at the time of the procedure. The valve configuration and operation described above is repeated using the bypass valve, isolate valve, TMP alarm limits and purge valve. The substitution pump delivers the programmed rinseback amount to the patient. Again, previously discarded solution is pulled back through the system to balance the fluid flowing to the patient through the match flow equalizer. Here, instead of delivering the amount to the venous dialyzer, as with the bolus solution, the amount is delivered to the arterial access line prior to the arterial drip chamber, so that as much of the extracorporeal circuit as possible is rinsed.
[0027] To communicate the substitution pump with the arterial access line, the operator can connect the access line to the second leg of the “Y” connector described above. Or, if the system is used in combination with the pinch clamps described above, the post-dilution clamp is closed and the predilution clamp is opened, allowing for automatic operation.
[0028] The machine is set to alert the operator when the rinseback is complete. After the fluid pressures have stabilized, the purge valve is closed, the isolate valve and bypass valve are opened, the TMP limits are activated and treatment is ended per the normal procedure.
[0029] In a further aspect of the present invention, the machine uses a ceramic piston rotating reciprocating pump for ultrafiltration (“UF”) instead of a more complicated, more accident prone and more expensive diaphragm pump type UF flowmeter assembly. The location of the ceramic pump is predialyzer, immediately downstream of the purge valves. The rotating, reciprocating piston pump is capable of running at a suitable high rate of speed, such as four to eight liters per hour, for rinse and disinfect modes. During therapy, the pump runs at a flowrate equivalent to the desired patient UF rate.
[0030] The substitution fluid flow and a volumetric equivalent to the patient's UF is taken from the flow path pre-dialyzer, that is, fresh solution is removed from the system. In one embodiment, the ceramic pump operates with balancing chambers that add and remove an equal volume of fluid to and from the system. Any fluid taken from the system by the ceramic piston pump and any substitution fluid given to the patient as an HDF or an HF infusion is automatically removed from the patient by the post-flow balancing chamber. The fresh solution is removed from the dialysate flow path, therefore, downstream from the balancing chambers so as not upset the balance of same.
[0031] There are many advantages to using the ceramic pump and associated flow configuration. The rotating reciprocating ceramic piston pump does not allow flow directly from the input to the output, in contrast to the balancing chamber type UF flowmeter. If the balancing chamber type of UF device fails, there is an uncontrolled flow during half of the cycle, resulting possibly in an overfiltration of the patient. The piston pump of the present invention, on the other hand, is not subject to that type of failure, because its input port does not communicate fluidly with the pump's outlet port. If the pump fails, it fails closed, stopping fluid flow. The piston also prevents purge valve errors from causing a UF error.
[0032] The rotations of the pump are monitored using a Reed Switch, optical sensor, flowmeter, tachometer or other type of feedback device, so the pump rotations and the corresponding ultrafiltration volume removed can be checked by an independent mechanism. The pump is placed before the dialyzer, preventing the pump from becoming clogged with organic substances removed from the dialyzer. The pump is, however, placed downstream from at least one membrane filter used to help purify the fresh dialysate. That arrangement provides a continual rinse along the surface of the membranes of the filters. The rinse removes at least a portion of the build-up of bacteria and endotoxin along the membrane surfaces. As a further advantage, the arrangement also removes air from the membrane filters during treatment. The removal of the balancing chamber type UF meter and addition of the rotating, reciprocating pump makes the flow path of the dialysis system simpler, while improving the safety and performance of the equipment. The ceramic piston pump in one embodiment is used to perform the rinseback and bolus infusion features that have been described previously. The pump in those applications operates in the opposite direction so that flow travels to the patient.
[0033] In a further aspect, an improved filter configuration and filtration method are provided. The configuration includes at least two filters placed in series between pumps or other hydraulically complicated flow mechanisms. The filter portion of the dialysate flow path is simplified to reduce the accumulation of bacteria and endotoxin. Also, a pump located upstream of the filters is operated to create a higher flowrate than a pump located downstream from the filters. The flow differential also helps to strip accumulated bacteria and endotoxins from membrane surfaces located within the filters as well as tubing connecting the filters.
[0034] Each of the above aspects can be employed alone or in any combination with one another.
[0035] It is therefore an advantage of the present invention to provide a hemofiltration (“HF”) or hemodiafiltration (“HDF”) system that can perform both pre- and postdilution clearance modes with a single substitution pump.
[0036] It is another advantage of the present invention to provide an HF or HDF system that performs certain net positive fluid flow functions, such as a prime, a bolus function and a rinseback function.
[0037] It is a further advantage of the present invention to provide an improved ultrafiltrate flow metering system.
[0038] It is yet another advantage of the present invention to provide an HF or HDF system with safety improvement features.
[0039] Moreover, it is an advantage of the present invention to provide an HF or HDF system with a simplified flow regime.
[0040] Still further, it is an advantage of the present invention to provide an HF or HDF system with performance improvement features.
[0041] Yet an additional advantage of the present invention is to provide a HF or HDF system with an improved filtration system and method.
[0042] Additional features and advantages of the present invention are described in, and will be apparent from, the following Detailed Description of the Invention and the figures.
BRIEF DESCRIPTION OF THE FIGURES
[0043] FIG. 1 illustrates systems and methods of the present invention for providing pre- and/or postdilution HF/HDF clearance modes, a bolus volume to the patient, a prime to the patient and/or a blood rinseback volume to the patient.
[0044] FIG. 2 illustrates one embodiment of a therapy fluid delivery manifold used in the systems and methods shown in FIG. 1 .
[0045] FIGS. 3 and 4 illustrate systems and methods of the present invention for removing ultrafiltrate from the patient and for filtering medical therapy fluid.
[0046] FIGS. 5 to 7 illustrate one embodiment of an ultrafiltrate pump used in the systems and methods shown in FIGS. 3 and 4 .
DETAILED DESCRIPTION OF THE INVENTION
[0047] The present invention provides systems and methods for improving medical fluid delivery systems, such as hemodialysis (“HD”), hemofiltration (“HF”) and hemodiafiltration (“HDF”) systems. In various embodiments, systems and methods for selectively performing pre- and postdilution HF and HDF clearance modes are provided. In other embodiments, systems and methods for providing bolus, prime and rinseback fluid volumes during/after HD, HF and HDF therapies are provided. In further embodiments, improved systems and methods for removing ultrafiltrate from the patient are provided. Still further, the present invention provides an improved filtration configuration and method.
Pre/Postdilution HDF and HF
[0048] Referring now to the drawings and in particular to FIG. 1 , an HF and/or HDF system 10 is illustrated. System 10 in one embodiment is part of a machine that can perform HD, HF or HDF as selected by a doctor or nurse. The machine is typically used in a treatment center and in one embodiment generates dialysis solution via generation unit 12 . One suitable dialysate generation unit 12 for system 10 is described in the maintenance manual for Baxter's System 1000® therapy machine. It should be appreciated from the disclosure herein, however, that the present invention is not limited to dialysate delivery systems or in-center systems but instead applies to any suitable medical fluid therapy treatment.
[0049] Whether system 10 operates in an HF or HDF mode, system 10 includes a dialysate flow path 20 and an extracorporeal or blood circuit 70 . In dialysate flow path 20 , fluid generated via generation unit 12 is pumped via a supply pump 14 through a supply regulator 16 , which sets the maximum pressure of the dialysate in the flow path. Dialysate path 20 employs a number of flow control devices that ensure that the desired amount of fluid is delivered to and removed from the patient (described in commonly owned U.S. Pat. No. 5,486,286, the teachings of which are incorporated herein by reference). In particular, dialysate flow path 20 includes a flow equalizer or balancing chamber 30 and an ultrafiltrate flowmeter 50 . Flow equalizer 30 includes a pair of fixed volume chambers 32 and 34 that each have a flexible membrane within, creating four variable volume cavities C 1 , C 2 , C 3 and C 4 . For fixed chamber 32 , the volume in variable cavity C 1 is inversely proportional to the volume in variable cavity C 2 . Likewise, for fixed chamber 34 , the volume in variable cavity C 3 is inversely proportional to the volume in variable cavity C 4 .
[0050] The two chamber pairs 32 and 34 are provided so that one fixed volume chamber 32 or 34 pumps fluid to the filter/dialyzer, while at the same time, a second fixed volume chamber 32 or 34 pumps an equal amount of fluid from the filter/dialyzer. Match flow equalizer or balancing chamber 30 therefore ensures that any fluid going through equalizer 30 is in turn removed from equalizer 30 , resulting in a net fluid gain or loss to the patient of zero. Cavities 32 and 34 also alternate so that in each stroke fluid is pumped to and from the patient, resulting in a steady or non-pulsitile flow profile.
[0051] Cavities 32 and 34 operate with inlet valves 36 and outlet valves 38 , which are alternated to achieve the above-described flow equalization. In particular, those valves are configured to enable one of the chamber pairs 32 or 34 to receive dialysate flowing through line 18 from regulator 16 to fill one of the cavities C 2 or C 4 . That filling action causes a corresponding one of the cavities C 1 or C 3 to decrease in volume and thereby push used or spent dialysate that filled cavity C 1 or C 3 in the previous stroke out line 22 , through an output pressure equalizer 24 , through a blood leak detector 26 and flow restrictor 28 to drain line 40 . While that action is happening, a dialysate pressure pump 42 is pulling spent dialysate from filter/dialyzer 44 and pushing that spent dialysate through a pressure regulating recirculation loop 46 to the other flow chamber pair 32 or 34 . Pump 42 pushes fluid into one of the variable spent dialysate cavities C 1 or C 3 .
[0052] The increasing volume of spent dialysate in the variable chamber necessarily decreases a like volume of fresh dialysate that filled variable cavity C 2 or C 4 in the previous stroke, pushing same toward the patient. Fresh dialysate is pushed out line 48 , through output pressure equalizer 24 , through a first ultrafilter 52 , through a portion of filtration line 88 , through a second ultrafilter 54 and through a dialysate monitoring manifold 56 . Suitable ultrafilter brands are discussed below. From manifold 56 , fresh filtered fluid flows either through a three-way bypass valve 58 , out bypass valve through line 60 into filter/dialyzer 44 or out through substitution port 86 , through the remainder of filtration line 88 and to blood circuit 70 .
[0053] As illustrated, a second outlet or bypass line 62 extends from bypass valve 58 and extends either into post-dialyzer line 64 , leading to pressure regulating recirculation loop 46 , or alternatively extends into rinse line 66 and through rinse valve 68 to drain 40 . Bypass line 62 , rinse line 66 and rinse valve 68 enable various system components to be rinsed or cleaned prior to the beginning of therapy.
[0054] Blood circuit 70 includes an arterial access line 72 and a venous access line 74 . Arterial access line 72 includes a Y-connection 76 that connects to a dialysate input line described below. Arterial line 72 carries blood from patient 78 to an arterial drip chamber 80 . Blood is transferred through extracorporeal circuit 70 via a peristaltic blood pump 82 . Pump 82 pumps blood from arterial line 72 , through drip chamber 80 , to the blood inlet of dialyzer 44 . The blood is pumped through the inside of membranes contained within the dialyzer, wherein diffusive transport of toxins and waste products from the blood takes place, and from the output of dialyzer 44 into a venous drip chamber 84 , through venous access line 74 , and back to patient 78 .
[0055] Predialyzer dialysate line 60 , dialyzer 44 , postdialyzer line 64 and the remainder of dialysate flow path 20 are maintained at a pressure lower than that of the blood within circuit 70 , resulting in the convective transport of waste out of the membranes within dialyzer 44 and a transport of waste and other undesirable substances from the patient's blood. System 10 is additionally or alternatively capable of performing hemofiltration, in which solution flows along filtration line 88 , through substitution port 86 , through microfilter/ultrafilter 90 , through postfilter line 92 , through substitution fluid pump 94 and through a pre/postdilution fluid manifold 100 , directly to blood circuit 70 .
[0056] Referring additionally to FIG. 2 in combination with FIG. 1 , pre/postdilution manifold 100 is illustrated in greater detail. Filter 90 in one embodiment is a microfilter. One suitable microfilter is a Pall™ Gelman™ single use 0.22 micron filter. In another embodiment, filter 90 is an ultrafilter. One suitable reusable ultrafilter is a Medica™ Diapure™ 28 filter. One suitable single use ultrafilter is a Medica™ 150u filter. In general, microfilters differ from ultrafilters in the capability of the different filters in removing small particles. In general, ultrafilters can remove smaller particles than can microfilters. For purposes of the present invention, the term “microfilter” includes filters having a membrane pore or membrane opening size of about 1000 to about 105 Angstroms (“Å”), which effectively filters particles, such as red blood cells, yeast, fungi, bacteria and some proteins. The term “ultrafilter” as used herein includes filters having a membrane pore or membrane opening diameter or length of about 10 to about 1000 Å, which effectively filters particles such as endotoxins (pyrogen), viruses and proteins. In one preferred embodiment, the ultrafilters used in the present invention have a range of pore sizes of about 10 to about 40 Å.
[0057] Filter 90 operates with ultrafilters 52 and 54 to ensure that a sterile or injectable quality fluid is pumped via substitution pump 94 into the substitution fluid manifold 100 . Fluid is pumped via pump 94 , through Y-connection 102 into either postdilution line 104 or predilution line 106 . A cap 108 is shown removed from a union 109 located at the end of pigtail 126 in line 106 . Manifold 100 in an alternative embodiment provides only postdilution line 104 and pigtail 126 , wherein remainder of line 106 is removed and the corresponding output from Y-connector 102 is capped off via cap 108 . The remainder of line 106 can then be selectively added to pigtail 126 by removing cap 108 . When predilution line 106 is fully connected, system 10 can perform either pre- and/or postdilution HF and HDF as desired.
[0058] As seen in FIG. 1 , postdilution line 104 extends to the venous drip chamber 84 . Predilution line 106 extends in one embodiment to a Y-connector or T-connector 76 positioned in a line 73 , which is located between pump 82 and drip chamber 80 . In an alternative embodiment, line 106 (shown in phantom) extends via a solenoid valve 77 (in phantom) to a second Y-connector or T-connector 79 located in arterial access line 72 , which feeds into post-pump line 73 . The alternative embodiment is used with a rinseback feature described below. As described in more detail below, it is advantageous to connect predilution line 106 to arterial access line 72 via connector 79 when system 10 is combined with the bolus, prime and rinseback features described below. It should be appreciated however that the predilution therapy operates equally as well with line 106 connected to arterial access line 72 via connector 79 or to line 73 via connector 76 .
[0059] A check valve 110 is placed in postdilution line 104 , which allows fluid to flow only in the direction from pump 94 to blood circuit 70 , preventing blood from backing up through lines 92 and 88 into filters 52 and 54 or other parts of dialysate flow path 20 . Likewise, a check valve 112 is placed in predilution line 106 to prevent blood from backing into dialysate flow path 20 from predilution line 106 .
[0060] Postdilution line 104 includes a pinch clamp 114 . Predilution line 106 likewise includes a pinch clamp 116 . Suitable pinch clamps for system 10 are provided for example by Medica™, Model M03122. Clamps 114 and 116 are electrically operated, pneumatically operated or are otherwise controlled via a microprocessor of system 10 to be opened and closed selectively as specified by the therapy. Manifold 100 of system 10 enables HF or HDF therapy to occur: (i) via postdilution clearance only by opening valve 114 and closing valve 116 throughout therapy; (ii) via predilution clearance only by opening valve 116 and closing valve 114 throughout therapy; (iii) via pre- and postdilution clearance modes by sequentially opening valve 114 , while valve 116 is closed and then reversing that state and opening valve 116 , while valve 114 is closed; or (iv) via pre- and postdilution clearance modes simultaneously by opening valves 114 and 116 simultaneously.
[0061] Although not illustrated, when pre- and postdilution therapy is performed simultaneously, a variable flow restrictor can be placed in either one or both pre- and/or postdilution lines 106 and 104 , respectively, to partition the percentage flow of dialysate through lines 104 and 106 as desired (e.g., 80% of flow flows through postdilution line 104 , while the remaining 20% flows through predilution line 106 ). To that end, valves 114 and 116 could instead be needling-type valves that selectively allow a desired percentage flow to pass through lines 104 and 106 . Or, such needling valves can be placed in combination with on/off valves 114 and 116 , so that there are valved flow restriction settings and on/off control for both pre- and/or postdilution clearance modes.
[0062] In one embodiment, the operator sets the overall target substitution volume into the machine employing system 10 . The operator then enters a percentage rate or percentage volume of pre-versus postdilution fluid flow. The single substitution pump 94 runs continuously. The clamps 114 and 116 alternate to achieve the desired pre- and postdilution clearance rates. In one example, if the desired percentage breakdown is two-thirds postdilution and one-third predilution and the total flowrate is 150 ml/min, the postdilution clamp could be closed for five seconds, while the predilution clamp 116 is open. Afterward, that state is reversed so that the predilution clamp 116 is closed, while the postdilution clamp 114 is open for the next ten seconds. That sequence is repeated throughout therapy, or at least the portion of therapy that includes convective clearance. Alternatively, flow restrictions are placed in lines 104 and 106 and set to produce the desired two-thirds postdilution of one-third predilution profile, while valves 114 and 116 are opened throughout the convective clearance portion of the therapy.
[0063] The goal of diverting some of the convective flow from postdilution to predilution is to prevent hemoconcentration while providing a predominantly postdilution treatment. To that end, it is desirable not to cycle the valves over too long a period so that such a condition could occur. On the other hand, it is also desirable not to cycle the valves too frequently for wear and maintenance purposes. The desired cycle time for the valves is therefore chosen to accommodate both of those factors.
Bolus and Rinseback Functions
[0064] Referring still to FIG. 1 , a second primary embodiment of the present invention involves the ability of system 10 to perform not only a priming sequence, but to also provide a bolus of fluid to the patient as needed and to perform blood rinseback at the end of therapy. The bolus feature and blood rinseback feature are described hereafter in turn.
Bolus Infusion
[0065] To provide a bolus or volume of fluid to the patient, for example, when the patient has lost too much liquid from the patient's vascular system, the bypass valve 58 is set so that dialysate flow no longer flows through predialyzer line 60 but instead bypasses the filter/dialyzer 44 and line 60 and flows alternatively through bypass line 62 . Rinse valve 68 is closed so that dialysate flowing through line 62 tees into dialysate return line 64 , which shunts the fluid through match flow equalizer 30 to drain 40 . The bypass valve 58 configuration has the effect of modifying the dialysate flow path 20 so that dialysate flow bypasses filter/dialyzer 44 . As described above, dialysate returning through line 64 is cycled through pressure regulating recirculation loop 46 via dialysate pump 42 . Recirculation loop 46 helps to control pressure at the inlet of the flow equalizer 30 . In particular, recirculation loop 46 operates with input pressure equalizer 118 and supply regulator 16 . Supply pump 14 sets a pressure along line 18 . That pressure in line 18 moves a diaphragm within input pressure equalizer 118 back and forth, which either restricts an orifice that builds pressure in loop 46 or opens the orifice lowering the pressure in the loop, which in turn allows more or less fluid to circulate within loop 46 .
[0066] Besides de-energizing bypass valve 58 so that dialysate flows through bypass line 62 , shutting off flowmeter 50 , an isolate valve 120 placed in postdialyzer line 64 is closed. Valves 58 and 120 completely isolate filter/dialyzer 44 from the remainder of dialysate flow path 20 . To create the bolus volume, with filter/dialyzer 44 isolated, purge valve 122 is opened to drain. At the same time, a portion of the fluid flowing from flow equalizer 30 to bypass valve 58 flows through filtration line 88 , out of substitution port 86 , through filter 90 , through postfilter line 92 and is pumped via substitution pump 94 and postdilution line 104 (or predilution line 106 ) through venous drip chamber 84 , which purges any air from the solution, allowing an injectable quality bolus or volume of fluid to flow into patient 78 via venous access line 74 . Since valve 122 is connected to an open source of fluid, namely, from fluid pumped via flow equalizer cavities C 1 and C 3 , through blood leak detector 26 , through flow restrictor 28 , through line 125 and though line 126 (shown with dual directionally pointed arrows), a volumetric equivalent to the fluid pumped to the extracorporeal circuit 70 via pump 94 can be infused into the system between the pre and post flow equalizers of equalizer 30 . After the fluid flows goes through valve 122 , the fluid flows through filters 52 , 54 and 90 and is monitored for proper conductivity and temperature. Pump 94 will shut down if any of those measurements is outside of a correct range.
[0067] The control scheme of system 10 is operable to manually or automatically initiate the bolus volume. In one embodiment, the control scheme automatically commences the bolus feature upon receiving an appropriate signal from a biosensor, such as a hemoconcentration sensor, a blood volume sensor, an electrolyte sensor, an oxygen sensor and any combination thereof.
[0068] It is important to note that the transmembrane pressure (“TMP”) alarm limits should be disabled or opened during the time that the isolate valve is closed. The TMP alarms in normal operation ensure that there is a positive pressure differential from the blood circuit 70 to the dialysate flow path 20 through dialyzer 44 , so that the net flow of liquid is from the blood stream to the dialysate flow path 20 . In addition, the TMP is monitored to detect pressure changes that may indicate a problem. When isolate valve 120 is closed, the TMP in dialyzer 44 isolated between valve 120 and bypass valve 58 may tend to equalize. However, because dialysis is not being performed at this moment, such equalization is not a concern and thus the alarms are not necessary.
[0069] Flow equalizer 30 requires an equal volume of fluid to flow from line 18 to the equalizer as the volume flowing to equalizer 30 from recirculation loop 46 . It should be appreciated that because there is a volume of fluid being delivered to the patient and no fluid can be pulled from the patient with dialyzer 44 isolated, less fluid would return to flow equalizer 30 through line 62 , compared to the amount of fresh fluid delivered to flow equalizer 30 from source 12 . Accordingly, a makeup source of fluid is needed. For example, if supply pump 14 delivers 300 ml/min to flow equalizer 30 and 100 ml/min is pulled through substitution port 86 to the patient, only 200 ml/min will return through bypass line 62 , postdialyzer line 64 , recirculation loop 46 to flow equalizer 30 . The fluid return is deficient by 100 ml/min with respect to the 300 ml/min global supplied via source 12 , and such deficiency will cause flow equalizer 30 to operate improperly.
[0070] To provide the additional fluid, purge valve 122 , which operates with ultrafilter 52 , is opened during the bolus infusion as discussed above. Purge valves 122 and 124 operate normally with ultrafilters 52 and 54 , respectively, to enable the filters to be rinsed prior to therapy. Opening purge valve 122 enables the additional needed fluid, e.g., the additional 100 ml/min, to be pulled through lines 125 and 126 and into the dialysate flow path 20 . Liquid pulled through drain line 126 has previously flowed through dialyzer 44 and been pumped to drain 40 after passing through flow equalizer 30 . Accordingly, the additional fluid pulled through line 126 needs to be sterilized to be of an injectable quality. The filters 52 and 54 and additional disposable filter 90 in filtration line 88 achieve that requirement. That is, fluid entering system 20 through purge valve 122 flows through ultrafilters 52 and 54 , out substitution port 86 , through a third ultrafilter or microfilter 90 and ultimately to patient 78 . Filters 52 and 54 in one embodiment are large surface area, reusable filters. Disposable filter 90 can be an ultrafilter or a microfilter. Placing three filters in series enables system 10 to have triple redundancy during normal operation and for the bolus infusion.
[0071] As an extra safety measure, if for some reason the makeup fluid pulled from drain line 126 and passing through both filters 52 and 54 does not produce an injectable quality solution, dialysate monitoring manifold 56 , which includes a dialysate conductivity probe, temperature sensor, a flow sensor and a dialysate pressure transducer will trip an alarm upon which substitution pump 94 is shut down. In the event that an alarm is tripped and substitution pump 94 is shut down, the configuration of the peristaltic pump 94 is such that the rotating head clamps the tubing off at a point along the tubing wrapped around the pump head, effectively stopping flow of fluid at that point.
[0072] To deliver the bolus volume, the substitution pump 94 pumps the volume through a check valve, such as check valve 110 of post dilution line 104 , into venous drip chamber 84 . It should be appreciated that pre- and postdilution manifold 100 is not necessary to practice the bolus solution feature of the present invention. However, the bolus solution volume can be implemented via pre- and postdilution manifold 100 discussed above. To do so, pinch clamp 114 is opened to allow the bolus volume to pass through check valve 110 , pass by clamp 114 and travel via line 104 to drip chamber 84 or, pinch clamp 116 is opened to allow the bolus volume to pass through check valve 112 , pass by clamp 116 via line 106 and travel to drip chamber 80 . From drip chamber 80 or 84 the bolus volume travels via venous access line 74 to patient 78 .
[0073] The amount of the bolus volume is either predetermined or set by the operator upon initiating the bolus function, for example, via a touch screen controller. In one embodiment, the bolus amount is set into the machine employing system 10 via a keypad on the touch screen. The amount of bolus can be controlled, for example, by monitoring the number of rotations of substitution pump 94 or by pumping until a desired setting is achieved on one of the biosensors described above. After the bolus volume is delivered to the patient, isolate valve 120 is opened, purge valve 122 is closed, and bypass valve 58 is energized to allow dialysate to flow through predialyzer line 60 , and not to line 62 . Opening valves 120 and 58 re-establishes fluid communication with dialyzer 44 . The TMP limits are accordingly reset or reopened. Prior to opening isolate valve 120 , one stroke can be taken of the UF flowmeter 50 to help create a positive transmembrane pressure when isolate valve 120 is opened. That procedure may be helpful in achieving a set UF target for the patient.
Blood Rinseback
[0074] The blood rinseback feature of the present invention operates in a similar manner to the bolus infusion feature described above. The blood rinseback amount can be set at the time the procedure is started or preset according to a prescription or therapy protocol. Again, a touch screen having a keypad can be used to set the rinseback amount. While the rinseback function can be initiated manually in one embodiment, the present invention also contemplates automatically starting the rinseback function at the end of treatment. Further, while the blood rinseback procedure can be controlled by inputting a set amount of fluid, it is also possible to control the feature via a blood detector placed near the patient end of venous access line 74 , which detects when no more blood is present in blood circuit 70 and stops substitution pump 94 accordingly and automatically.
[0075] Each of the major steps described above for performing the bolus infusion procedure is also performed for the blood rinseback procedure. Obviously, the procedures are performed at different times during therapy because the different procedures are for different purposes. The bolus function as described above is initiated manually or automatically when the patient appears to have become or is becoming hypotensive. Blood rinseback is performed at the end of treatment to push any blood remaining in the system back to patient 78 . Nevertheless, both procedures involve the use of isolate valve 120 and bypass valve 58 to isolate dialyzer 44 from the remainder of dialysate flow path 20 . Also, purge valve 122 is opened to enable an equal amount of fluid delivered to patient 78 to be drawn via drain line 126 , through filters 52 , 54 and 90 into dialysate flow path 20 , so that flow equalizer 30 operates properly.
[0076] One difference between the bolus function and the blood rinseback procedure is the location at which the blood rinseback volume is delivered to extracorporeal circuit 70 . As discussed above, the bolus volume can be delivered to venous drip chamber 84 . The rinseback amount is delivered on the other hand to the end of or to a point of arterial access line 72 marked by Y-connector or T-connector 79 , which is appropriate to clean blood in arterial line 72 through pump 82 , through arterial drip chamber 80 , through dialyzer 44 , through venous drip chamber 84 and finally through venous access line 74 to patient 78 . Connector 79 is connected to predilution line 106 via solenoid valve 77 to enable automatic control of the rinseback feature. It is contemplated therefore to use the pre- and postdilution manifold 100 in combination with the rinseback feature of system 10 and to deliver the rinseback volume from substitution pump 94 , through Y-connector 102 , through predilution line 106 , including check valve 112 and pinch valve 116 , through line 106 and solenoid 77 , to the arterial access line 72 at connector 79 .
[0077] It should be appreciated, however, that manifold 100 is not necessary to deliver the rinseback volume of the present invention. For instance, the fluid connection can be made manually by the operator or nurse. FIGS. 1 and 2 show a cap 108 that connects to a union 109 located at the end of pigtail 126 . It is possible that instead of using the already existing predilution line 106 when the rinseback volume is needed, cap 108 is removed from the union 109 of pigtail 126 and a substitution line (not illustrated) is manually coupled to the end of pigtail 126 and to either connector 79 of line 72 after being uncoupled from the patient or to connector 76 located in line 73 , for example, by removing a cap from connection 76 . In a preferred embodiment, that substitution line would include at its end a one-way valve or check valve, such as check valve 112 .
[0078] To couple the substitution line manually to connectors 76 or 79 , blood pump 82 is shut down and either a cap is removed from connector 79 or the arterial access line 72 is disconnected from an arterial needle of the catheter that is inserted into patient 78 . A clamp is closed at the end of the arterial needle so that no blood is lost from the patient. Connector 76 or 79 is then connected to the substitution line, which is also connected to the end of pigtail 126 . In a further alternative embodiment, a luer connector with a rotating hub is provided in one embodiment at the end of arterial access line 72 to couple the line directly to the substitution line extending from pigtail 126 . After that connection is made, the rinseback volume is delivered as described above.
[0079] The known way to provide a rinseback is to connect a saline bag to the arterial access line 72 after disconnecting such line from the arterial needle. Thereafter, saline flows from the saline bag through the arterial access line 72 to provide the saline rinseback or flush. Both the manual and automatically operating embodiments described above enable system 10 to eliminate the need for a separate saline or injectable solution supply to provide the blood rinseback.
Prime
[0080] The prime feature of the present invention operates using the apparatus described above in connection with FIG. 1 for the bolus and rinseback features to prime the extracorporeal circuit 70 prior to therapy. The prime includes a volume of fluid, such as dialysate, that is delivered at the beginning of the therapy to remove air from the extracorporeal circuit. The prime feature is used within a system or with a controller that is operable to receive an operator input to commence delivery of the prime. Alternatively, the system or controller is operable to commence delivery of the prime automatically at the beginning of therapy. In one embodiment, the amount or volume of the prime is entered by an operator when commencing delivery of the prime. The amount or volume can be predetermined prior to commencement of therapy. Alternatively, the amount or volume is delivered until air is no longer sensed in the extracorporeal circuit.
UF Flowmeter
[0081] Referring now to FIGS. 3 to 7 , another primary embodiment of the present invention is illustrated. FIGS. 3 and 4 illustrate systems 150 and 160 , respectively, which include many of the same components described above in connection with FIGS. 1 and 2 . Those components are marked with the same element numbers as used in FIGS. 1 and 2 . The description of those elements including each of the alternatives discussed above in connection with FIGS. 1 and 2 apply equally to like element numbers in FIGS. 3 and 4 .
[0082] One primary difference between the embodiments described in FIGS. 1 and 2 compared with the systems 150 and 160 of FIGS. 3 and 4 is that the UF flowmeter 50 is removed in FIGS. 3 and 4 . The function of the UF flowmeter so shown in FIGS. 1 and 2 is to remove fluid from the patient 78 that has accumulated in the patient's body over the time between the patient's last therapy and the current therapy. One of the problems that occurs with kidney failure is that the patient in many instances loses some or all of the ability to urinate. The fluid that would otherwise be removed from the patient via urination becomes stored in the patient's blood and surrounding tissues. Thus, while the dialyzer and the infusion of clean solution into patient 78 operate to clear waste products and other undesirable products from patient 78 , UF flowmeter 50 operates to remove an additional amount of fluid from the patient, which is equivalent to the amount of fluid gained by the patient between treatments.
[0083] UF flowmeter 50 operates in a similar manner to one of the chamber pairs 32 and 34 of flow equalizer 30 . UF flowmeter 50 defines a fixed volume chamber 132 that is separated by a diaphragm into two alternating variable volume cavities C 5 and C 6 . Fixed volume chamber 132 is sized in a desired relation to the matched volume chambers 32 and 34 . Inlet valves 136 and 138 of UF flowmeter 50 can be cycled with inlet valves 36 and outlet valves 38 of flow equalizer 30 . In that manner, a known volume of fluid is removed with each stroke or valve cycle. The valves 136 and 138 alternate so that cavity C 6 fills and pushes fluid previously drawn into cavity C 5 through one of the outlet valves 138 , whereafter the valves switch so that cavity C 5 fills and pushes the previously filled volume in cavity C 6 through the other outlet valve 138 .
[0084] UF flowmeter 50 is an effective but relatively complicated device. Also, the failure of one of the valves 136 or 138 can cause an uncontrolled flow during half of a cycle of the diaphragm, resulting in an overfiltration of the patient.
[0085] Another potential problem with system 10 illustrated in FIG. 1 is that air can become trapped in ultrafilters 52 and 54 . It is possible for air to also become trapped in disposable filter 90 , however, it is more likely that air enters reusable filters 52 and 54 . Another possible problem with system 10 is that dialysate pump 42 is placed directly in front of a UF removal line 134 , which leads to UF flowmeter 50 . That configuration can lead to the clogging of UF meter 50 . Also, the purge valves 122 and 124 are closed during normal therapy in system 10 , so that there is no flow across the outside the membranes of those filters (operational flow through filters is from the inlet of the filters to outside the membranes inside the ultrafilters, through the walls of the membranes, and through the inside of the membranes out the outlet of the ultrafilters). The material that is filtered in filters 52 and 54 remains inside the filters until a rinse cycle is performed after therapy, when purge valves 122 and 124 are opened. That is, bacteria and endotoxin that are filtered by the membranes inside ultrafilters 52 and 54 remain inside those filters throughout the duration of therapy.
[0086] Another potential problem in system 10 of FIG. 1 is that the only way to detect if one of the purge valves 122 and 124 is not functioning properly is to detect an increase or decrease in TMP. A TMP error that is not examined and diagnosed properly by an operator could result in a UF error for the patient.
[0087] Referring now to FIGS. 3 and 4 , the above-described problems are solved by removing UF flowmeter 50 and replacing same with a ceramic UF pump 140 in dialysate flow path 20 . Ultra pure dialysate for online HF and online HDF treatments is enabled by locating ceramic pump 140 downstream from the single purge valve 122 in system 150 of FIG. 3 and downstream of dual purge valves 122 and 124 in system 160 of FIG. 4 . In both cases, the purge valves are located downstream from the rinse outlet 142 of one of the ultrafilters 52 or 54 . Fluid that reaches pump 140 is therefore fluid that is to be removed along drain line 126 . As discussed below, pump 140 is a ceramic rotating, reciprocating piston pump in one embodiment, which is advantageous because it does not establish fluid communication between the inlet and outlet of the pump. That pump configuration enables the pump to fail safe, where uncontrolled fluid flow does not occur.
[0088] Locating ceramic pump 140 downstream of purge valves 122 and 124 provides additional advantages. That is, besides isolating the inlet and outlet of the pump and thereby eliminating the potential for UF error due to component failure, locating pump 140 predialyzer reduces the possibility of the UF pump becoming clogged or corrupted with organic substances. That is, UF removed to drain from pump 140 is clean or sterile solution from generation unit 12 . The likelihood of a UF occurring error due to endotoxin and bacteria building up in the UF removal device is therefore substantially decreased in systems 150 and 160 of the present invention.
[0089] Also, because pump 140 pulls fluid from the rinse outlet 142 of filters 52 and 54 , systems 150 and 160 provide a continual rinse along the outside of the membranes within those filters. In system 160 of FIG. 4 , the purge valves 122 and 124 are cycled. e.g., at fifty percent for each valve, so that both filters 52 and 54 are rinsed and cleaned as therapy takes place. The rinse along the outer surface of the membranes of filters 52 and 54 also removes air from the filters continuously or semi-continuously during treatment. Even though pump 140 removes fresh dialysate as UF, dialyzer 44 functions as described above to diffuse waste products from the patient's blood. Waste is also removed through convective transport caused by the direct infusion of blood into the extracorporeal circuit 70 . That waste is then pumped through balancing chambers 30 , via dialysate pump 42 , to drain. The UF pumping of fresh dialysate via pump 140 does not alter the effectiveness of the therapies of systems 150 and 160 .
[0090] As discussed above, one major advantage with using the ceramic rotating reciprocating piston pump 140 of the present invention is that fluid communication does not exist between the inlet and outlet of UF pump 140 . FIGS. 5 to 7 illustrate one embodiment of UF pump 140 , which is a rotating and reciprocating piston pump. FIGS. 5 to 7 illustrate the rotating reciprocating piston pump 140 in three states, namely, a fluid-in state in FIG. 5 , a dwell state in FIG. 6 and a fluid-out state in FIG. 7 . One suitable rotating reciprocating piston pump is supplied by Diener Precision Pumps, Embrach, Switzerland.
[0091] In FIGS. 5 to 7 , valve 140 includes a rotating chamber 142 defining an opening 144 that receives an end of a rotating and reciprocating piston 146 . The end of the piston 146 includes an arm 148 with a ball bearing type head 152 that is received slidingly inside a coupling aperture 154 , which is in fluid communication with opening 144 . As chamber 142 is rotated via a shaft 156 having a substantially vertical axis, head 152 is carried by the outer wall of coupler opening 154 , which in turn rotates arm 148 and shaft 146 . Due to the angle of shaft 146 relative to substantially vertical shaft 156 , head 152 , arm 148 and shaft 146 are also translated in a direction of the angle of shall 146 back and forth depending on the rotational location of coupler opening 154 during rotation of chamber 142 . As illustrated in FIG. 5 , during the fluid-in state, piston head 152 is pulled a further distance away from a pump body 158 than the vertical distance between piston head 152 and body 158 in the fluid-out state of pump 140 in FIG. 7 . Piston head 152 is accordingly at an intermediate relative distance away from body 158 in the dwell state of pump 140 shown in FIG. 6 . It should be appreciated, therefore, that the rotation of drive shaft 156 causes both a rotational motion and translational motion of shaft 146 relative to fixed body 158 .
[0092] Body 158 defines port openings 162 that enable a lubricant such as water to lubricate the sliding engagement between shaft 146 and the inner bore of body 158 . Body 158 also defines inlet and outlet ports 164 and 166 , respectively. The lower end of shaft 146 defines a notch 168 . Notch 168 in the fluid-in state of pump 140 enables fluid to enter via inlet port 164 into a pump chamber 170 . Importantly, in the fluid-in state, no fluid communication exists between pump chamber 170 and outlet port 166 . In the dwell state of pump 140 in FIG. 6 , shaft 146 has rotated to a position wherein notch 168 does not face or communicate with either port 164 or 166 , so that no fluid communication takes place between pump chamber 170 and the openings of ports 164 and 166 . In the fluid-out state of pump 140 in FIG. 7 , shaft 146 has rotated to a position wherein notch 168 enables fluid communication to exist between pump chamber 170 and outlet port 166 . Importantly, in the fluid-out state, no fluid communication exists between pump chamber 170 and inlet port 164 .
[0093] In operation, as the shaft moves from the fluid-out state ( FIG. 7 ) to the fluid-in state ( FIG. 5 ), the volume in pump chamber 170 increases, creating a vacuum and drawing fluid into chamber 170 . In the dwell state ( FIG. 6 ), the volume in pump chamber 170 has decreased from the volume in the fluid-in state ( FIG. 5 ), creating a positive pressure inside chamber 170 . As the shaft 146 moves from the dwell state ( FIG. 6 ) to the fluid-out state ( FIG. 7 ), the volume in chamber 170 further decreases and pushes fluid out of outlet port 166 .
[0094] Because inlet port 164 never communicates fluidly with outlet port 166 , pump 140 even upon a failure or loss of power cannot allow an uncontrolled UF flow, decreasing significantly the inherent error potential in comparison to the error inherent in the valves 136 and 138 of prior flowmeter 50 and with the flowmeter 50 itself, as well as potential UF errors that could occur from a failure of one of the purge valves 122 and 124 .
[0095] As alluded to above, the amount of ultrafiltrate removed from the patient is controlled in one embodiment by monitoring the number of rotations of shaft 146 . Rotating, reciprocating piston pump 140 is inherently accurate. If needed, however, a flow measuring device can be placed in drain line 126 to monitor the output of pump 140 .
[0096] Pump 140 may also be used with each of the embodiments described above in connection with FIGS. 1 and 2 , including the pre- and postdilution features, the bolus feature and the rinseback purge. In particular, FIGS. 3 and 4 can employ the manifold 100 discussed above in connection with FIG. 1 however same is not shown for the sake of clarity. To infuse the bolus and rinseback volumes, pump 140 rotates in the opposite direction to pull fluid from line 126 shown with dual directional arrows in FIGS. 3 and 4 in the same manner as discussed above.
Filtration Configuration
[0097] The present invention in FIGS. 1 and 4 shows an improved filtration configuration. To produce a suitable replacement fluid for patient 78 , an electrolyte solution such as dialysate is filtered by ultrafilters and/or microfilters to achieve an injectable quality output. The present invention employs three filters in series without an intervening pump placed between the filters. The filters each add successive log reduction of bacteria and endotoxin. When a pump is placed between the filters, the pump becomes a place where bacteria and endotoxin accumulate during quiescent times, such as when the system is off. Accordingly, the present invention eliminates the need for placing a pump between the in-series filters. It should be appreciated however that sensors and other flow components besides pumps are contemplated to be placed between the in-series filters.
[0098] In an attempt to remove as much bacteria and endotoxin as possible, the present systems shown in FIGS. 1 and 4 uses three filters in series, namely, filters 52 , 54 and 90 . Those filters help to ensure the quality of the solution by providing successive log reductions of bacteria and endotoxin. Filters 52 , 54 and 90 can be any combination of single use or reusable ultrafilters, microfilters or other endotoxin/bacteria reducing devices, such as a clarigen dialguard column. In one embodiment, filters 52 and 54 are reusable and the hydraulics path 88 is constructed without complex hydraulic features, such as a pump, after the first filter in the system, thereby reducing risk of microbial and biofilm growth after the solution is first filtered. In one embodiment, filter 90 is a single use microfilter.
[0099] For proper log reduction, it is important to lower the potential for bacteria growth and subsequent endotoxin production. To that end, the filtration configuration of FIGS. 1 and 4 employs no pumps between filters 52 , 54 or 90 . The flow of medical fluid from filters 52 and 54 passes through sterile tubing (and possibly other flow components) to the inlet of the next filter. Because more complex lumen surfaces of flow components have a greater the chance of forming biofilm, only tubing is provided in one embodiment between filters 52 and 54 and only a single dialysate monitoring manifold 56 is placed between filters 54 and 90 . Limiting the components between filters to only simple tubing (and possibly sensor components) helps to prevent the proliferation of bacteria on complex surfaces and to ensure the efficacy of the disinfection.
[0100] The purging function during the preparation phase of the medical fluid systems of the present invention also helps to remove bacteria or endotoxin that may have grown since the machine was last used. With the simplified flow path between filters 52 , 54 and 90 , however, very little growth occurs.
[0101] Placing pumps before and after the filters 52 , 54 and 90 enables the flowrate of fluid pumped, e.g., via dialysate pump 42 , through the filters to be higher than the flowrate pumped, e.g., via infusion pump 94 , to the patient 78 . The systems of FIGS. 1 and 4 can therefore be set so that that the medical fluid flow to patient 78 is only a portion (albeit a potentially large portion) of the total flow out of the filters, which can be reusable filters. For instance, if the systems are used for hemofiltration and are set to flow 250 ml/min of replacement fluid to patient 78 , the flow out of filters 52 , 54 and 90 can be 300 ml/min. The purpose for that excess flow is to prevent stagnant areas in the reusable filters at the connections of the filters to filtration line 88 , which helps to ensure that during quiescent times bacteria does not proliferate between filters 52 and 54 or after filter 54 in device 56 or filtration line 88 .
[0102] Due to the use of filters in the above-described manner, the quality of the replacement fluid can be ensured through the combined log reduction of the filters and because the filters to a large extent only have to filter contamination from the incoming medical solution. In addition if one of the filters fails, the resulting log reduction of the remaining filters in most instances is still sufficient to provide a medical grade solution. In addition, the smooth clean surfaces in between the filters are easily and effectively disinfected, preventing growth during quiescent periods. It should be appreciated that while the filtration configuration described herein is particularly well suited for the systems of FIGS. 1 and 4 , the configuration is expressly not limited to being used with the other features and inventions described in those figures and indeed is applicable to many different types of injection fluid flow regimes and configurations.
[0103] It should be understood that various changes and modifications to the presently preferred embodiments described herein will be apparent to those skilled in the art. Such changes and modifications can be made without departing from the spirit and scope of the present invention and without diminishing its intended advantages. It is therefore intended that such changes and modifications be covered by the appended claims.
|
A renal therapy blood cleaning system includes: a blood filtering device in communication with an extracorporeal circuit; a first pump configured to pump fluid to the blood filtering device; a second pump configured to pump fluid from the blood filtering device; a balance chamber in fluid communication with first and second lines, the first and second lines in fluid communication with the first and second pumps, respectively, the balance chamber configured to exchange like volumes of fresh and spent fluid; a plurality of valves; and a control scheme programmed to operate the plurality of valves to enable spent fluid taken from the balancing chamber through one of the first and second lines to be recirculated to the balance chamber through the other of the first and second lines to compensate for a volume of fresh fluid delivered to the blood filtering device.
| 0
|
BACKGROUND OF THE INVENTION
The present invention relates to a water temperature regulator, and more particularly to a water temperature regulator that may not only regulate water temperature depending on personal preference or actual need but also help save valuable water resource, and is therefore very suitable for mounting in a bathroom and connecting to a plumbing system having a hot-water pipeline included therein.
General water heaters for family use can be divided into two types, namely, gas heater and electric heater.
When using a gas heater to supply hot water, water that has remained in the hot-water service pipe since last use of the heater would directly flow to the faucet instead of flowing through and heated by the heater. A user would usually turn open the hot-water faucet to release and drain such water that has not been heated. It is, of course, a pity to waste so much useful water only because the water is not heated to a desired temperature for our use. Such unnecessary waste of useful water occurs each time we turn open a hot-water faucet immediately after we ignite the gas heater. When there is finally hot water released from the hot-water faucet, the user would usually turn open the cold-water faucet at the same time in order to regulate the temperature of released hot water by mixing the cold and the hot water. A lot of valuable water resource and heat energy is therefore unnecessarily wasted in the course of obtaining a desired temperature of hot water supplied by the gas heater.
And, in the case of an electric heater, there would still be water unnecessarily wasted when the hot-water faucet is first turned open to let out hot water that has been heated but stored in the hot-water service pipe before the use. This is because the user would usually drain some hot water before it reaches a desired higher temperature. Such unnecessary waste of water would occur again when we turn open the faucets the next time. And, there are also chances that the user needs to lower the temperature of hot water by mixing it with some amount of cold water. This would also, of course, unnecessarily waste some heat energy used to heat the water.
The above two situations of unnecessary waste of water resource and heat energy frequently happen in almost every family houses. Therefore, it is desirable to develop a set of improved domestic water temperature regulator with which any water that is to be used but has not reached a desired temperature may be sent to a separate water storage for reuse later and thereby avoid unnecessary waste of water.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a water temperature regulator that has means to display the temperature of water flowing through the regulator and means to guide water having a temperature lower than a desired value to a separate water storage for reuse later instead of being arbitrarily wasted.
To achieve the above and other objects, the present invention mainly includes a closed container on which a cold-water inlet pipe, a hot-water inlet pipe, a discharge pipe, a water service pipe, a control, and a water temperature indicator are provided.
The cold-water inlet pipe is connected to a cold-water pipe of a plumbing system in the house in order to introduce cold water into the container, and has a cold-water flow control connected thereto for regulating a flow of the cold water being introduced into the container via the cold-water inlet pipe.
The hot-water inlet pipe is connected to a hot-water pipe in the house plumbing system in order to introduce hot water into the container, and has a hot-water flow control connected thereto for regulating a flow of the hot water being introduced into the container via the hot-water inlet pipe.
The discharge pipe is connected to a pipeline in the house plumbing system for discharging water in the container to a water storage via the pipeline, and the pipeline has a check valve connected thereto to prevent water from flowing back into the container via the discharge pipe.
The water service pipe is led to a water supply outlet to allow water in the container to flow to the water supply outlet via the water service pipe.
The control controls open/close of the discharge pipe and the water service pipe at different time or close of the discharge pipe and the water service pipe at the same time, so that water in the container either flows out the container via the discharge pipe or the water service pipe or is stored in the container, depending on one of three control modes selected for the control.
The water temperature indicator includes a water temperature sensor and a water temperature display and is able to immediately show a temperature of water in the container.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects of the present invention and the features and functions thereof can be best understood by referring to the following detailed description of the preferred embodiments and the accompanying drawings, wherein
FIG. 1 is a perspective of a first embodiment of the present invention;
FIG. 2 illustrates the connection of the first embodiment of the present invention of FIG. 1 to a plumbing system in a house;
FIG. 3 is a perspective of a second embodiment of the present invention;
FIG. 4 illustrates the connection of the second embodiment of the present invention of FIG. 3 to a plumbing system in a house; and
FIG. 5 shows another type of water temperature indicator used in the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Please refer to FIG. 1 that shows a water temperature regulator according to a first embodiment of the present invention. As shown, the water temperature regulator includes a closed container 1 provided with a cold-water inlet pipe 2, a hot-water inlet pipe 3, a discharge pipe 4, a water service pipe 5, a control 6, and a water temperature indicator 11. The cold-water inlet pipe 2 downward extends from a right side of a bottom of the container 1 for connecting a cold-water pipe 22 thereto in order to introduce cold water into the container 1. A flow of the cold water introduced into the container 1 is regulated by a cold-water flow control 21 connected to the cold-water inlet pipe 2.
The hot-water inlet pipe 3 downward extends from a left side of the bottom of the container 1 for connecting a hot-water pipe 32 thereto in order to introduce hot water into the container 1. A flow of the hot water introduced into the container 1 is regulated by a hot-water flow control 31 connected to the hot-water inlet pipe 3.
The discharge pipe 4 sideward extends from an upper point on a right wall of the container 1 for discharging water in the container 1 via a pipeline connected to the discharge pipe 4. A check valve 41 is connected to the pipeline at a predetermined position to prevent water from flowing back into the container 1 via the discharge pipe 4.
The water service pipe 5 upward extends from a right side of a top of the container 1 to allow water in the container 1 to flow out for service via the water service pipe 5.
The control 6 is located at a top right corner of a front of the container 1 for controlling the open of the discharge pipe 4 or the water service pipe 5 at different time or the close of the discharge pipe 4 and the water service pipe 5 at the same time, so that water in the container 1 either flows out the container 1 via the discharge pipe 4 or the water service pipe 5, or is stored in the container 1, depending on a control mode selected for the control 6.
The water temperature indicator 11 is mounted on a central portion of the front of the container 1 so that a user may easily observe it. The water temperature indicator 11 mainly includes a water temperature sensor and a water temperature display and is able to immediately show the temperature of water in the container 1.
Please refer to FIG. 2 that illustrates the connection of the water temperature regulator of the present invention to a family plumbing system. The water temperature regulator shown in FIG. 2 is mounted in a bathroom with the cold-water inlet pipe 2 connected to a cold-water supply pipe 22 extended from a water tower 23, the hot-water inlet pipe 3 to a hot-water supply pipe 32 extended from a water heater 33, the discharge pipe 4 to a first pipeline 42 that leads to an upper part of a water storage 43 and has a check valve 41 connected thereto at a predetermined position, and the water service pipe 5 to a second pipeline led to a shower head 51. The water storage 43 is provided at a bottom with a third pipeline 44 that leads to a water tank 45 of a toilet 47. The cold-water supply pipe 22 extended from the water tower 23 has a branch that extends into a lower part of the water storage 43 and has a float-ball switch 48 connected to an end of the cold-water supply pipe branch 22.
When a user wants to, for example, take a shower, and it is assumed the water heater 33 is used for the first time on that day, the user may first turn the control 6 to open the discharge pipe 4 and then turns open cold-water and hot-water faucets for cold water and hot water to flow from the cold-water supply pipe 22 and the hot-water supply pipe 32 into the container 1 via the cold-water inlet pipe 2 and the hot-water inlet pipe 3, respectively. Since the discharge pipe 4 is opened, cold and hot water flown into the container 1 would finally flow out the container 1 via the discharge pipe 4 and into the water storage 43 via the water pipe 42. The cold-water flow control 21 and the hot-water flow control 31 may be turned to respectively regulate flow of the cold and the hot water into the container 1. Meanwhile, the user may observe the water temperature display of the water temperature indicator 11 for a temperature of the water in the container 1. When the observed temperature of water is suitable for shower and meets the user's preference, the control 6 may be switched to close the discharge pipe 4 and open the water service pipe 5, so that water in the container 1 is supplied via the water service pipe 5 to the shower head 51 for use. With these arrangements, any water flowing into the container 1 and not reaching a desired water temperature could be discharged from the discharge pipe 4 to the water storage 43 via the first pipeline 42 for reuse later without being unnecessarily wasted. In the example illustrated in FIG. 2, the water flown from the container 1 into the water storage 43 may be supplied to the water tank 45 via the third pipeline 44 for flushing the toilet 47. After the shower, the user may switch the control 6 to close both the discharge pipe 4 and the water service pipe 5, making the container 1 in a closed condition. At this point, both cold and hot water supplies are stopped. When the water heater 33 is used for a second time later, for example, by a second user for shower, the user may observe the temperature display of the water temperature indicator 11 for the temperature of water in the container 1. In the case the temperature of water in the container 1 has lowered since last use of the water heater 33, the control 6 may be switched to open the discharge pipe 4 and close the water service pipe 5. When the hot water supplied into the container 1 mixes with the cold water in the container 1 and the temperature of mixed water reaches a desired a value, the control 6 can be switched to close the discharge pipe 4 and open the water service pipe 5 for the hot water to flow to the shower head 51. Again, any water discharged from the container before the water temperature reaches a desired value would flow via the first pipeline 42 to and be collected in the water storage 43 for reuse later without being wasted.
In the case a user is not sure about a value of temperature of water that would be most suitable for shower or meet his or her personal preference, the user might need to test and obtain the preferred water temperature by switching the control 6 more than one time. However, after a preferred or most suitable water temperature has been found through tests and shown on the display of the water temperature indicator 11, the user may, in all future uses of the water temperature regulator of the present invention, conveniently determine whether the suitable or preferred water temperature has been reached simply by observing the temperature value shown in the display 11.
When the present invention is connected to the plumbing system as shown in FIG. 2, water collected in the water storage 43 can not only be guided to the water tank 45 via the third pipeline 44 for flushing the toilet 47 but also be introduced directly to the toilet 47 via a fourth pipeline 46 when a water level in the water storage 43 exceeds a port provided at an upper part of the water storage 43 to which an upper end of the pipeline 46 is connected. On the other hand, when the water level in the water storage 43 is low, the float-ball switch 48 functions to admit water in the water tower 23 into the water storage 43 via the water pipe branch 22, allowing water in the water tank 45 always at a full level.
It is to be noted that the water temperature regulator of the present invention is not limited to have only one water service pipe 5. FIG. 3 illustrates a second embodiment of the present invention that is similar to the water temperature regulator according to the first embodiment of the present invention, except that it has an additional water service pipe 7 provided on the top of the container 1 near a left side thereof, and an admission pipe 8 provided at a central portion of a left wall of the container 1. A second control 71 is provided at a top left corner of the front of the container 1 to control the open or close of the additional water service pipe 7. Please now refer to FIG. 4 that illustrates the connection of the water temperature regulator according to the second embodiment of the present invention to a family plumbing system. As shown, the connections of all components that are similar to the first embodiment of the present invention are the same as that shown in FIG. 2. However, the additional water service pipe 7 is led to a faucet 72 and the admission pipe 8 is connected to a fifth pipeline 81 that leads to a bathtub 84 and has a pump 82 and a cock 83 connected thereto. When the control 6 is set to close both the water service pipe 5 and the discharge pipe 4, the second control 71 can be turned to open the additional water service pipe 7 for water of suitable temperature in the container 1 to flow to the faucet 72 via the water service pipe 7. And, when the cold-water and the hot-water flow controls 21 and 31, respectively, are both closed, the pump 82 could be actuated to pump used water in the bathtub 84 into the water temperature regulator of the present invention for sending to the water storage 43. Thereby, used water in the bathtub 84 may be recycled via the present invention.
The temperature display of the water temperature indicator 11 of the present invention is not limited to a mechanical or an electronic type. However, when the temperature display is of an electronic type, as that shown in FIG. 5, it is preferable to mount it outside the container 1 and remotely connect to the container 1 via a suitable wire.
Moreover, it is not a prerequisite to have a three-mode control 6 provided on the container 1 for controlling the open or close of the discharge pipe 4 and the water service pipe 5. Instead, the discharge pipe 4 and the water service pipe 5 may have their own independent control for controlling the open and close thereof.
With the above arrangements, the water temperature regulator of the present invention is not only novel in its structure but also practical in use with respect to its function of helping general consumers to recycle waste water and save valuable water resource and heat energy.
What is to be noted is the form of the present invention shown and disclosed is to be taken as a preferred embodiment of the invention and that various changes in the shape, size, and arrangements of parts may be resorted to without departing from the spirit of the invention or the scope of the subjoined claims.
|
A water temperature regulator having a closed container that is provided with a cold-water inlet pipe and a hot-water inlet pipe having flow control connected thereto for introducing cold and hot water, respectively, into the container at a desired flow rate, a discharge pipe for guiding water in the container to an external water storage, at least one water service pipe for guiding water in the container to at least one water supply outlet, such as a showerhead or a faucet, at least one control for controlling open/close of the discharge pipe and of the at least one water service pipe, and a water temperature indicator for showing a temperature of water in the container. Instead of being drained, water introduced into the container that has not reached a desired temperature is discharged to and stored in the water storage for reuse later without being unnecessarily wasted.
| 8
|
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 12/053,229, filed Mar. 3, 2008, which in turn is a continuation of U.S. application Ser. No. 10/837,605, filed May 4, 2004, entitled “Personal Virtual Assistant,” now U.S. Pat. No. 7,415,100, which in turn is a continuation of U.S. application Ser. No. 09/519,075, filed Mar. 6, 2000, now U.S. Pat. No. 6,757,362; all of these applications are hereby incorporated by reference in their entireties.
FIELD OF THE INVENTION
[0002] The present invention relates to a computer-based, personal virtual assistant for managing communications and information, whose behavior can be changed by the user and whose behavior automatically adapts to the user.
BACKGROUND OF THE INVENTION
[0003] Mobile professionals, such as physicians, attorneys, sales representatives and other highly mobile professionals often find it difficult to communicate with clients, customers, colleagues and assistants. These mobile professionals travel frequently and are not accessible via a desk telephone or traditional, wired computer network. They typically employ human assistants to relay important information, maintain their schedules and filter out all unnecessary interruptions. The virtual assistant of the present invention allows the mobile professional to access personal, company, and public information, including contacts, schedules, and databases from any interactive device, such as telephone.
[0004] Electronic assistants with voice interfaces are known. U.S. Pat. No. 5,653,789 to Miner, et al. discloses a method implemented by a computer-based electronic assistant to receive and manage incoming calls to a subscriber. The electronic assistant in Miner, however, does not disclose a virtual assistant whose underlying behavior can be changed by the user or who has any degree of automatic adaptivity.
[0005] Voice response systems (VRS) that automatically adapt to the user are known. For example, U.S. Pat. No. 5,483,608 to O'Sullivan discloses an interactive VRS that automatically adapts to suit the speed at which the caller interacts with the system. The VRS disclosed in O'Sullivan is programmed to measure the response times of the caller and adjust the playing speed of the application dialogue's voice messages accordingly using an algorithm incorporated into the application software of the voice response system. Thus, if the caller is responding relatively fast and without error to the voice message prompts, the system will gradually speed up subsequent voice message prompts. If the caller is responding more slowly to the voice message prompts or is making errors in their responses, the system will slow down subsequent voice message prompts. The system disclosed in O'Sullivan, however, does not perform the actions of a virtual assistant, nor does it permit the user to control how the system adapts.
[0006] Another caller adaptive VRS is disclosed in U.S. Pat. No. 5,553,121 to Martin et al. Martin et al. discloses a system for varying the voice menus and segments presented to the user of a voice response system according to the competence of the user. The response time of a user to voice prompts is measured and an average response time is determined. It is assumed that the lower the average response time, the greater the competence of the user. The average response time is used as an index to a table of ranges of response times. Each range has respective voice segments associated therewith. The voice segments comprise oral instructions or queries for the user and vary according to the anticipated competence of the user. If the average response time changes such that the voice segments indexed are different to the current voice segments then a data base containing information relating to user competence is updated to reflect such a change. Accordingly, when the user next interacts with the voice response system a new set of voice segments more appropriate to the user's competence will be played. The system in Martin et al. also discloses determining user competence by identifying individual callers using existing caller identification technology. The call identification code of a telephone call can be used as an index to data stored in a user database comprising information relating to the competence of a user. Alternatively, the user can be asked to enter a password before further access is allowed to the system. The password can then serve as an index to the stored data associated with the user. The stored data identifies which set of voice data is appropriate for use during an interaction with said user. Alternatively, determining the number of times per day that a user accesses the system or the length of time which a user has subscribed to such a system may also be indicative of their competence. Again, VRS disclosed in Martin does not perform the functions of a virtual assistant, nor does it permit the use to have any significant degree of control over the behavior of the system.
[0007] Further, while the prior art systems adapt automatically to the caller, the degree of adaptation is relatively limited. For example, the prior art systems do not disclose a virtual assistant that automatically uses words associated with polite discourse when the user's input contains words associated with polite discourse. Prior art systems also do not disclose a virtual assistant that adapts to the user based on the user's emotional state.
SUMMARY OF INVENTION
[0008] The present invention relates to a personal virtual assistant with many discrete features, each of which comprises a separate but related invention. Thus, one aspect of the present invention is a computer-based virtual assistant the behavior of which can be changed by the user, comprising a voice user interface for inputting information into and receiving information from the virtual assistant by speech, a communications network, a virtual assistant application running on a remote computer, the remote computer being electronically coupled to the user interface via the communications network, wherein the behavior of the virtual assistant changes responsive to user input.
[0009] Another aspect of the present invention is a computer-based virtual assistant that automatically adapts its behavior comprising a voice user interface for inputting information into and receiving information from the virtual assistant by speech, a communications network, a virtual assistant application running on a remote computer, the remote computer being electronically coupled to the user interface via the communications network, wherein the remote computer is programmed to automatically change the behavior of the virtual assistant responsive to input received by the virtual assistant. As detailed below, the virtual assistant adapts to the user in many different ways based on the input the virtual assistant receives. Such input could be user information, such as information about the user's experience, the time between user sessions, the amount of time a user pauses when recording a message, the user's emotional state, whether the user uses words associated with polite discourse, and the amount of time since a user provided input to the virtual assistant during a session.
[0010] Other features and advantages will become apparent based on the following detailed description of the preferred embodiments and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is an overview of the virtual assistant (VA) of the present invention;
[0012] FIG. 2 is a diagram of the VA Server;
[0013] FIG. 3 is a diagram of the VA Studio;
[0014] FIG. 4 is a diagram of the VA Engine conceptual model;
[0015] FIG. 5 is a diagram of the VA Manager conceptual model;
[0016] FIG. 6 is a screen shot of the Microsoft Management Console for managing the VA Server Manger;
[0017] FIG. 7 is a screen shot of a web page that uses Active Server Pages to manage the VA Server Manager;
[0018] FIG. 8 is a diagram of the component relationships of a VA Server Set;
[0019] FIG. 9 is a diagram of a relatively small VA system;
[0020] FIG. 10 is a diagram of a large VA system;
[0021] FIG. 11 is a diagram of a very large VA system;
[0022] FIG. 12 is a diagram of a hardware configuration for a single ISDN PRI link;
[0023] FIG. 13 is a diagram of a hardware configuration for a two ISDN PRI links;
[0024] FIG. 14 is a screen shot of the Custom Component Selection screen;
[0025] FIG. 15 is a screen shot of GlobalCall Feature Selection screen;
[0026] FIG. 16 is a screen shot of the Outlook Feature Selection pane;
[0027] FIG. 17 is a screen shot of the VA Management Console;
[0028] FIG. 18 is of the VA Management Console with the general information form displayed in the right panel;
[0029] FIG. 19 is a screen shot of the Add Application Instance Dialog box;
[0030] FIG. 20 is a screen shot of the Select TTS Server Dialog box;
[0031] FIG. 21 is a screen shot of the Add Recognition Server Dialog box;
[0032] FIG. 22 is a screen shot of the Add VA Engine Dialog box;
[0033] FIG. 23 is a screen shot of the Set Application File Dialog box;
[0034] FIG. 24 is a screen shot of the Add Process Dialog box;
[0035] FIG. 25 is a screen shot of the Properties Display Panel for a Resource Manager Service;
[0036] FIG. 26 is a screen shot of the Alert Configuration Interface;
[0037] FIG. 27 is a screen shot of the TTS Dictionary Display;
[0038] FIG. 28 is a screen shot of the Dictionary Entry Dialog box;
[0039] FIG. 29 is a screen shot of the Database Manager Panel;
[0040] FIG. 30 is a screen shot of the Mailbox Properties Dialog with Virtual Assistant Tab;
[0041] FIG. 31 is a screen shot of the General tab on the Virtual assistant Preferences screen;
[0042] FIG. 32 is a screen shot of the Phone/Pager Tab on the of the Virtual assistant Preferences screen;
[0043] FIG. 33 is a screen shot of the VA Interaction tab on the of the Virtual assistant Preferences screen;
[0044] FIG. 34 is a flow chart that illustrates a call flow based on different tempo and assertiveness settings;
[0045] FIG. 35 is a screen shot of the Phone Schedule screen;
[0046] FIG. 36 is a screen shot of the Virtual assistant Tab; and
[0047] FIG. 37 is a diagram of a choice prompt stream with corresponding active segments.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0048] The subheadings used herein are meant only so as to aid the reader and are not meant to be limiting or controlling upon the invention. Generally, the contents of each subheading are readily utilized in the other subheadings.
[0049] Overview
[0050] Mobile professionals, such as physicians, attorneys, sales representatives and other highly mobile professionals often find it difficult to communicate with clients, customers, colleagues and assistants. These mobile professionals travel frequently and are not accessible via a desk telephone or traditional, wired computer network. They typically employ human assistants to relay important information, maintain their schedules and filter out all unnecessary interruptions. The virtual assistant of the present invention allows the mobile professional to access personal, company, and public information, including contacts, schedules, and databases from any interactive device, such as telephone.
[0051] The virtual assistant (“VA”) system of the present invention is comprised of two main components: (1) the VA Server, which is built on a Windows NT telephony server platform, and (2) the VA Studio, which allows skilled information technology professionals to develop VA applications that interface with electronic messaging systems, such as Microsoft Exchange and Lotus Notes. The VA Server is a component of the Service Deployment Environment (“SDE”), which is discussed in more detail below. The VA Studio is a component of the Service Creation Environment (“SCE”), which is also discussed in more detail below.
[0052] As shown in FIG. 1 , the VA Server 10 is comprised of a human interface 12 and a network interface 14 for handling calls and providing automated access to information to corporate 28 , private 30 and pubic 32 information repositories and sources. The human interface 12 is comprised of a graphical user interface 22 , which may be a web browser, a subscriber (or user) voice user interface 24 , generally accessed by a telephone, and a public voice user interface 26 . The virtual assistant allows a user to use a voice interactive device, such as a telephone, either wired or wireless, to access and update such information. The VA Server also manages all incoming communications by sorting, prioritizing, and filtering such communications, while providing notice to the user of important messages and events.
[0053] VA Server
[0054] As seen in FIG. 2 , a core component of the VA Server 40 is the voice-enabled Virtual Machine 42 , which is also referred to as the VA Engine. The VA Engine receives spoken commands, interprets and executes them. The VA Engine supports a COM interface 44 , which in turn enables VA applications to provide voice access to network applications.
[0055] The VA Engine also supports a telephony interface 46 to voice messaging 52 and private branch exchange systems 54 , enabling third-party systems to be integrated with the VA Server.
[0056] The VA Server conforms to Windows NT telephony and speech interface specifications. The voice messaging interface 56 supports the VPIM (Voice Profile for Internet Mail) standard, and provides a gateway between proprietary voice messaging systems and VA Server.
[0057] The VA system management services provide operations, administration and maintenance capability (OA&M) 60 . The OA&M applications also provide a Simple Network Management Protocol (“SNMP”) interface to third party management applications, such as HP Openview and CA Unicenter.
[0058] In the preferred embodiment, the VA Server is operable on Windows NT Server, release 4.0 or higher, in both single and multiprocessor configurations. Those skilled in the art, however, recognize that the VA Server can be ported to other computing platforms. Multiple systems may be clustered together to support higher system workloads and fail-safe operation.
[0059] VA Application
[0060] The VA Application, in the preferred embodiment, is compatible with a messaging server 62 , such as Microsoft Exchange/Outlook. The VA's architecture, however, advantageously permits integration with other commercially available and customized messaging applications. The VA Application can be easily modified to satisfy specific requirements of a user. The basic functions of the VA Application include:
[0061] Messaging—voice-mail, e-mail, and faxes
[0062] Contact Management—scheduling, planning, group calendar, contact and referral organization
[0063] Call Control—remote users to perform conference calling and call management; notification and forwarding features allow remote users to be contacted immediately by phone/pager when they receive specific voice-mails, e-mails, faxes, or pages Internet Applications—users can access and internet via an internet server 64 and obtain public information such as weather, travel, financial, competitive data and news
[0064] Intranet Applications—users can remotely access information contained on a corporate network (inside the company firewall) using the VA, for example, customer data, shipping and inventory information, sales reports, and financial data, or any information on a database server 66 , including SQL databases such as Oracle or Informix.
[0065] Customer Relationship Management applications—the VA Server integrates with commercially available customer relationship management (CRM) software applications 70 , such as Siebel, Pivotal, Sales Logix and Onyx.
[0066] VA Studio
[0067] As seen in FIG. 3 , the VA Studio 80 is comprised of a grammar generator 82 and a publishing toolkit 84 . The VA Studio allows a user to create, modify and debug applications that run on the VA Server 40 without requiring the user to be skilled in the complexities of the underlying components of the VA Server, such as the speech recognition engine, text to speech engine, switch control and unified messaging.
[0068] VA Studio employs a graphical user interface (GUI) application that runs on a Windows NT workstation. It allows developers to create projects, each of which defines a VA application. VA Studio is a multiple document interface (MDI) application that follows the workspace-based model.
[0069] The VA Studio follows the Microsoft Component Object Model (COM). VA applications are developed using Active Scripting languages such as VBScript and JScript, thus enabling integration with a variety of third party components. The VA applications created with the VA studio will include voice query to SQL databases, message stores, business logic and mainframe applications.
[0070] VA applications are composed of discourses and resources. Discourses are the context of conversations between a user and the VA. Resources are items like voice prompts and dictionaries. A developer can utilize the VA Studio Wizard to generate a “skeleton” VA application template. Application templates consist of packages of predefined discourses and resources. Discourses are the context of conversations between a user and the VA. Resources are items like voice prompts and dictionaries. Once a VA application template is generated, the application is further customized using any supported Active Scripting languages.
[0071] After writing the VA application, it is then submitted to the build process. During the build process, VA Studio checks for dialog errors, builds a master intermediate grammar and builds a master lexicon. Once compiled and error-free the application is ready to be published.
[0072] When an application is published, it is transported from the VA Studio to the VA Server. The VA Server allows a scripted application to access services such as voice mail, databases, and telephony equipment.
[0073] A VA application is created, modified, debugged and tested using the VA Studio. The completed application is then automatically installed and configured to run on the VA Server, which enables the VA application to take incoming calls and provide access to both public and private information.
[0074] Platform Overview
[0075] An Introduction to Virtual Assistant Applications
[0076] A VA application allows a user to manage electronic communications and access his or her business's computer resources through a telephone. Using speech recognition and text-to-speech technology, the VA communicates with callers in spoken English. By calling into the VA on a standard telephone, a user can perform functions such as the following:
[0077] Sending and receiving voice mail messages
[0078] Checking, replying to, and forwarding email messages
[0079] Looking up phone numbers and addresses in an electronic address book
[0080] Accessing information in a company database
[0081] Accessing information on the World Wide Web
[0082] In addition, the VA can perform many of the functions of a personal secretary, such as the following:
[0083] Informing the user via pager when new voice and email messages arrive
[0084] Filtering incoming voice mail, email, and pages as instructed by the user
[0085] Automatically dialing phone numbers
[0086] In the preferred embodiment, the VA performs the above functions by interfacing with a company's Microsoft Exchange server. This application, in effect, allows users to use their desktop Outlook software over the telephone.
[0087] The VA software includes a development platform (the SCE) and run-time platform (the SDE), which can host a variety of different VA's. The SDE provides the core components necessary for the functionality of a VA: a telephony interface, speech recognition facilities, a text-to-speech engine, interfaces with databases and mail servers, and an administrative framework in which the assistant applications will run. The SCE also includes development tools that programmers can use to create custom VA applications.
[0088] VA Platform Components
[0089] As discussed above, the VA Platform consists of three main components:
[0090] The Service Deployment Environment (SDE)
[0091] Virtual Assistant Applications
[0092] The Service Creation Environment (SCE)
[0093] The function of each of these components can be understood using a World Wide Web analogy. The SDE functions like a web server, providing connections with the network and telephone system, controlling the execution of VA applications, and providing resources such as text-to-speech and voice recognition engines that will be accessed by the applications that run on it.
[0094] The VA applications are analogous to web pages, determining the content that will be presented and controlling the interactions with the user. A VA application uses scripting languages such as VBScript, JavaScript, and Perl, so that developers can add significant functionality to a VA, such as performing mathematical calculations, processing text, and calling ActiveX and COM objects.
[0095] Just as Microsoft Front Page and Netscape Composer are used to create web pages, the SCE is the development environment used to create the VA applications. The main component of the SCE is the VA Studio application, which is based on the Microsoft Visual Studio paradigm and provides a graphical environment with a variety of tools that can be used to create, debug, and publish applications that are run on the SDE. The SCE also includes a set of COM objects that can be used in applications to perform functions such as checking email, reading from a database, and manipulating sound files.
[0096] The SDE Service Processes
[0097] The Service Deployment Environment consists of eight processes that run simultaneously and perform the functions necessary to support a VA application. In the preferred embodiment, each of these SDE components runs as a Windows NT Service or background process.
[0098] Although they may all run on the same hardware platform, for large VA implementations the components can be distributed across several servers and communicate over the network. Such distribution can allow, for example, one server to be dedicated to performing voice recognition functions while another supports the VA Engine that actually runs the applications. When multiple VA components are distributed across multiple machines, these machines are collectively termed a VA server set.
[0099] The VA Engine
[0100] As illustrated in FIG. 4 , the VA Engine 100 is the virtual machine on which a VA application 102 runs. Based on the application's instructions, the VA Engine uses its telephony interface 104 to communicate with the user 106 and its speech interface 110 to recognize speech into text and translate text into speech. The VA Engine connects to an Active Scripting Engine 112 to execute the scripts contained in the VA application, and it also communicates with administrative processes such as the VA Server 114 and VA Manager 116 .
[0101] In the preferred embodiment, the user is electronically coupled to the virtual assistant application via a public switched telephone network. As can be appreciated by one skilled in the art, the communications network that electronically couples the user interface to the computer on which a virtual assistant application is running could be a packet switched telephone network. Also, the communications network could be a wireless communications network.
[0102] A VA Engine process can support user interaction over only one telephone line, but multiple VA Engines can be run simultaneously on a single platform. If the VA platform is connected to more than one telephone line, then a separate VA Engine will be running for each incoming line.
[0103] The Text-to-Speech (TTS) Server
[0104] The Text-to-Speech Server 120 receives text from other components, translates it into speech (that is, into a sound file), and returns it to the requesting component. This speech translation service is isolated in a separate component to improve performance and to allow for TTS vendor-independence. The preferred embodiment uses the AcuVoice TTS system, but the platform can be easily modified to support a TTS engine from a different vendor. Only the TTS Server component would have to be modified for such a customization, not the entire platform.
[0105] Multiple VA Engines can use the same TTS Server process, and more than one TTS Server can be running at the same site, allowing translation services to be distributed across multiple machines for load-balancing.
[0106] The Recognition Server
[0107] The Recognition Server 122 receives sound files from other components, attempts to recognize them as speech, and returns the recognized text. Like the TTS server, the Recognition Server is a component that isolates speech-recognition functions from the rest of the VA platform. The server provides an interface to a third-party voice recognition engine (in the preferred embodiment, Nuance) that can be changed to a different vendor's brand without requiring the entire VA platform to be modified.
[0108] Multiple VA Engines can use the same Recognition Server process, and more than one Recognition Server can be running simultaneously.
[0109] Recognition Server Sub-Processes
[0110] The Recognition Server process requires three additional processes to be running:
[0111] The Resource Manager: The Resource Manager is a management process that automatically load-balances requests when more than one instance of the Recognition Server is running. Rather than making recognition requests to a particular Recognition Server, the VA Engine makes the request to the Resource Manager, which forwards it to the first available Recognition Server.
[0112] The Compilation Server: The Compilation Server compiles dynamic grammars.
[0113] The License Manager: The License Manager server runs continually in the background and dispenses licenses to all requesting components. Only one license manager need run in a single server set, but no Recognition Server components can launch unless the license manager is already running.
[0114] In the preferred embodiment, all of the sub-processes of the Recognition Server are recommended only for Nuance brand Recognition Servers. If a user uses different speech recognition software, a different set of processes may be needed.
[0115] The VA Server
[0116] The VA Server 114 performs persistent VA functions that should occur even when no user is connected to a VA application. These functions include the following:
[0117] Monitoring external sources such as email boxes, databases, and web sites for events (e.g. a new mail message arrives or a database field is updated)
[0118] Applying rules and filters to external source events to determine whether the VA system should take any actions
[0119] Paging users when specified events occur
[0120] Only one VA Server can run on a system, but a single VA Server can provide persistent services to multiple VA Engines running both locally and on remote systems.
[0121] The VA Manager
[0122] As illustrated in FIG. 5 , each system that is running one or more VA components should also be running the VA Manager application 116 . This application creates and monitors all VA components that are active on the system, and it provides management interfaces that are used for the following purposes:
[0123] Configuration (both at start-up and during run-time)
[0124] Signaling of events such as errors and informational messages
[0125] Logging of events
[0126] Logging of each call received by the VA applications running on the system
[0127] Performance monitoring (through an interface to Window NT's Perfmon utility)
[0128] The VA Manager provides the interface through which the VA Server Manager 130 communicates with all systems in use at the site.
[0129] The VA Server Manager
[0130] The VA Server Manager 130 provides a single point of control for all of the processes and servers being used in a VA server set. It communicates with the VA Manager 116 running on each VA server in the set and, through this interface, allows an administrator to use a single system to manage the entire site.
[0131] There are two ways an administrator can connect with the VA Server Manager application:
[0132] Using the Microsoft Management Console (MMC): As illustrated in FIG. 6 , the VA software includes an MMC snap-in component 140 that allows the VA Server Manager services (and, thereby, the entire VA site) to be managed from the Microsoft Management Console application.
[0133] Using an Administrative Web Page: The VA software also includes an administrative web page 142 that uses Active Server Pages to interface with the VA Server Manager service, allowing an administrator to manage the site through a standard web browser.
[0134] Returning to FIG. 5 , the VA Server Manager 130 monitors all of the VA components (such as Recognition Servers 132 , TTS Servers 134 , and VA Engines 136 ) running on all the systems within the server set, and it can be configured to page the system administrator with an alert if components fail or other system-critical events occur.
[0135] Additional VA Platform Components
[0136] In addition to the service processes, the following components are used on the VA platform.
[0137] The VA Database
[0138] The VA Server Manager process uses a Microsoft MSDE database to store configuration parameters and platform logs. The MSDE database engine is installed automatically as part of the VA platform install, and the recommended tables and initial data are created during the installation routine.
[0139] The VA Server Manager uses a COM object called DBManager to communicate with the database. This object is created automatically at start-up by the VA Server Manager and provides a set of application programming interfaces (API's) that other VA components can use to retrieve configuration information and log data. In addition, the DBManager object automatically handles version checking, database restoration, and other database management functions.
[0140] The VA Web Server
[0141] In the preferred embodiment, as illustrated in FIG. 7 , the VA platform uses a Microsoft IIS Web Server to support browser-based administrative utilities. These utilities include the following a VA Logging Tool, which is used by the administrator to view and manage system logs.
[0142] VA Shared Directories
[0143] The VA software uses a set of shared directories for storing files necessary for platform operations. In a multi-server implementation, these shares are stored on a central server (the same server that hosts the VA Server Manager process) and can be accessed by all the systems in the server set. The shared directories used by the VA platform are described in the table below.
[0000]
TABLE 1-1
VA Platform Shared Directories
Directory
Description
% conitava
Used to store the source files for the
%.backslash.VAApplications
applications that will run on the platform
% conitava
Used to store application logs
%.backslash.VALogs
% conitava
Used to store information about VA users
%.backslash.VAUsers
% conitava
Used to store temporary sound files
%.backslash.VAUtterances
containing he commands spoken by
VA users
% conitava % represents the base path under which the VA platform software was installed. By default, this path is c:.backslash.Program Files.backslash.Conita Virtual Assistant.
VA Platform Configurations
[0144] The service processes that make up the VA platform either can be run on a single server (a VA platform server) or can be distributed across multiple servers (a VA platform server set). A single-server implementation is adequate for small companies that need to support only a few incoming VA calls at a time. For larger companies, however, a server set implementation will be necessary for load balancing.
[0145] As illustrated in FIG. 8 , when the VA platform is distributed across multiple servers, one node in the server set is designated the Server Set Controller Node 150 . As the platform's primary server, the Server Set Controller Node will host the following components:
[0146] The VA Server Manager service 152
[0147] The VA DBManager service 154 and the VA database 156
[0148] The IIS web-server
[0149] Shared directories that will be used by all the servers in the server set to store logs, utterance files, application files, and user information
[0150] Each secondary node 160 in the set will host one or more instances of VA Engines 162 , TTS Servers 164 , and/or Recognition Servers 166 . These processes will be monitored by a VA Manager process 170 on each server, which will in turn communicate with the VA Server Manager 172 on the Server Set Controller Node 150 . In single-server implementations, the lone server is configured as the controller node, hosting the database, web-server, and VA Server Manager process along with all other VA services.
[0151] Scaling a VA Implementation
[0152] The way a business configures its VA platform will depend on the number of users who will be interacting with the VA application. As illustrated in FIG. 9 , for smaller sites, all the VA components can be run on a single server 180 . Such a site could support several incoming telephone lines 182 , allowing up to multiple instances of the VA application to be running simultaneously.
[0153] For larger sites that need to support many simultaneous VA application sessions, the VA components can be distributed across multiple systems. As illustrated in FIG. 10 , a medium-sized company may, for instance, use a six-server rack 184 , with two of the servers running VA Engines 186 a , 186 b , two servers running Recognition Servers 190 a , 190 b , one running VA Servers 192 , and one running TTS Servers 194 .
[0154] A large organization may require even more scalability. As illustrated in FIG. 11 , to support a public switch 196 with 32 incoming T1 lines 200 , the site may use upwards of eight systems for VA Engines 202 , sixteen for Recognition Servers 204 a , 204 b , four for VA Servers 206 , and four for TTS Servers 206 .
[0155] Duties of the VA Administrator
[0156] The duties of the VA Virtual Assistant platform administrator include the following tasks:
[0157] Preparing the server(s) for installation of the VA platform software
[0158] Installing the VA software on the systems
[0159] Ensuring that the application software can communicate with the telephone system and other hosts such as a Microsoft Exchange server
[0160] Configuring Microsoft Exchange to support VA users
[0161] Using the VA management interfaces to manage the systems in the server set, start and stop the VA services, and run VA applications
[0162] Monitoring the platform interfaces and error logs
[0163] Maintaining the VA database
[0164] Managing VA user accounts
[0165] In order to perform the above duties, a VA administrator needs to have experience with the following software packages:
[0166] Windows NT
[0167] Microsoft Exchange Server
[0168] Microsoft Internet Information Server (IIS)
[0169] Microsoft MSDE or SQL Server databases
[0170] Platform Server Prerequisites
[0171] In the preferred embodiment, a VA platform server system uses two (2) personal computers, each of meets the minimum hardware requirements listed in the table below:
[0000]
Component
Requirement
Processor
Pentium III central processing unit (CPU)
Memory
128 MB
Disk Space
200 MB Minimum, 1 GB Recommended
Network
a PCI 10/100 local area network (LAN)
adaptor
Sound Card
A Windows-compliant sound card
Microphone
A Windows-compliant external microphone
Telephony Adapter
Dialogic D/240PCI-T1 (PCI Bus)
(Telephony Server Only)
Conferencing Adapter
One of the following:
(Optional, Telephony Dialogic DCB/320 (ISA
Bus) Server Only) Dialogic DCB/640 (ISA
Bus) Dialogic DCB/960 (ISA Bus)
recommended only for installations that
support the call conferencing feature
Voice Resource Board
One of the following:
(Optional, Telephony Dialogic D/320SC (ISA
Bus) Server Only) Dialogic D/640SC (ISA
Bus)
RAID (Optional, Servert
A RAID solution is recommended for use on
Se Controller Node only)
the Server Set Controller in High-traffic
environments
[0172] In the preferred embodiment, the following operating system and third-party software are be installed on a server in order to support the VA platform software.
[0000]
Component
Requirement
Operating System
Windows NT 4.0 with the following options
and add-on software:
Windows Messaging Option NT Service Pack
5 Windows NT Option Pack 4.0 (Controller
Node Only) Microsoft Management Console
(MMC), Version 1.1 Microsoft Data Access
Controls (MDAC) Version 2.1
Web Server
Microsoft Internet Information Server Version
(Controller Node only)
Web Browser
Microsoft Internet Explorer Version 5.0
Voice Recognition
Nuance 6.2.1
Software
Text-To-Speech Software
AcuVoice 3.02
Exchange Client
Microsoft Outlook 2000
Should be installed with the Collaboration
Data Objects (CDO) option
Fax Services (optional)
Facsys or Jfax Recommended only for systems
that will support Fax services
[0173] Prerequisites for Other VA Systems
[0174] In the preferred embodiment, the prerequisites for installing the SCE on a workstation are listed in the table below:
[0000]
Component
Requirement
Operating System
Windows NT Workstation or Server 4.0 NT
Service Pack 5 or higher
Web Browser
Microsoft Internet Explorer Version 5.0
[0175] In the preferred embodiment, the prerequisites for installing the VA Management Console software on a remote workstation are listed in the table below:
[0000]
Component
Requirement
Operating System
Windows NT Workstation or Server 4.0 NT
Service Pack 5 or higher
Web Browser
Microsoft Internet Explorer Version 5.0
[0000]
TABLE 2-2
VA Administrative Station Requirements
Concurrent
Users Supported
Processes Recommended
23
23 VA Engines (391 MB memory)
1 Recognition Server
46
46 VA Engines (782 MB memory)
1 Recognition Server
[0176] Smallest configuration supported:
[0177] 1 Controller Node (uniprocessor)—VA Engines & Telephony
[0178] 1 Rec Node (multiprocessor)
[0179] Pre-Requisite Installation Process
[0180] Although in general there is no one order required for installing the pre-requisite software packages for the VA platform, the following sequence is generally used when preparing a VA platform server:
[0181] Windows NT 4.0 operating system
[0182] NT Service Pack 5.0
[0183] Windows NT Option Pack 4.0 (Controller Node only)
[0184] Dialogic DNA 3.2 software (Telephony server nodes only)
[0185] Nuance Speech Recognition software
[0186] AcuVoice TTS software
[0187] Microsoft Management Console (MMC) Version 1.1
[0188] Microsoft Data Access Controls (MDAC) Version 2.1
[0189] Outlook 2000
[0190] Installing & Configuring Windows NT
[0191] Domain Considerations
[0192] In the preferred embodiment, all of the VA platform servers and the Microsoft Exchange Server are located in the same Windows NT domain. A server's domain should not be changed after the VA platform is installed. For this reason, when installing the VA software on a machine, it is recommended that the server already be properly configured on the domain in which it will be used.
[0193] Initial Configuration
[0194] When installing and configuring the Windows NT operating system on VA platform servers, the following steps should be performed:
[0195] When partitioning the hard drive(s), use NTFS on all disk volumes. If there are already have FAT volumes on the system, they can be updated to NTFS after Windows NT is installed
[0196] During the Select Components phase of the installation, select the Windows Messaging option. If the Windows Messaging option is not selected, or if a server on which Windows NT has already been installed is being prepared, the option can be added later.
[0197] Installing Windows NT Add-Ons
[0198] After the basic Windows NT operating system is installed on the server, the following set of add-on packages should be installed in the specified order:
[0199] NT Service Pack 5.0:
[0200] Windows NT Option Pack 4.0 (On the Server Set Controller Node only): The Option Pack is needed to install the proper version of the Microsoft Internet Information Service (IIS) on the node. Although IIS can be select as an option when installing Windows NT 4.0, the version included on the core media does not support Active Server Pages and therefore cannot be used.
[0201] When installing the Option Pack, Upgrade Only option should be used. Although IIS is recommended only on the Server Set Controller Node, this Option should be installed.
[0202] Pack on secondary servers in case Controller Node later needs to be moved to a different server.
[0203] Microsoft Management Console (MMC) Version 1.1: The Windows NT Option Pack installs an earlier (1.0) version of MMC, so the MMC Version 1.1 should be installed after installing the Option Pack software.
[0204] Microsoft Data Access Components 2.1
[0205] Internet Explorer Version 5.0: Although an earlier version of Internet Explorer is installed along with the Windows NT and the Option Pack software, Version 5.0 is used in the preferred embodiment on VA platform.
[0206] Configuring RAID
[0207] For the server that will act as the Server Set Controller Node, a RAID solution should be installed to provide large, reliable storage for VA logs and utterance files. If a RAID solution is used, it should be properly configured after installation of the operating system on the Controller Node.
[0208] Configuring the Telephony Hardware
[0209] Hardware Requirements
[0210] The VA platform requires up to three different types of telephony boards, depending upon the types of services that will be available. Telephony hardware is recommended only in the platform's telephony server(s). Small installations will likely have only a single machine performing telephony services, though larger configurations may require multiple systems.
[0211] Telephony Adapter Boards
[0212] VA platform installations should have an ISDN PRI connection to the local telephone network. The Dialogic D/240PCI-T1 Board is recommended to connect the platform to the telephone system. This board provides both the interface to the telephone network and the voice processing resources that are recommended for speech recognition. The D/3240PCI-T1 board supports 24 ports on a single ISDN PRI link, providing 23 active channels for voice connections (one channel is reserved for internal use). The D/240PCI-T1 board provides approximately half the total amount of voice resources recommended to support concurrent VA sessions on all of the board's channels. In order to support simultaneous sessions on all 23 available ports, a voice resource board (described below) is recommended:
[0213] Voice Resource Boards
[0214] A voice resource board provides the extra processing power recommended to support the full simultaneous use of all ISDN PRI channels on the telephony adapter board(s). Each D/240PCI-T1 adapter contains enough hardware resources to support 12 simultaneous VA sessions. Generally, an additional 22 voice resources are recommended to support VA sessions on all 23 channels. In the preferred embodiment, the Dialogic D/320SC voice resource board provides 32 voice resources, and the Dialogic D/640SC voice resource board provides 64 voice resources.
[0215] Based on the number of resources provided, one D/320SC board will provide full support for a single ISDN PRI link. A D/640SC board is recommended to fully support two PRI links.
[0216] Conferencing Adapters
[0217] A Dialogic audio conferencing adapter is recommended for all VA platforms that will support the VA application's call conferencing feature. Three different models of conferencing adapters can be used, depending upon the call traffic that needs to be supported:
[0218] Dialogic DCB/320: Supports up to 32 simultaneous conferees
[0219] Dialogic DCB/640: Supports up to 64 simultaneous conferees
[0220] Dialogic DCB/960: Supports up to 96 simultaneous conferees
[0221] If the telephony server is installed without a conferencing adapter, the VA platform software will still function, but the call conferencing feature will not be available.
[0222] Typical Configurations
[0223] As shown in FIG. 12 , the following telephony hardware is recommended to support a single ISDN PRI link, which can handle 23 simultaneous calls:
[0224] 1 D/240PCI-T1 Adapter 210
[0225] 1 D/320SC Voice Resource Adapter 212
[0226] 1 DCB/320 Conferencing Adapter 214
[0227] 1 CTBUS to SCBus Connector 216
[0228] 2 SCBus ribbon cables 218
[0229] As shown in FIG. 13 , to support two ISDN PRI links, which can support 46 simultaneous calls, the following telephony hardware is recommended:
[0230] 2 D/240PCI-T1 Adapters 220 a , 220 b
[0231] 1 D/640SC Voice Resource Adapter 222
[0232] 1 DCB/640 Conferencing Adapter 224
[0233] 1 CTBUS to SCBus Connector 226
[0234] 2 SCBus ribbon cables 228 a , 228 b
[0235] Installing the Telephony Hardware and Software
[0236] Before the VA platform is installed, the recommended telephony hardware and software should be first installed and configured.
[0237] Installing the Telephony Hardware
[0238] In the machine or machines that have been designated telephony servers for the VA platform, the recommended telephony cards should be installed according to the manufacturer's instructions. When installing the Dialogic D/240PCI-T1 card(s), be set the Bus ID rotary switch to the proper value. In systems with a single card, the card's rotary switch should be set to ‘1’. In multi-card systems, the rotary switch should be set to a different number for each card, starting with ‘1’ and progressing sequentially.
[0239] Installing the Dialogic DNA 3.2 Software
[0240] After installing the Dialogic hardware in the telephony server(s), it is recommended that version 3.2 of the Dialogic Native Architecture (DNA) software be installed. When installing DNA 3.2, options that should be selected to ensure proper support for the VA platform are as follows:
[0241] When starting the DNA 3.2 Install Shield, select the Complete Install option.
[0242] 1. As shown in FIG. 14 , on the Custom Component Selection screen 230 , the following components should be selected for installation:
[0243] Dialogic Core Drivers, Firmware, & Configuration Files 232
[0244] Springware Development Library 234
[0245] Springware TAPI Service Provider 236
[0246] Online Documentation 238
[0247] ISDN Package 240
[0248] GlobalCall API Package 242
[0249] 2. On the ISDN Protocol Selection Screen, select the ISDN Protocol(s) recommended by the local telephone service provider. (Consult the local provider for the specific protocols needed.)
[0250] 3. As shown in FIG. 15 , on the GlobalCall Feature Selection screen, the GlobalCall ISDN option 246 should be selected.
[0251] Configuring the Dialogic Hardware
[0252] During the installation of the VA platform software, Dialogic-specific data files will be modified by the installation routine. For this reason, there is no need to configure the Dialogic boards before installing the VA platform. The Dialog configuration steps necessary after installing the VA platform are discussed.
[0253] Installing Nuance 6.2.1
[0254] In the preferred embodiment, Nuance 6.2.1 is installed on each machine that will be used in the VA platform server set. The Nuance 6.2.1 installation media contains five separate software packages, which should be installed on each system in the following order:
[0255] 1. Nuance 6.2.1 Core Software
[0256] 2. Dialog Optimizer Beta 1)
[0257] 3. Java Plug-In (Version 1.1.2)
[0258] 4. Nuance Grammar Builder (Beta 1)
[0259] 5. Foundation Speech Objects (Beta 1)
[0260] More detailed instructions on installing the Nuance packages can be found in the Nuance documentation that accompanies the installation media.
[0261] Installing AcuVoice TTS
[0262] In the preferred embodiment, Version 3.02 of the AcuVoice Speech Synthesis software should be installed on each system in the server set. Install the software according to the documentation included with the product.
[0263] Installing Microsoft Outlook 2000
[0264] In the preferred embodiment, all VA platform servers running a VA application should have Outlook 2000 installed on them. The Outlook software is used not by a regular user but by the platform itself to communicate with the Exchange server. As shown in FIG. 16 , at the Feature Selection Pane 250 , the Collaboration Data Objects option 252 should be selected. When installing Outlook 2000, perform the following steps to ensure selection of the proper version:
[0265] 1. Choose a Custom Install from the main selection menu
[0266] 2. On the Features screen, right-click the box next to each Node other than Microsoft Outlook for Windows. From the drop down menu, select Not Available.
[0267] 3. Ensure that the Microsoft Outlook for Windows node is marked as Run From My Computer.
[0268] 4. Expand the Microsoft Outlook Node, right-click the box next to Collaboration Data Objects 252 , and choose Run From My Computer.
[0269] Creating the ConitaVA User Account
[0270] By default, all of the VA platform server processes run under the domain user account “ConitaVA.” Before configuring Microsoft Exchange or installing the VA platform, this account needs to be created on the domain in which the VA platform server(s) will be running. The account should be a member of the Administrators group. The ConitaVA user name is not hardwired into the VA platform software, so the administrator can, if desired, create a different account name under which the services will run. The Install Shield application for the platform software will use ConitaVA as a default, so the administrator should be sure to enter the proper user name if a different account is to be used.
[0271] Configuring the Microsoft Exchange Server
[0272] In the preferred embodiment, organizations installing the VA platform will already be using Microsoft Exchange for their regular email and communication services. In such environments, the existing Exchange server and its user accounts will likely continued to be used, with the VA services added on to them. In some situations, however, a new Microsoft Exchange platform may be installed along with the VA platform. If so, the Exchange server should be fully installed and configured according to Microsoft's documentation before installing the VA platform software.
[0273] The default VA application maintains only a small amount of information about each of its users, and the majority of user management functions are performed through the standard Microsoft Exchange interfaces. For this reason, it is recommended that Microsoft Exchange accounts be set up for each person who will also be using the VA application. New users can be added and old users can be removed after the VA platform is installed and in operation.
[0274] Creating ConitaVA as a Service Account Administrator
[0275] In the preferred embodiment, in order for the VA platform services to have access to the necessary Microsoft Exchange interfaces, the ConitaVA user account should be given permissions as an Exchange Service Account Administrator. This configuration is performed through the Microsoft Exchange Administrator application.
[0276] Preparing Fax Services
[0277] If the VA platform will support fax services, then the fax provider software should be prepared before installing the VA platform. In the preferred embodiment, the VA platform supports the following two separate fax services, Facsys and Jfax.
[0278] Installation Overview
[0279] When installing the software for a VA implementation, an administrator should perform three different types of installations:
[0280] VA Server Install, which installs the application components on a system that will be part of the VA server set.
[0281] VA Exchange Administrator Extension, which is installed on the Microsoft Exchange server. This package includes the add-in interface that will be used to manage VA users from within the Exchange Administrator framework.
[0282] VA Outlook Client, which installs the VA add-in for Microsoft Outlook. This allows VA users to configure their Virtual Assistants from within a standard Outlook interface. This installation should be performed on the desktop systems for each person who will have a VA account.
[0283] There are two additional types of installations that can be performed if needed within a particular environment:
[0284] VA Application Developer Workstation, which is used to install the VA Studio and other application development components on a programmer's workstation. This package is needed only if a developer will be writing custom VA applications at the site.
[0285] VA Administration Station, which is used to install the VA Management Console on an administrator's workstation. The VA Management Console will already be installed along with the VA platform software on the systems that make up the VA server set. The Administration Station install is useful, however, for an administrator who wishes to manage the server set from a remote system.
[0286] Installation Media
[0287] Three different pieces of media can be used for installing the VA platform software. These CDs/floppy disks and the types of installs for which they are used are listed in the table below:
[0000]
CD-ROM Used
Installation Type
VA Platform CD
VA Server
VA Administration Station
VA Application Developer
VA Exchange CD
VA Exchange Administrator Extension
VA Outlook Client Floppy Disk
VA Outlook Client
[0288] Installation Procedure
[0289] In the preferred embodiment, the general process for installing and configuring a full VA platform implementation is as follows:
[0290] 1. Prepare the site for installation.
[0291] 2. Install the VA platform software on the Server Set Controller Node
[0292] 3. Install the VA platform software on each secondary node, if using a multi-system implementation
[0293] 4. Install the VA Exchange Administrator Extension on the Microsoft Exchange Server
[0294] 5. (Optional) Install an Administration Station and/or VA Application Developer's platform
[0295] 6. (Optional) Install the VA Exchange Administrator Extension on a remote Exchange administration station
[0296] 7. Configure the platform to run one or more VA applications
[0297] 8. Create VA user accounts with through the Exchange Administrator interface
[0298] 9. Distribute and/or install the Outlook Client component on the workstations of all VA users
[0299] Installing in Stages
[0300] In many situations—particularly when installing a VA server set for the first time—it may be desirable to install the platform servers in stages. In such a procedure, a single node with all the VA software is installed, configured to run a single VA application, and tested to see whether the application functions correctly—first over the system speakers and then over a phone line. Then, additional servers can be added to the server set until the full installation is complete.
[0301] For an installation in stages, the following procedure is recommended:
[0302] 1. Install the Server Set Controller Node software package on a single server
[0303] 2. Install the VA Exchange Administrator package on the Microsoft Exchange Server
[0304] 3. Configure the single VA platform server to run a VA application using a sound card interface
[0305] 4. Create one or two VA user accounts for testing purposes
[0306] 5. Test the application to be sure it functions correctly
[0307] 6. Remove the Sound Card Engine and replace it with a Dialogic Telephony Engine
[0308] 7. Test the application to be sure it functions over the phone lines
[0309] 8. Once the first server is functioning properly, add in each additional node in succession
[0310] 9. Create VA user accounts
[0311] 10. Distribute and/or install the Outlook Client component on the workstations of all VA users
[0312] 11. Bring the full VA platform online for general use
[0313] Calculating Disk Space Requirements
[0314] The amount of free disk space recommended to install the VA platform components on a server depends on the type of installation chosen for the system. Approximate space requirements are listed in the table below:
[0000]
Approximate
Space
Installation Type
Recommended
Server Set Controller Node plus MSDE
200 MB
Database
Server Set Controller Node without MSDE
100 MB
Database
Secondary Node
100 MB
Microsoft Exchange Administrator Extension
5 MB
Administration Station
10 MB
Application Developers Workstation
10 MB
[0315] The disk space requirements are for the VA platform software only. They do not include the amount needed for prerequisite packages such as Nuance and AcuVoice.
[0316] On the Server Set Controller Node, it is recommended that an additional 1 GB of free space be available for the storage of logs and temporary files during VA platform operation. An MSDE or SQL Server database is recommended by the VA platform to store configuration and log data. To be installed without the MSDE database, a Server Set Controller Node should already have either MSDE or SQL Server installed.
[0317] While only 100 MB is recommended for the initial installation of the VA platform software, in the preferred embodiment, because the VA platform software stores temporary speech and log files on the Server Set Controller Node during execution, the amount of disk space used can grow very quickly. It is recommended that there be one (1) GB of free disk space on the Server Set Controller Node in order to store a full set of speech and log data. For systems with smaller capacity, the amount of temporary data stored can be reduced, but such restrictions will limit the ability of an administrator to monitor the platform and track errors.
[0318] VA Platform Server Installation
[0319] When setting up a VA implementation, the first installation is the VA Server install. This installation should be performed first on the server that will be the Server Set Controller Node and then on each secondary server. Before beginning the VA platform installation, if a multi-node server set will be installed, identify which server will be the Server Set Controller Node
[0320] Installing the Server Set Controller Node
[0321] On the server that will be the controller node, perform the following steps to install the VA platform software:
[0322] 1. Insert the VA Platform CD in the CD-ROM Drive. The Install Shield application executes automatically.
[0323] 2. Read the introduction and license screens, clicking Next when finished. The Setup Type selection screen will appear.
[0324] 3. Select VA Server from the setup type list box and click Next. The Select Components screen will be displayed.
[0325] 4. Select the “Yes, this is the Serverset Controller” option and click Next.
[0326] The next screen will provide a prompt to select the directory into which the VA platform files will be installed. By default, this directory will be c:.backslash.Program Files.backslash.Conita Virtual Assistant.
[0327] To keep the default destination directory, click Next.
[0328] To change this directory, click Browse and select a new destination, then click Next.
[0329] 5. The next screen will ask to install the MSDE database. Select either yes or no, based on the following criteria:
[0330] Select No only if the MSDE database software or Microsoft SQL Server is already installed on the server. Click Next to move to the user account screen.
[0331] Select Yes if neither MSDE or Microsoft SQL Server is installed.
[0332] 6. If Yes is selected to install MSDE, there will be a prompt for the directory in which the database should be installed. By default, this directory is c:.backslash.Program Files.backslash.Conita Virtual Assistant.backslash.MSSQL7.
[0333] To accept the default directory, click Next.
[0334] To change the directory, click Browse, select a new directory, and click Next.
[0335] 7. After the database information is selected, the Enter Account Information screen will be displayed.
[0336] 8. On the Account Information screen, the username and password for the NT account under which the VA software will run should be entered. By default, this account will be named ConitaVA and should have already been configured on the server and/or domain before the installation began. Click Next to continue.
[0337] 9. The next screen will provide a prompt for entry of the password for the Conita VA service account. Enter the proper password and click Next.
[0338] 10. The next screen will provide a prompt for the name of the Windows NT domain to which the service account belongs. Enter this domain name and click and click Next.
[0339] Note: All VA servers in a server set and the Microsoft Exchange server with which they will communicate should be located in the same domain.
[0340] 11. The final interactive screen of the installation process will prompt the selection of the Program Folder in which the icons for the VA platform software are to be installed. Change the folder's name if desired, then click Next to begin the installation.
[0341] In most cases, no reboot is recommended after the VA Server installation. If, however, one or more system files were locked by other applications while the installation routine was running, a reboot of the system will be recommended to complete the VA installation, and a prompt will be provided to perform the reboot.
[0342] Installing Additional VA Server Nodes
[0343] The process for installing the VA software on secondary servers is very similar to that for Server Set Controller Nodes, but there will be no prompt to install the MSDE database because a database is recommended only on the controller node.
[0344] The full procedure for the VA Server install an a secondary node is as follows:
[0345] 1. Insert the VA Platform CD in the CD-ROM Drive. The Install Shield application should execute automatically.
[0346] 2. Read the introduction and license screens, clicking Next when finished. The Setup Type selection screen will appear.
[0347] 3. Select VA Server from the setup type list box and click Next. The Select Components screen will be displayed.
[0348] 4. Select the “No, this is not the Serverset Controller” option and click Next.
[0349] 5. The next screen will provide a prompt to select the directory into which the VA platform files will be installed. By default, this directory will be c:.backslash.Program Files.backslash.Conita Virtual Assistant.
[0350] To keep the default destination directory, click Next.
[0351] To change this directory, click Browse and select a new destination, then click Next.
[0352] 6. On the Account Information screen, enter the username and password for the NT account under which the VA software will run. By default, this account will be named ConitaVA and should have already been configured on the server and/or domain before the installation began. Click Next to continue.
[0353] 7. The next screen will provide a prompt to enter the password for the Conita VA service account. Enter the proper password and click Next.
[0354] 8. The next screen will provide a prompt for the name of the Windows NT domain to which the service account belongs. Enter this domain name and click and click Next. Note: All VA servers in a server set and the Microsoft Exchange server with which they will communicate should be located in the same domain.
[0355] 9. The final interactive screen of the installation process will provide a prompt to select the Program Folder in which the icons for the VA platform software are to be installed. Change the folder's name if desired, then click Next to begin the installation.
[0356] In most cases, no reboot is recommended after the VA Server installation. If, however, one or more system files were locked by other applications while the installation routine was running, the system will have to be rebooted to complete the VA installation. In such a case, there will be a prompt to perform the reboot.
[0357] Troubleshooting a VA Server Installation
[0358] The VA platform Install Shield routine generates a log file that is useful for diagnosing a failed installation. The full path to this file is c:.backslash.Program Files.backslash.Conita Virtual Assistant.backslash.Log.backslash.ConitaVAInstallLog.txt. In case of warning or error messages during an install, the log file should be checked first to see whether it contains a more detailed message.
[0359] Configuring the Platform after an Installation
[0360] Configuring IIS on the Controller Node
[0361] During the installation of the VA platform software on the Server Set Controller Node, the Install Shield routine will create two new subdirectories under c:.backslash.inetpubt.backslash.wwwroot. These directories contain a web-based tool used for managing the VA platform logs. Although the Install Shield creates these directories, perform the following steps to configure the virtual directories and security permissions for the files.
[0362] 1. Create two virtual directories under the default web sites and point them to the actual directories created by the install.
[0363] 2. Give the two virtual directories read and script access.
[0364] 3. Make default.htm the default document for both directories.
[0365] 4. Remove anonymous access to the two virtual directories.
[0366] 5. Enable Windows NT Challenge/Response access to the virtual directories.
[0367] Set access permissions on the two actual directories to allow access only to the user account(s) who will be functioning as an administrator for the VA platform.
[0368] Installing the VA Exchange Administrator Extension
[0369] For all sites that will be running the default VA application, the administrator should install the VA Exchange Administrator Extension package on the Exchange server that will be used with the VA platform. This package inserts a custom add-in into the Microsoft Exchange Administrator application. The add-in is used to manage the Exchange accounts that can be accessed through the Virtual Assistant application. In most cases, the VA platform software will be installed in an environment that has an existing Microsoft Exchange server in use. In some circumstances, however, an administrator may be installing Exchange fresh along with the VA software. In such a case, the Exchange server should be fully installed and configured before attempting to install the VA extensions.
[0370] In the preferred embodiment, the Microsoft Exchange server software runs on a separate machine from the VA platform software. At smaller sites, it is possible for Exchange and the VA platform to occupy the same server.
[0371] Before Beginning
[0372] Before beginning the installation of the VA Exchange Server Extension package, the following tasks should have been completed:
[0373] The Microsoft Exchange server on which the VA extensions will be installed has been fully installed and configured.
[0374] An Exchange administrative user's account has been set up for the person who will act as the VA administrator.
[0375] Regular Exchange user accounts have been set up for each person who will be a Virtual Assistant user.
[0376] Before beginning the installation, the Exchange organization, site, and container to which the extensions will be added should be determined, as well as the name of the Add-In shared directory for the Exchange server.
[0377] Installing the VA Extensions on an Exchange Server
[0378] The process for installing the VA extension on a Microsoft Exchange server is as follows:
[0379] 1. Insert the VA Exchange Server Extension CD in the server's CD-ROM drive.
[0380] 2. Read the introduction and license screens, clicking Next when finished.
[0381] 3. On the Setup Type screen, choose Exchange Server and click Next.
[0382] 4. On the Exchange Server Name screen, enter the name of the server on which the extensions are being installed. Click Next.
[0383] 5. On the Exchange Organization screen, enter the name of the organization to which the VA extensions are being added. Click Next.
[0384] 6. On the Exchange Site screen, enter the name of the site to which the VA extensions are being added. Click Next.
[0385] 7. On the Exchange Add-ins Share screen, enter the name of the shared directory under which Microsoft Exchange add-Ins are stored. By default, this directory is named “Add-Ins.” Click Next.
[0386] 8. On the Exchange Container Screen, enter the name of the container in which the VA user accounts will be held. By default, this container is named “Recipients,” but it may have been changed If the Exchange server has been customized. Click Next.
[0387] 9. On the Exchange Extension Display Name screen, enter the name to be displayed for the VA Add-Ins node. (This node will appear under the Add-Ins folder in the Exchange Administrator GUI.) By default, the display name will be “Virtual Assistant User Administration.” Click Next.
[0388] 10. On the Virtual Assistant Administrator Alias screen, enter the Exchange alias for the VA administrator user. By default, this user name is “ConitaVA,” but a different account name for administrative user may have been chosen. Click Next.
[0389] 11. The final interactive screen of the installation process will prompt the selection of the Program Folder in which the icons for the VA User Administrator software will be installed. Change the folder's name if desired, then click Next.
[0390] At this point, the automated portion of the install will begin. Once the Install Shield has finished copying the VA files to the system, there will be a prompt to click Finish to end the installation.
[0391] Installing the Exchange Extensions on an Administrative Station
[0392] In some environments, an administrator may have installed the Microsoft Exchange Administrator application on a system other than the Exchange server itself (that is, on a system used to administer Exchange remotely). The VA Exchange extensions can also be installed on this administrative station to allow for remote VA management. Note: Before the VA extensions can be installed on an administrative station, they should first be installed on the Exchange Server itself.
[0393] The process for installing the VA extensions on a remote administrative machine requires fewer user-input steps than the full Exchange Server install:
[0394] 1. Insert the VA Exchange Server Extension CD in the system's CD-ROM drive. The Install Shield application should execute automatically.
[0395] 2. Read the introduction and license screens, clicking Next when finished.
[0396] 3. On the Setup Type screen, choose Exchange Administrator Only and click Next.
[0397] 4. The next screen prompts for the directory in which the VA Extension files will be installed. Accept the default or select a new directory, then click Next.
[0398] 5. On the Virtual Assistant Administrator Alias screen, enter the Exchange alias for the VA administrator user. By default, this user name is “ConitaVA,” but a different account name for administrative user may have been chosen. Click Next.
[0399] 6. The final interactive screen of the installation process will prompt the selection of the Program Folder in which the icons for the VA User Administrator software will be installed. Change the folder's name if desired, then click Next.
[0400] Uninstalling the VA Extensions
[0401] To remove the VA Extensions from the Exchange Server, use the Add/Remove Programs function under Windows NT's Control Panel. The uninstall routine will remove the Virtual Assistant tab from the Recipients Properties dialog.
[0402] Installing the VA Outlook Add-In
[0403] Before users can begin logging into their Virtual Assistants, the VA Outlook Add-In should be installed on their desktop workstations. This package adds a configuration interface to the users' Microsoft Outlook applications that will be used to personalize the settings for the Virtual Assistants.
[0404] The installation media makes the VA Outlook Add-In install program available in two forms:
[0405] A regular Install Shield.file. Stored on a floppy diskette, this Install Shield can be executed on an individual machine or used with automatic software distribution systems.
[0406] A self-extracting ZIP file. Small in size (820 KB), the self-extracting ZIP is designed to be transmitted over email systems. When executed, it unpacks the recommended installation files and runs the install, which requires no user input.
[0407] Installing an Administration Station
[0408] If desired, an administrator can install the VA Management Console on a machine separate from the VA platform software. Such an administrative station advantageously allows the VA platform to be managed remotely over the network. This installation installs only the basic components needed to run the MMC Snap-In console and to communicate with the VA Server Manager process on the Server Set Controller Node.
[0409] To install an administration station, perform the following steps:
[0410] 1. Insert the VA Platform CD in the CD-ROM Drive. The Install Shield application should execute automatically.
[0411] 2. Read the introduction and license screens, clicking Next when finished. The Setup Type selection screen will appear.
[0412] 3. Select VA Administration Station from the Setup Type list box and click Next.
[0413] 4. The next screen will prompt to select the directory into which the VA platform files will be installed. By default, this directory will be c:.backslash.Program Files.backslash.Conita Virtual Assistant.
[0414] 5. The final interactive screen of the installation process will prompt to select the Program Folder in which the icons for the VA platform software are to be installed. Change the folder's name if desired, then click Next.
[0415] Installing a VA Application Development System
[0416] If programmers will be developing customized VA applications, then an application development system may need to be installed. This package installs the VA Studio and other development tools. Although the Application Development software can be run on the same server as the VA platform, in most cases, the development environment should be installed on a separate system and the custom applications “published” to the VA platform when they are completed.
[0417] To install a VA application development system, perform the following steps:
[0418] 1. Insert the VA Platform CD in the CD-ROM Drive. The Install Shield application should execute automatically.
[0419] 2. Read the introduction and license screens, clicking Next when finished. The Setup Type selection screen will appear.
[0420] 3. Select VA Application Development from the Setup Type list box and click Next.
[0421] 4. The next screen will prompt the selection of the directory into which the VA platform files will be installed. By default, this directory will be c:.backslash.Program Files.backslash.Conita Virtual Assistant.
[0422] To keep the default destination directory, click Next.
[0423] To change this directory, click Browse and select a new destination, then click Next.
[0424] 5. The final interactive screen of the installation process will prompt the selection of the Program Folder in which the icons for the VA platform software are to be installed. Change the folder's name if desired, then click Next.
[0425] Overview of the VA Management Console
[0426] As illustrated in FIG. 17 , the VA Management Console 260 allows an administrator to view and manage all the VA components running in a server set. This interface is implemented as a snap-in for the Microsoft Management Console (MMC) framework, which provides a consistent interface for application administration. Based on the Microsoft Windows Explorer paradigm, the VA Management Console includes a tree view of system components on the left side of the screen 262 and an information panel on the right 264 . Highlighting a component in the tree view will cause its configuration interface to appear in the right-hand pane. Right clicking on a component will open a pop-up menu listing additional functions such as viewing properties, adding new components, and deleting existing components. In a multi-node server set, the VA Management Console will be run only on the Server Set Controller Node.
[0427] Launching the VA Management Console
[0428] To launch the VA Management Console, select Start>Programs>Co-nita Virtual Assistant>Conita Management Console.
[0429] If the desktop icon is deleted, the VA Management Console can be launched by executing the MMC framework and loading the VA snap-in. To do so, use the following procedure:
[0430] 1. From the Start Menu, select Run.
[0431] 2. In the Run dialog, type “mmc” and click OK.
[0432] 3. From the MMC's Console menu, select Add/Remove Snap-In. The Add Snap-In dialog will open.
[0433] 4. Click the Add button. The Add Standalone Snap-In dialog will open.
[0434] 5. From the list of available snap-ins, choose the VA Serverset Manager and click OK. The Select Server dialog will be displayed.
[0435] 6. Click the Select button and choose the server on which the VAServerManager process is running (i.e. the Server Set Controller Node).
[0436] 7. Click Finish to close the Select Server Dialog and OK to close the Add/Remove Snap-In dialog.
[0437] The VA Management Console snap-in will now be displayed within the MMC. If the VA Serverset Manager snap in does not appear in the Add Standalone Snap-In dialog, it is likely that the VAServerManager service is not running. Start the VAServerManager service (through the Control Panel>Services interface) and try adding the snap-in console again.
[0438] Initial Configuration Tasks
[0439] When the VA platform is first installed, the administrator will need to perform the following tasks to configure the platform and launch the first application:
[0440] 1. Configure General Server Set Information
[0441] 2. Add the Server Set Controller Node to the list of managed servers
[0442] 3. (For multi-server platforms) Add secondary nodes to the list of managed servers
[0443] 4. Create an application instance for the Conita VA application
[0444] 5. Start the VA application services for the platform
[0445] 6. Test the application to ensure it is running correctly
[0446] 7. Configure alerts for the VA platform
[0447] 8. Set any TTS Dictionary entries that are known to be needed
[0448] Each of these tasks is discussed in detail below.
[0449] Configuring the General Server Set Information
[0450] The first configuration task to be performed within the VA Management Console is to set the general information for the server set. To do so, as shown in FIG. 18 , expand the VA Manager 270 and Configuration 272 folders in the component tree, then click the General Information node 274 . The general information form 276 will be displayed in the right-hand pane. In this form, enter the following information:
[0451] Exchange Server 280 : The machine name of the Microsoft Exchange Server with which the VA applications will communicate.
[0452] Company Name 282 : The name of the organization implementing the VA
[0453] Site Name 284 : The name of the site at which the VA platform is located. (This field is used to distinguish platforms at organizations that may be running more than one set of VA servers.)
[0454] Conita License Number 286
[0455] Nuance License Number 288 : This key, which is custom generated by Nuance for each organization, should be provided with the Nuance software.
[0456] Adding and Removing Servers
[0457] When the VA platform software is first installed, no servers will be configured. One of the first configuration tasks is adding one or more servers to the set. After the system is up and running, servers may need to be added or removed to expand the capacity of the server set or to replace a failing system.
[0458] After an installation, the Server Set Controller Node should be added to the list of managed servers. Then, if a multi-platform implementation is being used, add each of the secondary servers. Note: The process for adding a server is the same for the controller node and secondary nodes.
[0459] Adding a Server
[0460] Before a server can be added to the set controlled by the VA Management Console, it should have the VA platform software installed, and its VA Manager service should be started.
[0461] Note: The VA Manager process is registered as an auto-starting NT service by the install routine. If, however, the VA Manager service has been stopped on a system, it can be started using the Control Panel>Services interface. Unlike other VA processes such as VA Engines and Recognition Servers, the VA Manager service is started through the Windows NT Services interface, not through the VA Management console.
[0462] To add a server to the VA server set, use the following procedure:
[0463] 1. Expand the VA Manager node in the component tree (if unexpanded).
[0464] 2. Right-click the Server Set node. A pop-up menu will appear.
[0465] 3. From the pop-up menu, select New>Server. The Select Computer dialog will open.
[0466] 4. From the dialog's list, select the server to be added and click OK. A Logon dialog will open.
[0467] 5. Enter the Username and Password for the VA user for the server being added, and then click OK.
[0468] If an error message is received when attempting to add a new server to the server set, check the following:
[0469] The VA Manager service is running on the server to be added
[0470] The correct name and password for the VA user was entered
[0471] The ConitaVA user account has been properly created for either the domain as a whole or for the server being added
[0472] Removing a Server
[0473] To remove a server from the server set, right-click the server's node in the component tree and select Delete from the pop-up menu.
[0474] Configuring Applications
[0475] When the VA Platform is first installed, no applications are registered for execution. After adding all the servers to the server set, the next task is to create one or more applications. Periodically, additional applications may be needed to support new users.
[0476] The VA application, which is delivered on the platform installation media, is the application that will be used for most VA implementations. Some users, however, may elect to configure multiple instances of the VA application, or install other custom-written applications. The basic process for adding an application instance is the same, be it for the VA application or for a custom VA application.
[0477] Application Requirements
[0478] In order to be created and executed, each VA application requires a set of associated service processes and a publication file.
[0479] Associated Service Processes
[0480] Each application instances requires four different types of service processes to be running:
[0481] One or more VA Engines (on which the application will run). Each VA Engine will support a single active telephone call; a Virtual Assistant platform that supports multiple simultaneous callers will generally have one VA Engine per telephone channel.
[0482] One or more Text-to-Speech (TTS) servers for translating text into voice output
[0483] One or more Recognition Servers for translating voice input into text One VA Server process, which monitors users' mailboxes and notifies them when events occur, such as a message being received or a task being assigned. Note: A VA Server process is recommended only for applications that support event notification functionality. The default VA application uses a VA Server process, but a custom application may not require one.
[0484] Each of these recommended server processes could be created separately and then associated with the application instance. The VA Management Console, however, provides a mechanism for creating these processes in one batch while configuring the application.
[0485] The Publication File
[0486] A Virtual Assistant Publication (.vapub) file is an archive that holds the various source files that make up an application. These files include the following:
[0487] The application code executed by the VA Engine
[0488] A “grammar” containing the words and phrases recognized by the application
[0489] The recorded prompts and other sound files used by the application
[0490] A vapub file is generated by the VA application developer using the Service Creation Environment and then uploaded to the VA platform.
[0491] Part of the process of creating a new application instance is “publishing” its vapub file, meaning that its contents are unpacked and distributed to the appropriate directories on the VA platform servers. At publication time, the grammar is compiled into a format that can be understood by the Speech Recognition software and loaded in the recognition engines.
[0492] These publication functions are performed automatically by the Management Console software when an administrator creates a new application instance. In case of a failure during the publication process, any files created on the platform servers will be rolled back and removed.
[0493] Note: The source files for an application are published to every server in the server set, even if that server does not host any of the service components that will be associated with the application. This blanket-distribution allows a new process (such as an additional Recognition Server) to be associated with an existing application without having to republish the application files.
[0494] Creating an Application Instance
[0495] To create a new application instance (including the associated processes it will use), follow these steps:
[0496] 1. Expand the VA Management node in the component tree (if unexpanded).
[0497] 2. Right-click the VA Applications node. A pop-up menu will appear.
[0498] 3. From the pop-up menu, select New>Application Instance. The Add Application Instance dialog 290 will open, which is shown in FIG. 19 .
[0499] 4. In the dialog, enter a name for the application instance. It is recommended that the application instance be given a descriptive name, such as Conita VA.sub.—1, that reflects which type of application it is.
[0500] 5. Ensure that all three checkboxes for creating server processes are checked.
[0501] 6. Click OK. The Select TTS Server dialog 292 will open, as shown in FIG. 20 .
[0502] 7. Check the Create new TTS Server box.
[0503] 8. In the Process Name field, enter a name for the new TTS server process.
[0504] 9. From the TTS Server Type drop down box, select the type of TTS server to be created. In the preferred embodiment, the TTS server is AcuVoice, so this will be the only option available in the drop down box. If the system has been customized to support a different TTS server, additional choices may be available.
[0505] 10. Click OK. The Add Recognition Server dialog 294 will open as shown in FIG. 21 .
[0506] 11. Complete the name, target host, and server-type fields, then click OK. The Add VA Engine dialog 296 will appear, as shown in FIG. 22 .
[0507] 12. In the Add VA Engine dialog, enter a name for the new engine.
[0508] 13. From the Select Server drop down box, select the host on which the VA engine will run.
[0509] 14. In the Select Type drop down box, select the type of VA Engine process to be created. In most instances, the Telephony Engine will be selected as the VA Engine type. This engine type processes input and output from the telephone system via a telephony card. The other possible VA Engine type, Sound Card Engine, is used when the Virtual Assistant application will receive input from a microphone and output sound to a system's speakers. The Sound Card Engine can be used to test new applications before connecting them to the telephone system.
[0510] 15. Click OK. The Set Application File dialog 298 will appear, as shown in FIG. 23 .
[0511] 16. In the Path to file field, enter the full path to the vapub file for the application, or, click the Browse button and find the file using the Open File dialog. In the preferred embodiment, the .vapub file for the Conita VA application is located in the following directory:
[0512] % conitava %.backslash.VApplications.backslash.VAOutlook.pub where % conitava % indicates the installation path for the platform software (by default, C:.backslash.Program Files.backslash.Conita Virtual Assistant). For a custom-written VA application, the vapub file will be located in the directory chosen by the developer when he or she published the application to the VA platform.
[0513] After clicking OK, the new application instance and its related server processes will be added to the component tree.
[0514] Creating an Application Instance without Associated Components
[0515] Although the various VA service components recommended for an application will probably create all at once, it is possible to create a VA application instance without associated services and add those components later. To do so, right-click the VA Applications node in the component tree and select New>Application Instance from the pop-up menu. On the initial screen of the Add Application Instance Dialog, make sure that all of the component boxes are unchecked. Although this procedure will create the application instance in the component tree, the application cannot be run until the recommended service processes have been created and associated with it. The steps for manually creating services and associating them with an application are discussed below.
[0516] Removing Application Instances
[0517] To remove an application from the Server Set, use the following procedure:
[0518] 1. In the component tree, right click the node for the application to be deleted. A pop-up menu will open.
[0519] 2. Select Delete from the pop-up menu.
[0520] 3. A dialog box will open, listing all server processes linked to that application and asking whether to delete those processes along with the application.
[0521] Select Yes to delete all server processes linked to the application.
[0522] Select No to retain the linked server processes. (These processes can be deleted manually later if necessary)
[0523] Select Cancel to abort the delete operation
[0524] Creating Processes Manually
[0525] Although an administrator most likely will use the Create Application feature mechanism to create VA Engine, TTS Server, and Recognition Server processes, a process can be created manually.
[0526] Manual creation can be used to associate additional processes with an existing application. An application that is running slowly, for example, may need to have a second Recognition Server associated with it to speed up the processing of recognition requests. By manually creating and associating the new process, the administrator avoids having to create the entire application from scratch.
[0527] To create a new process, perform the following steps:
[0528] 1. In the VA Management Console's component tree, right click the node for the server on which the process is to be created. A pop-up menu will open.
[0529] 2. Select New>Process from the menu. The Add Process Dialog 296 will open, as illustrated in FIG. 24 .
[0530] 3. In the Name field, enter a name for the new process.
[0531] 4. From the Type combo box, select the type of process to be created. The default set of process types are listed in the table below:
[0000]
Type
Description
Accuvoice TTS Server
The service that performs Text-To-Speech
translation
Nuance RecServer
The service that recognizes speech into text
Nuance Resource
The Resource Manager is created
Manager
automatically by the platform when a VA
application instance is created.
Nuance License Manager
Recommended by the Nuance Manager
RecServer, the License Manager process
supplies a valid license to the recognition
server process
External App
A custom-written VA application
Telephony Server
A COM object server that provides an interface
between the VA platform and the telephony
hardware APIs
[0532] 5. From the Associate with application instance combo box, select the name of the application with which the process is to be associated. To create a global process, select “No Application.”
[0533] 6. Click OK. The new process will be added to the component tree
[0534] Starting VA Application Services
[0535] For a VA application to be able to handle incoming calls, all of its related services should be running. An administrator has the option to configure each service as “auto-start,” which indicates that when a system is rebooted the VA Server Manager will automatically attempt to start all of its registered services.
[0536] There are times, however, when a VA administrator will need to start or stop services manually. These situations include the following:
[0537] When a new application has been added to the system and needs to be started for the first time
[0538] When the platform needs to be brought down for maintenance
[0539] When a process has been terminated due to an error and could not be automatically restarted by the VA Server Manager
[0540] An administrator can choose to start or stop all of services running on a platform, all of an individual application's services, or each service individually.
[0541] Configuring Auto-Start Services
[0542] When a VA service process is created (either manually or through the creation of a new application instance), its auto-start property is by default set to False, indicating that the service will not automatically be started by the VA Server Manager at system start-up. If desired, an administrator can change the auto-start property for a service by clicking on the service's node in the component tree and, in the properties page that appears in the right-hand window, checking or unchecking the Auto-Start check box.
[0543] In most instances it will be desirable for all platform processes to be set to auto-start, which will save administrators from having to manually start the services when a server is rebooted. For this reason, it is recommended the Auto-Start option be selected for each associated service after an application is created.
[0544] Starting All Services (Global)
[0545] The global function will attempt to start all of the services currently being used in the server set, including TTS Servers, Recognition Servers, VA Engines, License Managers, and Resource Managers. This function, in effect, starts all the registered applications on the platform and prepares them to receive incoming calls.
[0546] The procedure for starting all services is as follows:
[0547] 1. Right-click the VA Manager node in the component tree. A pop-up menu will open.
[0548] 2. From the menu, select Start All Processes
[0549] Service Process Start Orders
[0550] When a global start-up is performed, all global service processes (such as the Nuance License manager) are started first, and then all per-VA Application processes (such as TTS Server and Recognition Servers) are started. Within these two categories (global and per-application), the order in which services are started is determined by Startup Groups. Based on its dependencies, each process type is assigned to a group, and each group is assigned a number indicating in which order it should be started (from lowest to highest). Each process in a group is started at roughly the same time. The default Startup Order Groups are listed in the table below:
[0000]
Type
Startup Order Group
Telephony Server
1
External App
1
Nuance Resource Manager
2
Nuance License Manager
2
Accuvoice TTS Server
2
Nuance RecServer
3
Sound Card Engine
4
Telephony Engine
4
[0551] As the table indicates, the telephony servers and external application services will be started first, and the two types of VA Engines (sound card and telephony) will be started last. Because a Telephony Engine cannot be started unless its associated TTS Server is already running, the engine is assigned to higher-numbered group than the TTS Server, guaranteeing they will be started in the proper order.
[0552] Starting All Services for an Application
[0553] An administrator can also start services at an application level. This function will attempt to start all the processes associated with a particular application. These processes usually include VA Engines, TTS Servers, and Recognition Servers.
[0554] To start all the services for an individual application, perform the following steps:
[0555] 1. Expand the VA Applications node in the component tree.
[0556] 2. Right-click on the node for the application for which all services are to be started.
[0557] 3. Select Start from the pop-up menu.
[0558] Once an application is started, it will be ready to receive incoming calls.
[0559] When an application is started, the VA Server Manager will first verify that any global services (such as the Nuance License Manager) needed for the application are already running. If a global dependency is not running, none of the application's services will be started and an error message will be displayed.
[0560] Starting Individual Services
[0561] Although in most instances either the global or application start-up functions will be used, at times only a single service may need to be started. To do so, right-click the component to start and select Start from the pop-up menu. As with starting an application, any global processes recommended by the individual service should already be running. Otherwise, the service will fail to start. Note: Alternatively, a service can be started manually by highlighting its name in the component node and clicking the Start (arrow) button on the MMC Snap-In's toolbar.
[0562] Troubleshooting Services that Fail to Start
[0563] To check on the status of a particular service, view its properties display panel. This panel appears in the right-hand window of the VA Management Console GUI when the service's name is clicked on in the component tree. As illustrated in FIG. 25 , the user has highlighted the TestApplicationResourceMgr node, which is the Nuance Resource Manager for the TestApplication application. The properties for the service appear in the right-hand part of the screen.
[0564] On this properties panel, the Process Status field indicates the status of the process. It can have one of the following values:
[0565] Running: The process is running properly
[0566] Stopped: The process has been stopped by an administrator
[0567] Error: The process has failed to start because of an error
[0568] If the process has an Error status, then the code for the error will be displayed in the Error Code field. This error code—a hexadecimal number—indicates the reason for the process's failure. A complete listing of the possible error codes and their meanings is set forth below. If one or more of the processes for an application fail to start, the displayed error code can be looked up to determine the reason for the failure.
[0569] In addition to displaying an error code, a failed process may also list troubleshooting information in the large Process Events text box on its properties panel. One of the most common causes for a component's failure to start is that one of its prerequisite services is not running. A VA Engine, for example, will not start if its TTS Server is not running. A Recognition Server will not start if its License Manager service is not already running. If a particular component has failed to start, make sure that all its associated services are running correctly and, if they are not, attempt to start them.
[0570] Stopping VA Services
[0571] As with starting VA services, the administrator has several options to choose from when shutting down services on the VA platform. When VA services are stopped, the applications will cease execution and no incoming calls can be received.
[0572] Shutting Down Gracefully
[0573] In the preferred embodiment, the method for shutting down a VA platform is to use the Stop All (Graceful) function. This function immediately sets the platform so that it will not receive any new incoming calls, but it does not disconnect any current VA sessions. Once all active sessions are complete, the platform will be shut down.
[0574] To perform a graceful shutdown, do the following:
[0575] 1. Right-click the VA Manager node in the component tree. A pop-up menu will open.
[0576] 2. From the menu, select Stop All (Graceful).
[0577] 3. Provide a prompt to confirm the shutdown command. Select Yes to proceed.
[0578] Shutting Down Immediately
[0579] In some cases, an administrator may need to stop all services on the platform immediately. Doing so will disconnect all current VA sessions and close all the platform's applications. To perform an immediate shutdown,
[0580] 1. Right-click the VA Manager node in the component tree. A pop-up menu will open.
[0581] 2. From the menu, select Stop All (Immediate).
[0582] 3. A prompt will be provided to confirm the immediate shutdown command. Select Yes to proceed.
[0583] Stopping Individual Applications and Services
[0584] The VA Management Console includes functions that allow a particular application or an individual service to be stopped. To do so, perform the following steps:
[0585] 1. Expand the component tree until the node for the application or service to stop is complete
[0586] 2. Right-click the node for the application or service and select Stop from the pop-up menu.
[0587] Configuring Alerts
[0588] The VA platform includes an alert feature that allows the administrator to be paged when selected system errors occur. Such alerts are sent via email pager, and the administrator can configure the type of errors to be monitored and how frequently he or she should be paged. To configure the alerts, double click on the Alerting Setup node under the component tree's Configuration folder. As shown in FIG. 26 , the alert configuration interface 300 will appear in the right-hand frame. In this interface, enter the administrator's pager email address in the Pager Email field 302 and click the Set button, then select the minimum amount of time between pages. It is recommend that an interval is selected (such as 10 minutes) that is long enough to prevent the administrator from being inundated with repeated messages for the same recurring error, but is short enough that the administrator will be informed in case a different error occurs. In the checkbox frame, select the subsystems to be monitored for errors. The Select All and Clear All buttons can be used to select or clear all of the checkboxes at once. If Logon errors is selected, the number of failed logon attempts that should occur before the administrator is notified should be specified. After selecting paging options, click the Test button to have a test message sent to the email pager.
[0589] Using the TTS Dictionary
[0590] By default, the TTS server is configured with pronunciation strings for most common English words. For other words—such as technical terms and proper names—the server uses an algorithm to determine the most likely pronunciation. In many cases, this algorithm may lead to a word's being pronounced incorrectly. For example, the TTS system may pronounce the name Conita as “Co-knit-ah” rather than the correct “Co-night-ah.” The TTS Dictionary feature allows the correction of the TTS's pronunciation of words and phrases. The mechanism works by simple string substitution, that is, whenever the TTS engine encounters a specified string, it will replace it with a more phonetically accurate version before processing the text. An ad ininistrator could, for example, specify that the TTS engine replace all occurrences of the string “Conita” with “Conighta” before translating it to speech. Such a substitution would result in the correct pronunciation of the word.
[0591] Setting TTS Dictionary Entries
[0592] As shown in FIG. 27 to view the current TTS Dictionary entries on the system, click the TTS Dictionary node 304 under the component tree's Configuration folder 306 . The TTS Dictionary display 308 will appear in the right-hand pane. The dictionary should be configured separately for each TTS server. To display the entries for a particular server, click the Select Server button 310 and select the name of the desired TTS server. As illustrated in FIG. 28 , to add a new entry to that server's dictionary, click the Add button. The Dictionary Entry dialog 312 will be displayed. In this dialog, enter the actual spelling of the word or phrase and the replacement string that should be used for a correct pronunciation. By default, all string replacements are not case sensitive. Selecting the Match Case checkbox 314 will make the matching case sensitive. It may take some experimenting to find a replacement string that will result in the proper pronunciation for a word. Use the Play button on the TTS Dictionary display screen to test a particular entry. When this button is clicked, the highlighted en try will be sent to the TTS Server and the resulting speech output played over the server's speakers.
[0593] Managing the VA Database and Call Logs
[0594] The VA Database, which is hosted by the Server Set Controller Node, is used by the VA Server Manager to store call log and platform configuration data. This database is implemented with the Microsoft Data Engine (MSDE). MSDE, which was released with the Microsoft Office 2000 suite, provides access to databases that are compatible with SQL Server 7.0, though with a smaller set of features. The engine does not include an interface such as the SQL Server Enterprise Manager, and it supports a maximum database size of 2 GB (compared to SQL Server's 32 TB). MSDE databases, however, can be read by the SQL Server interfaces, and they can be upgraded to SQL Server databases if increased size is needed.
[0595] Using the VA Management Console to Manage the Database
[0596] Because MSDE does not include its own user interface, most management tasks for the VA Database will be performed through the VA Management Console application. As Included in the console's component tree is a node called Database Manager which, when highlighted, will cause the database management panel 316 to be displayed in the right side of the console window, as shown in FIG. 29 .
[0597] Backing up the Database
[0598] The configuration parameters and user information stored in the database are essential to the operation of the VA platform. For this reason, the database should be regularly backed up. In the Backup frame on the Database Manager panel, the Last Database Backup field indicates when the last backup of the current VA database occurred. It is recommended that the VA database be backed up regularly. The directory in which the database will, be backed up is indicated in the Backup Directory field. To change this, edit the field's value directly or click the browse button and select the new directory from a Browse for Folder dialog. To back-up the VA database, click the Backup button.
[0599] Restoring the Database
[0600] In case of a VA database failure, the database can be restored from a back-up. To do so, in the Restore File field enter the name of the back-up file from which to restore the database (or, click the browse button and choose the filename from an Open File dialog). Then, click the Restore button to begin the restoration.
[0601] Purging Call Logs and Transcriptions
[0602] The VA Server Manager maintains logs and transcriptions for all of the calls processed by the VA platforms. These logs are vital not only for diagnosing problems with the systems but also for performing accounting tasks such as billing departments for VA usage. These stored files, however, can grow quite large, particularly on platforms with many users; the logs and transcriptions should be purged periodically to free up disk space. The frequency with which these purges will need to be performed will depend upon the record-keeping needs of the organization and the amount of disk space available on the VA platform.
[0603] To purge call transcriptions and/or logs, perform the following steps:
[0604] 1. Select either the Purge Transcriptions older than or Purge Logs and Transcriptions older than option button.
[0605] 2. In the Days combo box, indicate how many days to retain transcriptions and/or logs.
[0606] 3. Click the Purge button to purge all outdated transcriptions and/or logs.
[0607] Establishing Maintenance Plans
[0608] 1. Although the database can be backed up and transcriptions and logs can be purged manually, it is usually much more convenient for an administrator to establish a Maintenance Plan, which allows scheduling of regular backup and purge operations. A new Maintenance Plan is added by clicking the Add button inside the Maintenance Plans frame.
[0609] Removing Maintenance Plans
[0610] To remove an unneeded maintenance plan, highlight the plan in the list box and click the Remove button.
[0611] User Administration Concepts
[0612] With the default VA application, all user account management functions are performed through the Microsoft Exchange Administrator interface. The majority of these functions are regular Exchange tasks (such as mailbox maintenance) that are unrelated to the Virtual Assistant application. For the few VA-specific administration tasks that are recommended, the VA Exchange Server Extension installation inserts a custom Add-In to the Microsoft Exchange Administrator application. As illustrated in FIG. 30 , this installation adds a new tab called Virtual Assistant 318 to the Mailbox Properties Dialog 320 for each user. This tab is used to edit the user's VA properties.
[0613] VA User Administration Tasks
[0614] An administrator uses the VA Exchange Add-In to enable and disable VA users, and to assign IDs and PIN's for VA users.
[0615] VA User Account Information
[0616] The Conita VA application requires the following information for each user account:
[0617] User ID, which corresponds to the DNIS number that callers will dial to access a particular user's VA. For example, if John Smith dials 555-1213 to access his Virtual Assistant, then his User ID will be 5551213. In any environment with multiple users, the User ID/DNIS number is essential for identifying which user's Virtual Assistant is being called. When an incoming call is received, the VA application automatically detects the DNIS number and uses it to identify the VA user for which the call is intended. The User ID should be exactly seven digits.
[0618] PIN—In addition to a User ID, each user account requires a Personal Identification Number, which will be entered by the user when he or she dials into the Virtual Assistant. The PIN can be any 4-digit number. The initial PIN for each user is assigned by the VA administrator when he or she sets up the user's account. Users can change their PIN numbers as desired through the Virtual Assistant preferences tab in their Microsoft Outlook application.
[0619] Enabling and Disabling VA Users
[0620] When the VA Exchange Extension package is first installed, the Virtual Assistant tab will be added to each user's mailbox properties dialog, but the user will not be registered with the VA system. Before these users can begin interacting with their Virtual Assistants, the administrator should enable each of them as a VA user. To enable a VA user, perform the following steps:
[0621] 1. In the Microsoft Exchange Administrator application, expand the site and container nodes under which the VA user accounts are located.
[0622] 2. Double click the node for the user that to be enabled as a VA user. Returning to FIG. 31 , the Mailbox Properties Dialog 320 for that user will open.
[0623] 3. Click the Virtual Assistant tab 318 .
[0624] 4. Check the box 322 next to Enable Virtual Assistant (see figure below), then click Apply. The ID and PIN text boxes will become enabled.
[0625] 5. In the ID field 324 , enter the User ID/DNIS number that will be used to access this user's Virtual Assistant account.
[0626] 6. In the PIN field 326 , enter the initial Personal Identification Number that the user will have to enter to access his or her account.
[0627] Note: When setting up user accounts for the first time, all users can be assigned the same PIN (e.g. ‘1111’) and requested that they change it to a new value when they first log in. Users can change their PIN's through the Virtual Assistant properties tab within their Microsoft Outlook applications.
[0628] 7. Click OK to accept the new VA settings for the user.
[0629] Disabling a VA User Account
[0630] To disable a VA user's account, the following steps should be performed:
[0631] 1. In the Microsoft Exchange Administrator application, expand the site and container nodes under which the VA user accounts are located.
[0632] 2. Double click the node for the user to be disabled. The Recipients Properties Dialog for that user will open.
[0633] 3. Click the Virtual Assistant tab.
[0634] 4. Uncheck the box next to Enable Virtual Assistant, then click Apply.
[0635] The ID and PIN text boxes will be greyed out.
[0636] 5. Click OK to accept the changes.
[0637] When a user account is disabled, that user can no longer dial into his or her Virtual Assistant. When a VA user account is disabled, the User ID and PIN are not retained. These properties should be entered again by the administrator if the account is re-enabled.
[0638] Batch Account Enabling and Disabling
[0639] Included with the VA Exchange Extensions is a utility that can be used to enable or disable all of the VA user accounts in a single batch. This utility is most useful for quickly disabling all VA accounts before removing the VA Exchange Extensions from the Exchange Server. Note: When a VA user account is disabled, the User ID and PIN are not retained. These properties should be entered again by the administrator if the account is re-enabled.
[0640] To launch the Enable/Disable utility, select Start>Programs>Conita Virtual Assistant User Administration>Enable/Disable Virtual Assistant. The utility presents two choices, enable or disable:
[0641] If disable is selected, then all users will have their VA accounts disabled
[0642] If enable is selected, then all user accounts will be enabled.
[0643] For these newly enabled accounts, the User ID and PIN numbers will remain undefined and should be set for each user by the administrator.
[0644] An additional task that this utility will perform is repair. If the VA Exchange administrative user is deleted or that user's Contacts folder is corrupted, then users cannot use their VA. However, all the VA information for the VA users is still valid. Creating a new VA Exchange administrative user and selecting the repair in the utility will repair the VA Exchange administrative user's knowledge of VA users, and allow users to access their VA again.
[0645] Setting DCOM Permissions
[0646] At install time, the Virtual Assistant platform software registers the following DCOM objects:
[0647] VADBManager
[0648] VAEngine
[0649] VAExternalApp
[0650] VAManager
[0651] VAServer
[0652] VAServerManager
[0653] VATelephony
[0654] VATextToSpeechAcuVoice
[0655] VATextToSpeechBT
[0656] The security parameters for these DCOM objects are set automatically by the Install Shield. The default values for each of the objects is as follows:
[0657] Access Permissions: Allow access to the ConitaVA user account
[0658] Launch Permissions: Allow launch to the ConitaVA user account
[0659] If necessary for a particular site's security arrangements, a VA administrator can modify the DCOM configuration. However, because setting improper parameters can prevent the VA services from running, such modifications should be made only by an administrator with advanced DCOM experience.
[0660] Because the VA Manager processes should be able to access and launch other VA DCOM objects, the ConitaVA user account (or which ever user account under which the VA processes are running) should have access and launch permissions for all VA objects.
[0661] Resetting DCOM Permissions
[0662] In case the DCOM settings for the VA platform objects are modified, a utility called vladcom is available to reset the objects to their original configuration. This utility is copied to the VA bin directory at install time. To use vladcom to reset the DCOM permissions of VA objects, perform the following steps:
[0663] 1. Open a DOS command line window.
[0664] 2. Change to the c:.backslash.Program Files.backslash.Conita Virtual Assistant.backslash.bin directory.
[0665] 3. Execute the following command:
[0666] vladcom-cf dcomcfg.txt-pf DCOM_progid.txt-id<domain>.backslash.<user>
[0667] Where <domain> is the server's NT domain and <user> is the NT username under which the VA services are running (e.g. “ConitaVA”).
[0668] Securing File System Data
[0669] The VA platform installation routine automatically sets the access permissions for each directory that it creates. The following user accounts are granted Full Control of all the directories under the root install path (by default, c:.backslash.Program Files.backslash.Conita Virtual Assistant):
[0670] Domain Administrator
[0671] Local System Administrator
[0672] System
[0673] ConitaVA
[0674] All other user accounts are granted permission to these directories.
[0675] If a system's security arrangements require it, these permissions can be modified to grant or deny access for other accounts. However, because the ConitaVA account should have access to the VA directories, it should always grant be granted Full Control.
[0676] VA Database Security
[0677] When the VA platform software is installed on the Server Set Controller Node, the installation routine automatically sets the MSDE database (and/or SQL Server, if it is being used instead) to NT Authentication only. The ConitaVA NT account will then be used by the platform software to access the VA database. This setting of authentication is effective at the server-level, not the database level. If other MSDE and/or SQL Server databases are supported on the Controller Node, however, the SQL Server authentication methods may be set for these databases. The VA-established authentication can be modified by performing the following steps:
[0678] 1. In the SQL Server Enterprise Manager, change the authentication method for the entire server to SQL Server authentication
[0679] 2. Change the authentication method for the VA Database to NT Authentication. No matter which method is used for the server-wide authentication, the database-specific method for the VA Database should be NT Authentication.
[0680] Error & Message Codes
[0681] The first three digits of the code indicate which type of message the code represents. These digits can have one of three values, as indicated below:
[0682] 0.times.0 Success Message
[0683] 0.times.4 Informational Mess age
[0684] 0.times.8 Warning Message
[0685] 0.times.C Error Message
[0686] The complete set of possible error codes and their descriptions are listed in the table below.
[0687] Notes:
[0688] The entries in the table are ordered numerically by the code, but the first three digits are ignored. 0x40000034, for example, appears immediately after 0xC00000033.
[0689] This table lists only those errors and messages generated by the VA platform software. The VA Management Console interface, however, will also report messages generated by Windows NT. If an error displayed in the Management Console does not appear in this list, it is likely an NT error.
[0690] Windows NT error codes can be translated using the Error Lookup feature of Microsoft Developer Studio.
[0000]
Message Code
Description
0xC0000001
VAVM ALREADY STARTED
0xC0000002
VAVM ERROR PARSING VADL STRING
0xC0000003
VAVM ERROR PARSING VADL FILE
0xC0000004
VAVM EXTERNAL MODULE NOT FOUND
0xC0000005
VAVM MODULE NAME ALREADY EXPORTED
0xC0000006
VAVM START DISCOURSE NOT SPECIFIED
0xC0000007
VAVM DISCOURSE NOT DEFINED
0xC0000008
TTS NOT INITIALIZED
0xC0000009
TTS NULL STRING
0xC000000A
TTS UNKNOWN TYPE
0xC000000B
AUDIO STREAM NOT DEFINED
0xC000000C
AUDIO STREAM FORMAT NOT SUPPORTED
0xC000000D
AUDIO STREAM OVERFLOW
0xC000000E
TTS RENDER STRING ERROR
0xC000000F
TTS SYNTHESIS FAILED
0xC0000010
WRITE OPERATION FAILED
0xC0000011
VAVM INTERNAL ERROR
0xC0000012
VAVM GETSCRIPTINGHOST FAILED
0xC0000013
VAVM INVALID DISPID FOR NAMESPACE
0xC0000014
VAVM NAMESPACE MEMBER NOT DEFINED
0xC0000015
VAVM INVALID DISPID FOR RECRESULT
0xC0000016
VAVM INVALID TYPE FOR RECRESULT
0xC0000017
VAVM SCRIPT ITEM NAME ALREADY DEFINED
0x40000018
VAVM SHUTDOWN
0x40000019
VAVM REMOTE HANGUP
0xC000001A
VAVM BARGE IN
0xC000001B
VAVM NO ACTIVE CALL
0xC000001C
VAVM RECOGNITION ERROR
0x4000001D
VAVM RECOGNITION UNRECOGNIZED
0xC000001E
SPEECH INITIALIZE ERROR
0xC000001F
SPEECH UNINITIALIZE ERROR
0xC0000020
SPEECH GRAMMAR ERROR
0xC0000021
SPEECH ABORT ERROR
0xC0000022
SPEECH RECOGNITION ERROR
0xC0000023
SPEECH SETPARAMETER ERROR
0xC0000024
TELEPHONY INITIALIZE ERROR
0xC0000025
TELEPHONY NOT INITIALIZED
0xC0000026
TELEPHONY UNINITIALIZE ERROR
0xC0000027
TELEPHONY ANSWER CALL ERROR
0xC0000028
TELEPHONY TERMINATE CALL ERROR
0xC0000029
TELEPHONY PLACE CALL ERROR
0xC000002A
TELEPHONY TRANSFER CALL ERROR
0xC000002B
TELEPHONY INVALID CALLID
0xC000002C
TELEPHONY RECORD ERROR
0xC000002D
TELEPHONY STOP RECORD ERROR
0xC000002E
TELEPHONY PLAY ERROR
0xC000002F
TELEPHONY SETPARAMETER ERROR
0xC0000030
TELEPHONY GETPARAMETER ERROR
0xC0000031
TELEPHONY CHANNEL CLOSED
0xC0000032
PROCESSID OUT OF RANGE
0xC0000033
DELETED PROCESS
0x40000034
VAMANAGER PARAMETER CHANGE
0xC0000035
VAMANAGER PERFMON FAILED
0xC0000036
INSUFFICIENT MEMORY RESOURCES
0xC0000037
COUNTER ARRAY TOO SMALL
0x40000038
INACTIVITY TIMEOUT
0xC0000039
VAVM INITIALIZATION ERROR
0xC000003A
VAVM TOPIC NOT FOUND
0xC000003B
VAVM STARTUP ERROR
0x0000003C
VAVM STARTUP COMPLETE
0xC000003D
VAVM NOT IMPLEMENTED
0xC000003E
VAVM GRAMMAR NOT DEFINED FOR
DISCOURSE
0xC000003F
VAVM SCRIPTING ERROR
0xC0000040
TTS INITIALIZE ERROR
0x40000041
BEGIN CALL
0x40000042
USER LOGIN
0x40000043
END CALL
0x40000044
BEGIN SESSION
0x40000045
END SESSION
0x80000046
TTS TOO MANY CHANNELS
0x80000047
TTS SEND FAILED
0xC0000048
SYSTEM ERROR
0xC0000049
DCOM ERROR
0x0000004A
TTS ABORTED
0x4000004B
TTS CLIENT CONNECTED
0x4000004C
TTS CLIENT DISCONNECTED
0xC000004D
VAMANAGER PROCESS TERMINATED
0x4000004E
VAMANAGER PROCESS STARTING
0xC000004F
VAMANAGER PROCESS FAILED TO START
0xC0000050
TTS UNKNOWN STRING TYPE
0xC0000051
VAVM PROMPT RESOURCE NOT FOUND
0xC0000052
VAVM PROMPT INVALID RESOURCE
0xC0000053
VAVM INVALID PROMPT EXPRESSION
0xC0000054
VAVM INVALID PROMPT RESOURCE
0xC0000055
VAVM NOT SUPPORTED
0xC0000056
VAMANAGER WRITE TO LOG FILE FAILED
0xC0000057
VAMANAGER INVALID COMPONENT ID
0xC0000058
VAMANAGER PROCESS NOT FOUND
0xC0000059
VAMANAGER PROCESS ALREADY EXIST
0xC000005A
VAMANAGER CANNOT DESTROY RUNNING
PROCESS
0xC000005B
VAMANAGER COMPONENT NOT FOUND
0xC000005C
USER ALREADY SELECTED
0xC000005D
USER NOT SELECTED
0xC000005E
USER NOT FOUND
0xC000005F
USER ALREADY EXIST
0xC0000060
USER UPDATE FAILED
0xC0000061
USER CREATION FAILED
0xC0000062
UNKNOWN AUTH METHOD
0xC0000063
USER NOT AUTHENTICATED
0xC0000064
UNKNOWN IDENT METHOD
0xC0000065
DUP IDENT VALUE
0xC0000066
PARAMETER CREATION FAILED
0xC0000067
PARAMETER UPDATE FAILED
0xC0000068
BUFFER TOO SMALL
0xC0000069
PERMISSION DENIED
0xC000006A
DATABASE ERROR
0xC000006B
VASERVER RULE CREATION FAILED
0xC000006C
VASERVER RULEID ALREADY EXIST
0xC000006D
VASERVER RULEID NOT FOUND
0xC000006E
VASERVER USER HAS PENDING REQUEST
0xC000006F
POPMON NOT INITIALIZED
0xC0000070
POPMON ALREADY INITIALIZED
0xC0000071
POPMON RULES ENGINE NOT SPECIFIED
0xC0000072
POPMON DUPLICATE RULE
0x40000073
POPMON USER RELEASED
0xC0000074
POPRULE SYNTAX ERROR
0xC0000075
POPRULE UNDEFINED KEYWORD
0xC0000076
POPRULE WRONG NUM PARAMS
0xC0000077
POPRULE EMPTY RULE
0x80000078
SITEMANAGER SELECTSITE FAILED
0x80000079
SITEMANAGER ADDSITE FAILED
0x8000007A
SITEMANAGER REMOVESITE FAILED
0x8000007B
SITEMANAGER ENUMERATION ERROR
0x8000007C
SITEMANAGER SELECTCOMPUTER FAILED
x8000007D
SITEMANAGER ADDCOMPUTER FAILED
0x8000007E
SITEMANAGER REMOVECOMPUTER FAILED
0x8000007F
SITEMANAGER SETPARAMETER FAILED
0xC0000080
SITEMANAGER CONNECT FAILED
0x80000081
SITEMANAGER SETSITENOTIFY FAILED
0x80000082
SITEMANAGER SELECTPROCESS FAILED
0x80000083
SITEMANAGER ADDPROCESS FAILED
0x80000084
SITEMANAGER PROCESSCOMMAND FAILED
0xC0000085
SITEMANAGER CONNECTLOCAL FAILED
0xC0000086
SITEMANAGER CONNECTREMOTE FAILED
0x80000087
SITEMANAGER ADDUSERNOTIFY FAILED
0x80000088
SITEMANAGER SETUP FAILED
0xC0000089
SITEMANAGER DATASOURCE FAILURE
0x8000008A
SITEMANAGER CONNECTION TIMEOUT
0x8000008B
SITEMANAGER COMPONENTMANAGER FAILURE
0x4000008C
SITEMANAGER VAMANAGER CONNECTION
0xC000008D
APP NOT FOUND
0xC000008E
VAPROCESS NOT STARTED
0x8000008F
UNKNOWN PAGE TYPE
0x80000090
UNKNOWN PAGE KEYWORD
0x80000091
PAGE FILE SYNTAX ERROR
0x00000092
APPLICATION GENERAL SUCCESS
0x40000093
APPLICATION GENERAL INFORMATIONAL
0x80000094
APPLICATION GENERAL WARNING
0xC0000095
APPLICATION GENERAL ERROR
0xC0000096
APPLICATION LOGON FAILED
0x80000097
UNSYNCHRONIZED PARAMETERS
0x80000098
INVALID AUDIO STREAM
0x80000099
AUDIO BUFFER UNDEFINED
0xC000009A
TELEPHONY SET CONTROL ERROR
0x4000009B
COL INVALID INDEX
0x4000009C
COL PROPERTY DOES NOT EXIST
0x4000009D
COL NO MESSAGES
0x4000009E
COL NO PREVIOUS MESSAGE
0x4000009F
COL NO NEXT MESSAGE
0x400000A0
COL NO ATTACHMENTS
0x400000A1
COL NO PREVIOUS ATTACHMENT
0x400000A2
COL NO NEXT ATTACHMENT
0x400000A3
COL NOT MEETING REQUEST
0x400000A4
COL NO RECIPIENT
0xC00000A5
TELEPHONY CONTROL CALL ACTIVE
0xC00000A6
VAVM NO ACTIVE SESSION
0xC00000A7
VAVM INVALID CALL STATE
0xC00000A8
VAVM SESSION TERMINATION
0x400000A9
TELEPHONY BUFFER OVERFLOW
0x400000AA
TELEPHONY BUFFER HIWATER
0x800000AB
PARAMETER DOES NOT EXIST
0x800000AC
EVENTSINK ALREADY DEFINED
0x800000AD
EVENTSINK NOT DEFINED
0xC00000AE
TELEPHONY WAIT FOR CALL ERROR
0x400000AF
EXTERNAL EVENT
0xC00000B0
TELEPHONY CONF TOO BIG
0xC00000B1
TELEPHONY DUPLICATE JOIN
0xC00000B2
TELEPHONY UNKNOWN CONFEREE
0xC00000B3
TELEPHONY TROMBONE ERROR
0xC00000B4
TELEPHONY CONF JOIN ERROR
0x400000B5
VAVM LOG SESSION
0xC00000B6
TELEPHONY STOP WAIT CALL ERROR
0xC00000B7
TELEPHONY CONF DROP ERROR
0xC00000B8
TELEPHONY MUTE CALL ERROR
0xC00000B9
TELEPHONY LISTEN CALL ERROR
0x800000BA
SERVERMANAGER NOT INITIALIZED
0x800000BB
DB ENTRY ALREADY EXISTS
0x400000BC
PROCESS PARAMETERS NOT INITIALIZED
0xC00000BD
TELEPHONY HOLD CALL ERROR
0xC00000BE
TELEPHONY RELEASE HOLD ERROR
0xC00000BF
TELEPHONY ACQUIRE CALL ERROR
0xC00000C0
VADBM CREATE DATABASE FAILED
0xC00000C1
VADBM REGISTRY PARAMETER ERROR
0xC00000C2
VADBM SQL SCRIPT MISSING
0xC00000C3
VADBM SQL SCRIPT ERROR
0xC00000C4
VADBM SQL SERVER NOT FOUND
0xC00000C5
VADBM DATABASE UPDATE ERROR
0xC00000C6
VADBM TABLE READ ERROR
0x400000C7
VADBM COMPONENT VERSION ERROR
0xC00000C8
VADBM VAMANAGER CONNECT ERROR
0xC00000C9
VADBM INITIALIZATION ERROR
0xC00000CA
VADBM OLEDB SESSION ERROR
0xC00000CB
SYSTEM DIRECTORY ERROR
0xC00000CC
EXCHMON USER NOT FOUND
0xC00000CD
EXCHMON ALREADY INITIALIZED
0xC00000CE
EXCHMON NOT INITIALIZED
0xC00000CF
EXCHMON RULES ENGINE NOT SPECIFIED
0xC00000D0
TELEPHONY CONNECT CALL ERROR
0xC00000D1
VADBM BACKUP FAILED
0xC00000D2
VADBM RESTORE FAILED
0xC00000D3
VADBM INVALID RESTORE DEVICE
0xC00000D4
VADBM MAX LENGTH EXCEEDED
0xC00000D5
VADBM EXPORT FAILED
0xC00000D6
VADBM NO SUCH TABLE
0xC00000D7
VADBM LOG PURGE ERROR
0xC00000D8
VADBM JOB ERROR
0xC00000D9
VADBM JOB NAME ERROR
0xC00000DA
VADBM INVALID JOB
0xC00000DB
VADBM TABLE MIGRATION ERROR
0xC00000DC
VAPUBLISH APP ALREADY BEING PUBLISHED
0xC00000DD
VAPUBLISH APP COMPILE ERROR
0xC00000DE
VAPUBLISH MISC ERROR
0xC00000DF
VAPUBLISH APP COPY ERROR
0x000000E0
VAPUBLISH COMPLETE
0xC00000E1
VAPUBLISH VAL CREATE ERROR
0xC00000E2
VAPUBLISH VAL COMPILE ERROR
0xC00000E3
VAPUBLISH POSTBUILD ERROR
0x400000E4
VAPUBLISH INFORMATION
0x400000E5
VAPUBLISH CHILD PROCESS OUTPUT
0xC00000E6
VAPUBLISH COPY ERROR
0xC00000E7
VAPUBLISH FAILED
0xC00000E8
VAPUBLISH CLEAR DIR FAILED
[0691] The VA Application
[0692] Setting User Preferences for the VA Application
[0693] The VA application should be installed on the user's personal computer. After the VA application is installed, the following user preferences should be set:
[0694] The user's Personal Identification Number (PIN)
[0695] Name and telephone number of the user's human operator
[0696] How the VA can reach the user with incoming calls
[0697] How the user wants to be reminded of appointments and tasks
[0698] Tempo and assertiveness of the VA
[0699] In the preferred embodiment, the user preferences are set using Microsoft Outlook on the user's personal computer.
[0700] Obtaining the Virtual assistant Preferences Screen
[0701] As shown in FIG. 31 , the VA user preferences are located on the Virtual assistant Preferences screen 330 . The Virtual Assistant Preferences screen has three tabs: a General tab 332 , a Phone/Pager tab 334 and a VA Interaction tab 336 .
[0702] The General tab 332 has an Account Number field 340 , which displays the user's account number. The user's account number should be assigned by system administrator, and the user should not be able to change his or her account number. Also on the General tab is the PIN button 342 . The PIN is a four-digit code that is recommended for the user to log into the VA. The PIN is initially assigned by the system administrator, but can be changed by the user by clicking the PIN button 342 .
[0703] The General tab also has a field 344 for designating the contact where the user's information is located. The VA Application uses the user's contact information to page the user and route telephone calls and reminders to the user. The New Contact button 346 can be used to create a contact for the user. If the user desires to have the VA route telephone calls to the user, all of the user's telephone numbers should be stored in the user's contact record.
[0704] A user can move old messages from the Microsoft Outlook Inbox to an archive folder by clicking the Archive Folder field 350 , the Select Folder screen appears, which allows the user to select the folder to be used for archiving.
[0705] The My operator is field is used to select the user's operator from a list. If the user's operator is not included in the contact list, the user can create a new contact for his or her operator. Alternatively, the user can select A manually entered number from the drop-down list 352 and enter the operator's number in the And can be reached at field 354 . If user selected a contact as his or her operator, the operator's telephone number (for example, business) can be selected from the And can be reached at field 354 . If the only available selection is None, the user has not entered any telephone numbers for the contact.
[0706] Phone/Pager Tab
[0707] As shown in FIG. 32 , the Phone/Pager tab 360 allows the user to control how the VA notifies the user about incoming calls and reminders. When the user is away from his or her desk, the VA can attempt to route incoming calls to the telephone at a specified location via the “follow me” feature. The By Phone field 362 has three buttons that control how the “follow me” feature works. If the Route all calls to button 364 is selected, the VA routes all calls to the specific contact (the user or an operator) selected from the first drop-down list box 366 at the phone number (for example, business) from the second drop-down list box 368 . Alternatively, the user can also select A manually entered number from the first list box 366 , in which case the second box 368 becomes a text field in which the user can enter the phone number.
[0708] If the Route calls based on schedule button 370 is selected, the VA will route calls to the user only at specific times, or will route calls to different numbers at different times. For example, the user might want calls to be routed to the user from 8:00 am to 5:00 pm Monday through Friday. If the Route calls based on schedule button 370 is selected, selecting the Schedule button 372 will allow the user to specify a call routing schedule. Specifying a call routing schedule is discussed in more detail in the section entitled “Setting Up a “Follow Me” Schedule.”
[0709] If the Do Not Disturb button 374 is selected, the VA will not route calls to the user. Selecting the Do Not Disturb button also deactivates the “follow me” feature, the telephone notification for reminders feature and Rules Wizard messages. If this option is selected, the VA will ask callers to leave a voice message for the user.
[0710] The By Pager field 376 controls how the VA attempts to page the user. If the Route all pages to button 378 is selected, the VA will route all pages to a specified e-mail address. A contact (usually the user) is selected from the first drop-down list box 380 . If the contact has a pager e-mail address, it appears in the second box 382 . If not, a warning message is displayed. If the contact does not currently have a pager e-mail address, one can be entered on the Virtual Assistant tab of the contact information form. If A manually entered e-mail is selected from the first drop-down list box 380 , the second box 382 becomes a text field in which an e-mail address can be entered. If the Do Not Disturb button 384 is selected, the VA will not route pages to the user, and the pager notification for reminders feature and Rules Wizard messages feature is deactivated.
[0711] A reminder can be set so that the VA reminds the user of a task or appointment by selecting the telephone checkbox 386 and/or the pager checkbox 388 . Similarly, the user can be notified we he or she receives certain types of messages by selecting the telephone checkbox 390 and/or pager checkbox 392 .
[0712] VA Interaction Tab
[0713] As shown in FIG. 33 , in the preferred embodiment, the VA Interaction tab allows the user to specify how the VA interacts with the user. The Tempo field 394 controls the verbosity of the VA. When tempo is set to slow, the VA uses longer phrases to speak to the user. When tempo is set to fast, the VA uses shorter phrases. To change the tempo of the VA, the slider dragged to the desired position. For example, a user would set the tempo to slow when first learning how to use the VA, and after becoming more familiar with the VA, the tempo could be set to fast.
[0714] Returning to FIG. 33 , in the preferred embodiment, the assertiveness of the VA is controlled by the Assertiveness field 396 . When assertiveness is set to low, the VA asks for confirmation before performing a task. For example, if a user instructs the VA to delete a message, the VA asks for confirmation before actually deleting the message. When assertiveness is set to high, the VA carries out most commands without asking for confirmation. To change the assertiveness of the VA, the slider is dragged to the desired position. A user could set assertiveness to low when learning how to use the VA, and after becoming more familiar with the VA, assertiveness could be set to high.
[0715] FIG. 34 illustrates how a call flow changes based on different settings for assertiveness and tempo.
[0716] In an alternative embodiment, the user does not manually adjust the tempo and assertiveness settings. Rather, the VA automatically adjusts these settings based on input received by the virtual assistant, such as information about the user. For example, rather than manually setting a tempo or assertiveness setting, the virtual assistant could have a user competence setting. The options for the user competence setting could be, for example, novice, experienced and expert, and the tempo and/or assertiveness settings would change automatically responsive to a change in the user competence level. Thus, if the user competence level were set to novice, the assertiveness setting and tempo setting would automatically be set to low and slow, respectively. Conversely, if the user competence level were set to expert, the assertiveness setting and tempo setting would automatically be set to high and fast, respectively. As can be appreciated by one skilled in the art, any setting could change automatically responsive to changes in the user competence level.
[0717] In another alternative embodiment, the virtual assistant could automatically increase the tempo and/or assertiveness of the virtual assistant after the user has accessed the virtual assistant a predetermined number of times, preferably, twenty. Alternatively, the virtual assistant could automatically provide a prompt to the user in response to which the user could increase the tempo and/or assertiveness of the virtual assistant after the user accessed the virtual assistant a predetermined number of times, preferably, twenty.
[0718] In an alternative embodiment, the virtual assistant could play a tip to the user about the use of the virtual assistant, or a message of the day, which is determined by the system administrator. Either the tip or the message of the day, or both, might be played every time a user accesses the virtual assistant. The virtual assistant could automatically disable the tips or message of the day if the user accesses the virtual assistant a predetermined number of times. That predetermined number could be calculated automatically by the virtual assistant based on a multiple of the number of tips and/or messages of the day. For example, if there are thirty tips, the virtual assistant could automatically disable the tips after the user heard each tip two to ten times, and, preferably each tips was heard three times. In yet another embodiment, the tips and/or message of the day could be automatically disabled if the user access the virtual assistant a predetermined number of times for a predetermined period of time. For example, the virtual assistant could automatically disable the tips and/or message of the day if the user accesses the virtual assistant more than once in a day. In another alternative embodiment, the tips and/or message of the day could be automatically disabled during the current user session if the time since that last user session is a predetermined amount of time, such as ten minutes or less.
[0719] In another embodiment, the virtual assistant could have a politeness setting, which, when enabled, would cause the virtual assistant to include words or phrases associated with polite discourse in the output from the virtual assistant. Such words or phrases could be, for example, “please,” thank you,” “thanks,” “excuse,” “pardon,” “may I,” “would you mind,” or other words and phrases associated with polite discourse. Alternatively, the user information input into the virtual assistant could be information about the user's experience with the virtual assistant, particularly, whether words associated with polite discourse are included in input received from the user. If, such words of polite discourse are included in the input received from the user, the virtual assistant could automatically enable the politeness setting.
[0720] Alternatively, the user information input into the virtual assistant could be information about the user's emotion, which could be based on information about the user's voice volume, word choice and speech rate. Based on such information, the virtual assistant could automatically determine the user's emotional state, calm or angry, for example. If the user's emotional state is angry, the output of the virtual assistant could automatically include words associated with submissive discourse, such as “sorry,” “regret” and “apologize.” The virtual assistant could save the information obtained about the user's emotional state for use in future sessions.
[0721] The user information also could be comprised of information about the amount of time since the user last provided input to the virtual assistant. If the amount of time since the user last provided input to the virtual assistant is a predetermined amount of time, for example, fifteen seconds or more, the virtual assistant could perform a predetermined action. The predetermined action would be determined by context. For example, if the user was reading messages, the predetermined action would be to read the next message, or prompt the user by saying, “Shall I read your next message,” or provide a hint to the user by saying, “You could read your next message.”
[0722] Alternatively, the user experience information could be information about the amount of time a user pauses during the recording of a message. If this amount of time is greater than a some predetermined amount of time, such as two seconds, the virtual assistant would stop recording, provide the user with the option to continue recording. Then, the amount of time before the virtual assistant stopped recording would be automatically increased by some other predetermined amount of time, such as 500 milliseconds, so that the virtual assistant would continue recording during future pauses in recording by the user.
[0723] Speech recognition errors are always possible in which case the VA may misinterpret a command. For example, Read this message could be interpreted to mean Delete this message. In this case, if assertiveness is set to high, the VA will delete the message without asking the user for confirmation. Thus, an alternative embodiment of the VA would have a setting for the user competence. If the user competence setting is set to novice, the VA could be programmed not to execute a particular command, such as Delete this message or Delete all messages, without user confirmation. Conversely, if the user competence setting is set to expert, such commands could be executed without confirmation when the assertiveness setting is set to high.
[0724] Prompt to record a subject when sending messages
[0725] Returning to FIG. 33 , in the preferred embodiment, the VA Interaction tab includes a setting 400 to prompt a user to record a subject when sending a message.
[0726] Change VA Name
[0727] As shown in FIG. 33 , in the preferred embodiment, the VA Interaction tab includes a setting 402 to change the name for the VA from the default name “Conita.” If the user wants to change the name of the VA, this box should be checked and the new name of the VA should be entered in the text box 404 . The VA name entered in the text box 404 is used in the “Come back” command (for example, “Conita, come back”). This command allows a user to bring the VA back during a telephone call so that additional commands can be issued by the user. Adding a name to the “Come back” command makes it easier for the VA to understand this command and decreases the chance of the VA coming back accidentally because it misinterpreted a phrase in a phone conversation as the “Come back” command.
[0728] ‘Come back’ on keypad only
[0729] As shown in FIG. 33 , in the preferred embodiment, the VA Interaction tab includes a setting 406 for ‘come back’ on the keypad only. If this box 406 is not checked, the VA will come back from a break if the user says “Come back” or presses a predetermined key, such as the star (*) key, on a telephone keypad. If this box 406 is checked, the VA will come back only if a predetermined key, such as the star (*) key, is pressed on the telephone keypad.
[0730] VA Greeting
[0731] As shown in FIG. 33 , in the preferred embodiment, the VA Interaction tab includes VA Greeting settings 408 . When a user calls its VA and logs in successfully” the VA responds with a greeting message. There four check boxes 410 , 412 , 414 and 416 that allow the user to specify the information contained in the greeting message. For example, if user checks check box 414 for the number of Appointments for today, the VA will tell the user how many appointments it has, and other relevant information about such appointments, for a predetermined period of time, such as one day. Any combination of the boxes 410 , 412 , 414 and 416 can be checked.
[0732] In an alternative embodiment, the greeting information about the user's appointments or tasks could be automatically disabled during a user session if the time since the last user session is a predetermined amount of time, such as ten minutes or less.
[0733] In addition, the virtual assistant will provide time-of-day specific greetings to the user based on when the user accesses the virtual assistant. For example, if the user accesses the virtual assistant in the morning, the virtual assistant may greet the user by saying, “Good morning.” These time-of-day specific greetings can be automatically disabled during the current user session if the time since the last user session is a predetermined amount of time, such as ten minutes or less.
[0734] Setting Up a “Follow Me” Schedule
[0735] Returning to FIG. 32 , if the Route calls based on schedule setting is enabled, the user should establish a call routing schedule, which causes the VA to route phone calls to the user at different times. In the preferred embodiment, before establishing a call routing schedule, the user should define a contact for himself of herself in Microsoft Outlook. Under this contact, the user should specify each telephone number (home, business, and so on) to which it wants the VA to route calls. Returning to FIG. 31 , the user also should specify this contact in the Contact where my information is located 344 on the VA Preferences General tab 332 .
[0736] Returning to FIG. 32 , in the preferred embodiment, to set up a call routing schedule, the user should enable the Route calls based on schedule setting 370 on the Phone/Pager tab 360 and then click the Schedule button 372 . Upon clicking the Schedule button 372 , as shown in FIG. 35 , the Phone Schedule screen 418 is activated. A block of time is selected by clicking the box for the starting date and time and dragging the mouse to the box for the ending date and time. The block of time selected is highlighted in blue. Clicking the right mouse button activates a menu that displays the telephone numbers (for example, home or work) for the contact specified in the Contact where my information is located 344 on the VA Preferences General tab 332 . The user selects the telephone number to which the VA should route calls during the specified block of time. To cause the VA to route calls to a contact other than the user, Other can be selected from the menu and then the other contact and telephone number can be selected. In the preferred embodiment, if a contact other than the user is selected, the specified time block changes, for example, to white with a green border.
[0737] In the preferred embodiment, a user can select more than one block of time, and can specify a different telephone number for each block of time. In addition, the user can override the call routing schedule with the “Follow me” voice command, which is discussed above. If the user overrides the routing schedule with a voice command, a red line identifies the period of time for which the override is in effect. Also, if the contact where the user's contact information is located is changed, or if the contact to whom calls are being routing is deleted, the VA cannot use the schedule to route calls and a colored border, such as a red border, identifies the affected time blocks. The user should delete these time blocks and redefine them for the new contact.
[0738] Other VA Options Set with Outlook
[0739] In addition to the preferences that can set on the Virtual assistant Preferences screen, there are other options that can be set with Outlook, including Automatic message notification through the Rules Wizard and Additional contact information.
[0740] The VA can notify a user by telephone or pager when the user receives certain types of messages. For example, the user might want to be notified if he or she receives a message from his or her supervisor. In order to use this feature, the user should use the Outlook Rules Wizard to specify the types of messages that trigger automatic notification. Information concerning the use of the Outlook Rules Wizard can be found at the Microsoft web site, www.microsoft.com. To set up a rule for VA notification, the type of message for which the user wants to be notified should be selected. Also, the forward it to people or distribution list setting should be enabled. Under Rule Description, the underlined people or distribution list should be selected and then the VAManager should be selected, which causes the affected messages to be forwarded to the VA, which in turn forwards them to the user. Returning to FIG. 32 , in the preferred embodiment, in order for rules notification to function, the Phone setting 390 and/or the Pager setting 392 should be enabled.
[0741] As shown in FIG. 36 , when the VA software is installed, it adds a Virtual assistant tab 420 to the Outlook screen for defining contacts. This tab allows the entry of additional contact information for the VA. The VA tab 420 has Name Pronunciation—First 422 and Name Pronunciation—Last fields 424 which allow the entry of a phonetic pronunciation for a contact's first or last name. These fields can be used to enter a phonetic pronunciation if the VA does not pronouncing the contact's name correctly. For example, if a contact named “Conita” is being pronounced “Coneeta,” a user could enter “Conighta” in this field to change the pronunciation used by the VA.
[0742] The Nickname 426 and Nickname2 428 fields can be used to enter a contact's nickname. If a nickname is entered, the VA can look up that contact using the specified nickname. Alternatively, a contact's nickname can be entered on the Details tab 430 .
[0743] The Pager E-mail field 432 can be used to enter the e-mail address for a contact's pager.
[0744] The Gender field 434 can be used to select the contact's gender. The VA, when interacting with a user, will use words associated with the gender selected. If male is selected, the VA may ask the user, “Would you like to call him?”
[0745] Interacting with the VA
[0746] In the preferred embodiment, in making utterances to the VA, the user should speak clearly and at a moderate pace. The user also should speak at normal volume level. If the VA has difficulty in understanding the user, different volume levels should be tried. The user should use words and phrases that the VA understands. Background noise will reduce the ability of the VA to understand utterances from the user. A user should interact with the VA in a quiet place. The user should avoid pauses when saying a command. If a user pauses, the VA will interpret the pause as the completion of a command. The user should avoid pauses when saying a number, such as a telephone number because should a pause will be interpreted as the end of the number. The user should pronounce each digit when uttering a number to the VA. For example, if a user's PIN is 2314, the user should say “two, three, one, four.” An exception is time; for example, the user can utter either “12 o'clock” or “1200.”
[0747] If a user has difficulty performing a task, help can be requested by uttering “Help” or “What are my options?” The VA will respond automatically with information to assist the user in performing the current task. Also, if there is a period of silence and the user appears to be having trouble, the VA will offer help by reading a list of possible options.
[0748] The VA can provide either global help of context-sensitive help. Global help lists the tasks that can be performed with the VA. To request global help, the user should utter “What are my options?” after the VA says, “What can I do for you?”. The VA responds by listing the major tasks that can be performed. The user can then utter the desired option.
[0749] When the user is performing a task, any request for help results in a context-sensitive help message for that task. For example, if the user requests to send a message, the VA asks who is to be the intended recipient. If, at this point, the users utters “What are my options?” the VA will tell the user how to provide the contact name for the message recipient.
[0750] In the preferred embodiment, as an alternative to uttering commands, the VA allows a user to issue commands with predetermined key, such as the star (*) or “star” key, of the telephone keypad. This method of interaction, known as Star mode, is useful when the VA is having difficulty understanding a user's utterances because of background noise. To enable the Star mode, the star key (*) on the telephone keypad should be pressed. The VA will provide the user information as to the available options. At the time the desired option is being provided, the option can be selected by the user by pressing the * key. The star mode is discussed in more detail below.
[0751] If the VA is providing output, and the user desires to interrupt the VA, the VA is programmed to allow the user to “barge in.” When a user barges in, the VA stops talking. For example, if the VA is reading a message and user wants to hear the next message before the VA has completed reading the current message, the user can barge in and say “Next.” This will cause the VA to begin reading the next message. The barge in feature can be deactivated by pressing a predetermined key, such as the number sign (#) key, on the telephone keypad. When the barge-in feature is deactivated, the VA will continue to respond to user voice commands, but will not allow a user to barge-in while the VA is providing output, by speech or otherwise. The barge-in feature can be reactivated by pressing the # key again. A user might want to deactivate the barge-in off if background noise that will cause recognition errors is anticipated.
[0752] A user can stop the VA from performing an action by saying “Cancel” or “Stop.” For example, if a user asks the VA to place a telephone call and then decides not to place the call, uttering “Cancel” will stop the VA from placing the call. The cancel function is also useful if a user loses track of what he or she is doing or wants to restart a task. Uttering “Cancel” will stop the current task; the VA will indicate that it is ready to receive the next utterance by saying, “What can I do for you?”
[0753] A user can deactivate the VA, that is, put it on hold, at any time by uttering “Take a break.” The VA stops the task or action being performed and waits for the user to utter a predetermined command, such as “Come back.” After the VA back is reactivated, the VA can continue the task that it was performing when it was deactivated, or begin performing a new task or action.
[0754] When a user wants to end a VA session, the user can utter a predetermined phrase, such as “good-bye” or simply hang up. If the VA hears the user utter “good-bye,” it will also say “good-bye” and prepare to hang up. A short period between the time when the VA says “good-bye” and the time when it actually hangs up allows the user to restart the session by saying “wait” or any other supported system command.
[0755] If the VA does not understand a user utterance, it will ask the user to clarify the utterance. In many cases, the VA will not understand a user utterance because of a recognition error. Recognition errors can be the result of speech problems, syntax problems or inappropriate context.
[0756] Speech problems occur when the VA cannot recognize what is being uttered by the user for one of several reasons, such as background noise, bad phone connection, heavily accented speech, speech is too loud, too fast or too slow.
[0757] Syntax problems occur when a user utterance does not conform to the syntax recognized by the VA. Although the VA is very flexible in recognizing utterances, it is designed to recognize phrases for specific tasks. If the user does not provide the VA with sufficient information, or an utterance contains extraneous words, the VA might become confused. For example, the VA may not understand the utterance, “What I need to know is the number for John Smith's home extension.” However, the utterance, “What is John Smith's home phone number?” can be understood by the VA.
[0758] Recognition errors also occur if a user utters a valid command, but the command is inappropriate given the context. For example, if a user is creating an appointment, the VA expects to be provided information about the appointment. If the user utters a command to call a contact before finishing the task of creating the appointment, the VA will not recognize the command as valid.
[0759] If the VA is having difficulty understanding user commands, the user can be instructed to take the following actions:
[0760] Eliminate background noise.
[0761] Speak more loudly.
[0762] Speak more distinctly.
[0763] Speak at a natural pace—not too slowly.
[0764] Eliminate like pauses.
[0765] Make sure that those around the user are not speaking at the same time.
[0766] Say “Cancel” and start over again.
[0767] Instead of speaking commands, press the * key and use Star mode to issue commands.
[0768] Let the VA assist in framing a command.
[0769] Look up examples of the command to be issued.
[0770] The VA can be programmed to provide such instructions automatically, depending on the number and/or frequency of recognition errors.
[0771] In the preferred embodiment, the VA automatically disconnects and terminates the user session if it receives a predetermined number of recognition errors. The VA also automatically disconnects after predetermined period of inactivity, for example, approximately 15 seconds. Before disconnecting, the VA should inform the user to call back and try again. The automatic disconnect feature prevents an off-hook VA from staying connected due to background noise. The automatic disconnect feature also allows the user to obtain a better connection if recognition errors are due to a bad connection.
[0772] If a user wants to send the system administrator a comment about the VA, the user can utter “Leave a comment.” The VA then prompts the user to record and comment and automatically sends it to the system administrator.
[0773] Calling the VA and Logging In
[0774] When a user calls the VA, it should log in. The system administrator determines the recommended log-in information. If each user has a unique telephone number for his or her VA, then the user need only provide a PIN to log in. If every user uses the same number to reach his or her VA, the user should provide both an account number and a PIN to log in.
[0775] After a user has logged in successfully, the VA will respond with a brief tone and a greeting. For example, “You have four e-mail messages. You have two voice mail messages.” After the greeting, the VA will provide a prompt such as, “What can I do for you?” This indicates that the VA is ready to receive commands or utterances from the user.
[0776] The actual content of the greeting depends on settings specified by the user, as discussed above. In an alternative embodiment, the greetings will automatically change responsive to how the user has previously interacted with the VA. For example, the VA may be initially configured to provide time-of-day specific greetings (for example, “Good morning,” “Good afternoon,” “Good evening”) when the user logs in. Such time-of-day specific greetings may be automatically disabled for a predetermined period of time, such as a day, if the amount of time since the user last accessed the VA is a predetermined amount of time, such as ten minutes or less. The time-of-day specific greetings also could be disabled after the user accesses the VA more than a three times in a day.
[0777] Similarly, the VA may be initially configured to provide information to the user about the user's appointments scheduled for, or tasks that are due, the day. Such appointment and/or task information may be automatically disabled for a predetermined period of time, such as the rest of the day, if the amount of time since the user last accessed the VA is a predetermined amount of time, such as ten minutes or less. The providing of such appointment or task information also could be disabled after the user accesses the VA more than a three times in a day.
[0778] Overview of Messages
[0779] After a user logs in to the VA, the user will likely want to listen to new messages, such as voice mail messages, e-mails, meeting and task requests generated through Microsoft Outlook, and faxes received by the VA and stored as messages.
[0780] The VA provides several different options for listening to messages. These options allow a user to quickly determine which messages are important and then obtain more detail about them. The options are listed in the table set forth below:
[0000]
Option
Information provided
Count
Count of messages
Browse
Sender and subject
List
Sender and subject
Read
Sender, subject, body of the message,
attachments
Note: The VA cannot read faxes to a user To
read a faxed message, the user should forward
it either to a fax machine or to a personal
computer that contains fax display software
More detail
Detail in addition to that provided by the read
option; varies according to the type of message
[0781] “Navigating” is the process of directing the VA to the specific message or messages a user wants to hear. If a user instructs the VA to “Read my messages,” the VA reads all messages in order, beginning with the oldest new message. However, there are many options that allow a user to specify which message or messages VA should read.
[0782] “New” messages are those that have been received since the user last called the VA (and, perhaps, since the user last checked messages on a personal computer). “Old” messages include all other messages, even if they have not been read. If a user instructs the VA to read messages, it reads the new messages by default, and then will read the user's old messages. If the user instructs the VA to “Read my old messages,” the VA starts reading the most recent old message, and then reads the user's most recent old messages.
[0783] “Read” messages are those that the VA has read to the user or the user has read with Outlook on a personal computer. “Unread” messages are those that the VA has not read to the user and the user has not read with Outlook.
[0784] The “first” message is the most recent message received by the user. The “last” message is the oldest message received by the user. A user can tell the VA read the first or last message by saying “Read my first message” or “Read my last message.”
[0785] A user can tell the VA to read the next or previous message by saying “Next” or “Previous.” In order for these commands to work, the VA should have a message context. That is, it should be listing, reading, or performing a similar activity. If the VA says, “What can I do for you?” and a user says “Next,” a misrecognition will likely occur. As discussed above, a user is not required to wait for the VA to finish reading the current message; when the user wants to hear the next message, the user can barge in and request the VA to read the next message.
[0786] A user can filter, or tag, the messages the user wants to access by providing additional descriptive information to the VA. For example, if a user instructs the VA to “Read my new messages,” the VA reads all new messages beginning with the first new message. However, if a user is expecting an important message from a particular person, e.g., John Smith, the VA will read only messages from John Smith if the user instructs the VA to “Read my new messages from John Smith.”
[0787] Listening to Messages
[0788] A user can request the VA to provide a count of messages by saying, “How many messages do I have?” The VA will respond, for example, by saying, “You have four messages. Two of these are e-mail messages, and two are voice mail messages.
[0789] The following table shows other options available to a user in requesting a count of messages.
[0000]
Option
Example
Message type:
How many e-mail messages do I have?
E-mail
Do I have any voice mail messages?
Voice mail
Meeting requests
Task requests
Message status:
How many old messages do I have?
New or Old
Read or Unread
Urgent
A combination of the other
How many new meeting requests do I have?
options
[0790] A user can browse messages by saying, “Browse my messages.” The VA responds by reading the sender and subject for each message, beginning with the first message. For example, “Sally Jones . . . Need your timesheet,” and “James Ford . . . Lunch today?” If a user wants the VA to read a message, the user can barge in while the VA is reading the subject and say, “Read it.” The user-should say, “Read it” before the VA begins the next message. If the VA begins reading the next message before the user says, “Read it,” the user can say “Previous” to get back to the message. For voice messages, the VA plays back a recording of the sender's name. For faxes, the VA reads the number of the sending fax machine.
[0791] A user lists messages by saying, “List my messages.” The VA responds by reading the sender, delivery date, and subject for each message, beginning with the first message. Listing is an efficient way for a user to review messages and determine which ones are the most important. If the user wants the VA to read the current message it is listing, the user can barge in and say “Read it.” The following table shows other options available to a user in requesting a list of messages:
[0000]
Option
Examples
List my voice mail messages
List my meeting requests
Message type:
E-mail
Voice mail
Meeting requests
Task requests
Sender or subject
List my messages by sender
Message status:
List my unread messages
New or Old
Read or Unread
Urgent
A combination of the other options
List my e-mail messages by sender
[0792] In order to hear the body of a message, the user should ask the VA to read it. The most basic command for reading messages is simply “Read my messages.” This causes the VA to read all of a user's messages.
[0793] The VA reads different types of messages in different ways, based on the information available for the type of message. In general, however, the VA reads messages as follows:
[0794] Message description
[0795] Message text
[0796] Message attachments
[0797] As mentioned above, the VA cannot read faxes. To read a faxed message, a user should forward it either to a fax machine or to a personal computer that contains fax display software.
[0798] The message description contains the information necessary for a user to identify a message. The VA reads this information first so the user can decide whether to listen to the message. The message description is different for different message types, as shown in the following table:
[0000]
The message description contains the
For this message type
following
E-mail
Sender, delivery date, and subject
Voice mail
Message type, caller's name, delivery date, and
callback number
Meeting requests
Sender, delivery date, and subject
Task requests
Sender, delivery date, and subject
Faxes
Telephone number of the machine that sent the
fax
[0799] When a user instructs the VA to read messages, the messages can be filtered as follows:
[0000]
Option
Example
Message type:
Read my voice mail messages
E-mail
Voice mail
Meeting requests
Task requests
Sender
Read my messages from John Smith
Message status:
Read my first message
First or Last
Read my urgent messages
New or Old
Read or Unread
Deleted
Urgent
A combination of the other
Read my e-mail messages from John Smith
options
[0800] When the VA finishes reading the text of a message, it reads (or plays) any attachments included with the message. Before reading an attachment, the VA tells the user its type and name. If user asks for more detail, the VA tells the user the attachment's file size. In the preferred embodiment, the VA can read text, rich text, HTML, and sound files (e.g., .wav files). The VA informs a user if an attachment cannot be read. If a message contains more than one attachment, a user has the following navigation options:
[0801] First
[0802] Last
[0803] Next
[0804] Previous
[0805] If a user wants more detailed information about a message than the VA provides automatically by reading, the user can say, “Get more detail.” The VA will respond by providing additional detail, depending on the type of message.
[0806] If a user wants to remove a message from the Inbox and retain a copy, the user can move it to an archive folder. To move a message from Inbox to an archive folder, say, “File this message.” Once a message is archived, the user can access it from the VA only if it is returned to the Inbox by saying “Restore” immediately, before issuing the next command. Before a user can archive messages, an archive folder should be created under Microsoft Outlook, and the name of the archive folder should be specified in the user preferences, which is discussed above.
[0807] As user can delete any message from the Inbox by saying, “Delete this message.” The message to be deleted should be the current message, that is, the message the VA is describing or reading. If a user wants to restore a deleted message, it can do so by saying “Restore this message” immediately, i.e., before the user continues to the next command. Once the user issues the next command, the VA cannot restore the deleted message. When the user ends the current session, all deleted messages are moved to the Microsoft Outlook Deleted Items folder. Messages in the Deleted Items folder are subject to the permanent deletion policy defined with Outlook. If a user tells the VA to delete a meeting or task request, the VA will ask the user if it wants to respond to the sender with a rejection before deleting the message.
[0808] Managing Contacts
[0809] A user can browse contacts by saying, “Browse my contacts.” The VA responds by telling how many contacts in the contact list and reading the name of each contact (in alphabetical order).
[0810] If a user wants more information than browsing provides, a user can list contacts by saying, “List my contacts.” The VA responds by telling how many contacts in contact the list, and reading the name and company of each contact. If the user wants more detailed information about the current contact that the VA is listing, the user can barge in and say “Read it.”
[0811] If the user wants more information than listing provides, the user can read contacts by saying “Read my contacts.” The VA responds by telling how many contacts in the contact list, and reading each contact's name, title, company, telephone numbers, and e-mail address.
[0812] If the user wants more detailed information about a contact than the VA provides by reading, the user can say, “Get more detail.” The VA responds by reading the contact name, job title, birthday, spouse name, gender, anniversary and other telephone numbers.
[0813] To access a specific field of information (for example, a telephone number or e-mail address) for a specific contact, the user can use any of the following commands:
[0814] Look up a contact
[0815] Look up John Smith
[0816] Who is John Smith?
[0817] What is John Smith's telephone number?
[0818] What is John Smith's work telephone number?
[0819] What is John Smith's address?
[0820] What is John Smith's e-mail?
[0821] When a user inquires about a contact, the user should identify the contact for the VA. The user can use any of the following to identify a contact:
[0822] First name and last name
[0823] Last name only
[0824] First name only
[0825] Nickname1
[0826] Nickname2
[0827] Nickname and last name
[0828] The more information provided, the more precisely the VA can identify the contact. For example, if a user asks for a contact by last name only and the contact list contains more than one contact with that last name, the VA cannot immediately determine which contact the user wants. If the VA finds more than one matching contact, it begins with the first contact and asks whether this is the one the user wants. The user can respond by saying either “Yes” or “No” until the user identifies the desired contact.
[0829] To create a new contact, the user can say “Add a contact.” The VA prompts the user to provide first name, last name, e-mail address, work telephone number and home telephone number.
[0830] When prompting for a name, the VA first asks the user to say the name. The VA then repeats the name and asks if it is correct. If the name is correct, the user will say “Yes” and the VA prompts the user for the next piece of information. If the name is not correct, the user can either say “Try again” to say the name again, or say “No” to spell the name one letter at a time, with the VA confirming each letter. When the VA confirms the last letter of the name, that user can say, “That's it” to continue.
[0831] When spelling a contact's name or e-mail address, the user has the following options:
[0832] Say the letter (for example, “B”)
[0833] Say the International Phonetic Alphabet word for the letter (for example, “Bravo” for B) because the VA is morel likely to understand a word than a single letter.
[0834] Press the button on the telephone keypad that corresponds to the letter. The VA recites the International Phonetic Alphabet word for each letter on the button (for example, “Alpha Bravo Charlie”). The user can then say the word for the letter.
[0835] When spelling an e-mail address, user can say “At” for the at sign (@) and “Dot” for a period (.).
[0836] A user can create a new contact from an e-mail message. The e-mail should be the current message the VA is reading. To create a new contact from an e-mail message, the user can say “Add this contact.” The VA adds the sender of the e-mail to the user's contact list, if that person is not already in the contact list.
[0837] Sending Messages
[0838] A user can send a new message to any contact in the contact list by saying “Send a message.” The message is recorded as a sound file (.wav) and attached to an e-mail message. The recipient of the e-mail message should have some means of playing sound files. The user can specify the name of the contact in the command (for example, “Send a message to John Smith”). If the user says, “Send a message,” the VA asks for the name of the contact. If the contact has more than one e-mail address, the VA asks to specify which e-mail address to use. The user can specify the name of a distribution list (for example, “Send a message to Quality Team”) instead of a contact. The VA sends the message to each contact in the distribution list. When the contact name and e-mail address have been resolved, the VA asks whether to record a subject for the message. If the user says, “Yes,” the VA directs the user to record the subject. After requesting the subject, the VA asks to begin recording the body of the message. When finished recording the body, the VA asks whether to send the message.
[0839] A user can reply to a message in Inbox by saying “Reply to this message.” The message replied to should be the current message, that is, the message the VA is describing or reading. The reply is recorded as a sound file (.wav) and included as an attachment. A user can also record a sound file for the subject of the reply. The original message is included in the reply. All attachments (except those created by the VA) are stripped from the reply. The original message is appended to the reply message. If the user replies to a voice mail message, the VA attempts to call the person who left the message.
[0840] A user can forward any message in Inbox to a contact on the contact list by saying “Forward this message.” The message forwarded should be the current message, that is the message the VA is describing or reading. The VA handles forwarded messages in much the same way as it handles replies, except that the original attachments are included. The user can specify the name of a contact when forwarding a message. If the user says, “Forward this message,” the VA asks for the name of the contact. If the contact has more than one e-mail address, the VA asks to specify which e-mail address to use.
[0841] The user can fax a message by saying, “Fax this message.” The message to be faxed should be the current message, that is, the message the VA is describing or reading. A user can fax a message to either an existing contact in the contact list (the user should specify the name of the contact and the VA faxes the message to the contact's fax number) or a fax number that is recited to the VA at the time of the fax request. Attachments are included in a faxed message only if the fax software recognizes them.
[0842] Managing Telephone Calls
[0843] The VA handles incoming calls from the user and from other callers attempting to reach the user. When the VA receives an incoming call, it asks for the caller's name. If the user is the caller, the user identifies itself by saying, “It's me,” and logging in using the account number (if required) and PIN. The user can then start issuing commands to the VA. If another caller is attempting to reach the user, the caller should record a name when the VA asks for it. The VA then asks whether the caller wants to be connected to the user or leave a message. If the caller asks to be connected, the VA handles the call based on the user preference settings:
[0000]
If . . .
Then the VA . . .
the “follow me” feature is enabled
attempts to forward the call
to the “follow me”
telephone number specified
the “follow me feature” is disabled,. or
asks the caller to record a
the VA cannot reach the user, or
message
the “do not disturb” feature is enabled
the user rejects the call
[0844] After recording a message, the VA asks if the caller wants to send the message. If the caller does not respond immediately, the VA recites a list of options (for example, send the message, review the message or cancel). The caller can select the desired option by saying the correct phrase. The caller's message, including the recorded name and telephone number, is sent to the Inbox as a voice mail message. The user can then listen to this voice mail message the next time the user accesses the VA.
[0845] The VA assigns a line number to each inbound and outbound call. This is useful if the user needs to keep track of multiple calls or if the user is involved in a conference call. If the user has several active calls, the user can use the following calls to determine which caller is on which line:
[0000]
Command
Description
Who is on line?
Tells which caller is on each line
Who is on line <x>?
Tells which caller is on the specified line
[0846] After the VA connects a call, it become temporarily inactive, that is, it “goes to sleep.” While sleeping, the VA only responds to a specific wake-up command. This allows the user to talk with the calling or called party without interference from the VA. The user can interrupt a call and reactivate, or “wake up,” the VA at any time by saying “Come back.” The VA responds by saying, “I'm here.” The user can then issue commands to the VA again. If the user does not want the other party to the call to hear the dialog with the VA, the user can say “Go private.” When a call is completed, the VA returns to continue performing tasks.
[0847] A user can terminate a call by either hanging up (this also terminates the call with the VA) or saying one of the following commands:
[0000]
Command
Description
Drop line <x>
Terminates the call assigned to line <x> but
keeps the call with the VA open
Drop all lines
Terminates all calls on all lines but keeps the
call with the VA open
[0848] If a user receives an incoming telephone call while already on a call, the VA interrupts with a tone. This tone is referred to as a “whisper,” since it is audible only to the user, that is, no other parties on the line can hear the tone. When the user hears the whisper, the user can break from the current call and speak to the VA by saying, “Come back.” The VA gives the user more detail about the call and allows the user to accept it by saying, “Take the call” or reject it by saying, “Reject the call.” If the user does not respond in a predetermined amount of time, the VA sends the call to voice mail.
[0849] The VA prompts incoming callers to provide a name. If the user has the “follow me” feature enabled, the VA attempts to reach the user by telephone and inform the user of the incoming call. When the VA contacts the user, it recites the recorded name of the caller. The user then has the option to accept or reject the call. If the user accepts, the VA connects the caller. If the VA cannot transfer the call because the user rejected the call, the VA could not reach the user or the user as the Do Not Disturb feature enabled, it asks the caller to leave a message. The VA only attempts to reach the user at one number. The user can change this number at any time. The user also can set this number to change at different times of the day.
[0850] A user can set options for the “follow me” feature in the Microsoft Outlook VA user preferences, which is discussed above. The user can issue the following commands to override the user preferences for the “follow me” feature:
[0000]
Command
Description
Follow me
Use this command to turn “follow me” on or to
override the current call routing schedule. The
VA asks to specify the duration of the override
and the telephone number at which the user can
be reached.
Hold my calls
Use this command to enable on the “do not
disturb” option. The VA asks the user to
specify the duration.
[0851] When the VA asks for the duration of an override (“How long . . . ?”), the user can specify any of the following:
[0852] <x> hours (where x is a number from 1 through 96)
[0853] <y> minutes (where y is 15, 30, 45, or 90)
[0854] <x> hours, <y> minutes
[0855] All day
[0856] Forever
[0857] Until I tell you different
[0858] An override command expires when the specified duration has passed. The user can also cancel an override command at any time by saying “Put me on schedule.” When an override command expires or is canceled, the user preference “follow me” settings are reinstated.
[0859] The user can command the VA to call to a contact from the user's Microsoft Outlook list by:
[0860] Saying “Call <contact name>” (for example, “Call John Smith”).
[0861] Inquiring about the contact's telephone number (for example, “What is John Smith's work phone number”). The VA provides the requested number and then asks if the user wants to call it.
[0862] Before placing a call to a contact, the VA recites the contact's name and location and then remains silent for a short period. This period of silence allows the user to correct a mistake or cancel the call. If the contact has more than one telephone number, the VA asks which number to call. If the user has previously called a contact with more than one telephone number, the VA will automatically call the contact at the telephone number last used by the VA to call the contact. If no telephone number exists for the contact, the VA informs the user of this and returns to the main menu. If the contact's telephone number includes an extension, the VA reminds the user of the extension before placing the call. The VA determines whether the call is long distance or local and adjusts the number accordingly.
[0863] A user can command the VA to place a call to any telephone number from two to eleven digits long. To place a call to a telephone number, say “Call <phone number>” (for example, “Call 803-366-4509.”) Before placing the call, the VA repeats the number and the user has a short period of time to correct any mistakes.
[0864] The user can instruct the VA to call back a person who left a voice mail message. The voice mail message should be the current message, that is, message the VA is listing or reading. To instruct the VA to call back, say “Give them a call.” The VA should be able to determine the caller's telephone number. Either the caller should leave a number, or the VA should capture the number from which the call was placed. The VA informs the user if it cannot determine the caller's telephone number.
[0865] The VA uses the concept of a “conference room” to enable a user to make conference calls. If a user puts a call in the conference room, that person can hear and speak to all of the other parties in the conference room. If the user “goes private” with a line, none of the other parties on other private lines or in the conference room can hear the user. There are three ways a call can be placed in the conference room:
[0866] If the user is already talking to someone and accepts an incoming call without “going private,” the new call is placed in the conference room.
[0867] If the user is talking to someone and asks the VA to call another party without “going private,” the new call is placed in the conference room.
[0868] The user can instruct the VA to place a call or calls in the conference room.
[0869] The user can have both “private” and “conference room” calls active at the same time. The following table lists commands that the user can use to manage conference calls:
[0000]
Command
Description
Put line <x> in the
Puts the specified line in the conference room
conference room
Put everyone in the
Puts all of the user's current calls in the
conference room
conference room
Put me in the
Switches the user from a private call to the
conference room
conference room.
Who is in the conference
Lists all calls that are in the conference room
room?
[0870] Managing A Schedule
[0871] A user can obtain a summary of appointments by saying “Summarize my appointments.” The VA responds by asking for the date, in response to which the user can say “Today,” “Tomorrow,” or a specific date, for example, February 19th. When the user has provided the date, the VA recites the number of meetings, all day events, and appointments.
[0872] A user can browse his or her schedule by saying, “Browse my appointments.” The VA responds by asking for the date. When the user provides the date, the VA recites the subject and start time for each appointment.
[0873] A user can request a list of all appointments by saying, “List my appointments” or “What are my appointments?” The VA responds by asking for the date. When the user has provided the date, the VA tells the user how many appointments he or she has and recites the start time, duration, and subject for each appointment.
[0874] A user can filter the appointment list by any of the following:
[0000]
Type of Filter
Example
Date (today or tomorrow)
List my appointments today
First or last
List my first appointment
Next or previous
List my next appointment
A combination of the other filters
List my first appointment today
[0875] A user can request that the VA read all appointments by saying “Read my appointments.” The VA tells the user how many appointments he or she has, and then reads the start time, duration and subject for each appointment.
[0876] A user can filter the appointments to be read by the same criteria that used to filter an appointment list:
[0000]
Type of Filter
Example
Date (today or tomorrow)
Read my appointments for today
First or last
Read my first appointment
Next or previous
Read my next appointment
A combination of the other filters
Read my first appointment tomorrow
[0877] If a user needs more detailed information about an appointment than the VA provides by reading, the user can say, “Get more detail,” and the VA responds by providing information regarding whether or not the appointment is recurring, attendees and location.
[0878] A user can respond to a meeting request by saying “Reply” or “Forward” while the VA is listing or reading it. When a user says, “Reply,” the VA lists the options for replying to a meeting request, which are Accept, Tentatively accept, Decline, Forward and Reply.
[0879] When a user responds to a meeting request, the VA asks if the user wants to add an annotation. If a user accepts a meeting request, the VA deletes it from the Inbox and moves it to the Calendar folder. If the user chooses to forward a meeting request, the VA requests the name of the contact to whom the user is forwarding it.
[0880] A user can ask the VA to find free time in his or her schedule using the following commands:
[0881] Find free time (the VA will then ask the user to specify the date)
[0882] Find free time today
[0883] Find free time tomorrow
[0884] To add an appointment to a user's schedule, say, “Schedule an appointment.” (The user can also specify “Today” or “Tomorrow” in the command; for example, “Schedule an appointment tomorrow.”) The VA then asks the user to specify the following the duration of the appointment, date (if not specified in the original command), starting time and subject. The VA automatically checks free time when a user schedules an appointment.
[0885] The VA can remind a user of his or her appointments, by either telephone or pager or both. When notifying the user of a reminder by telephone, the VA plays a “whisper” tone. This tone is different from the “whisper” tone for an incoming call. The VA does not actually deliver the reminder until the user either completes or cancels the current function. When a user schedules an appointment, the VA uses the default reminder time specified for the Microsoft Outlook Calendar. In order for the VA to deliver reminders, the user should first set the correct notification options in the Microsoft Outlook VA user preferences. The option that controls reminder notification is notify me on reminders via on the VA Preferences Phone/Pager tab.
[0886] A user can delete an appointment by saying, “Delete this appointment” while the VA is describing or reading it.
[0887] A user can use the VA to deliver a wake-up call by creating an appointment with a reminder for the time the user wants to be awakened. To deliver wake-up calls the user should ensure that telephone reminders are enabled in the Microsoft Outlook user preferences.
[0888] A user can use the following commands to request the date and time:
[0889] What day is it?
[0890] What time is it?
[0891] If a user travels to a different time zone, the user can cause the VA adjust the time for emails, appointments, and tasks accordingly. To change time zone, say, “Change my time zone.” The VA asks for the current local time, which it uses to compute the new time zone.
[0892] Managing Tasks
[0893] A user can use the VA to manage task information stored in the Outlook Tasks folder. A user can do any of the following with the VA:
[0894] Request a task summary
[0895] Browse tasks
[0896] List tasks
[0897] Read tasks
[0898] Get more detail about a task
[0899] Create a task
[0900] Set reminders
[0901] Respond to a task request
[0902] Delete a task
[0903] Mark a task as complete
[0904] A user can receive task requests that other people send (task requests are treated as incoming messages by the VA). However, a user cannot use the VA to generate and send task requests.
[0905] A user can request a summary of tasks by saying, “What are my tasks?” The VA responds by telling the user how many tasks the user has that are due today, overdue, due in the future or have no due date.
[0906] A user can browse tasks by saying, “Browse my tasks.” The VA responds by reading the subject and due date for each task, beginning with the first task.
[0907] A user can request a list of all tasks by saying, “List my tasks.” The VA responds by telling the user how many tasks the user has, then reading the subject and due date for each task.
[0908] A user can filter the task list by any of the following:
[0000]
Type of Filter
Example
Category (future, due today, due tomorrow,
List my tasks due today
overdue, no due date)
First or last
List my first task
Next or previous
List my next task
A combination of the other filters
List my first task due today
[0909] A user can request that the VA read all tasks by saying, “Read my tasks.” The VA tells the user how many tasks the user has, then reads the subject, date, whether a reminder has been set, and, if so, the reminder date and time, and the body, for each task.
[0910] A user can filter the tasks to be read by the same criteria as a task list:
[0000]
Type of Filter
Example
Category (future, due today, due
Read my tasks due today
tomorrow, overdue, no due date)
First or last
Read my first task
Next or previous
Read my next task
A combination of the other filters
Read my first task due today
[0911] If a user needs more detailed information about a task than the VA provides by reading, the user can say, “Get more detail,” and the VA responds by providing the information regarding subject, due date, person who assigned the task, whether a reminder has been set, start date, status, priority, and percent complete.
[0912] To create a new task, the user should say, “Create a task.” The VA then asks the user to specify the task subject (description), due date, and whether the user wants a reminder.
[0913] A user can set a reminder so that the VA will remind the user of a task. A user can choose to be reminded either by telephone or by pager. The VA plays a “whisper” tone to notify the user of a reminder. This tone is different from the “whisper” tone for an incoming call. The VA does not actually deliver the reminder until the user either completes or cancels the current function. In order for the VA to deliver reminders, a user should first set the correct options in the Microsoft Outlook user preferences. The option that controls reminders is Notify me on reminders via on the VA Preferences Phone/Pager tab.
[0914] A user can respond to a task request by saying, “Reply” while the VA is listing or reading it. The VA then lists the following options: Reply or Forward.
[0915] When a user responds to a task request, the VA asks if the user wants to add an annotation. If a user chooses to forward a task request, the VA requests the name of the contact to whom the user is forwarding the task.
[0916] To delete a task, the user should say, “Delete this task.” The task that user deletes should be the current task (that is, the task that the VA is listing or reading. The VA responds with “Deleting task . . . done.” When a user attempts to delete a task request, the VA asks if the user wants to send a rejection message to the sender.
[0917] To mark a task as complete, the user should say, “Mark it as complete” while the VA is listing or reading the task. The VA responds with “Done. Task marked as complete.”
[0918] Using the Telephone Keypad to Issue Commands
[0919] As an alternative to voice commands, the VA allows a user to use the telephone keypad to issue commands. To use this feature, the user should press a predetermined key, such as the star key (*), to enable a choice prompt mode. When the choice prompt mode is enabled, the VA prompts the user with the available choices. A user can then use the keypad to select the desired choice.
[0920] If conditions are favorable for speech recognition, for example, the user is in a quiet car, the user may elect to interact with the virtual assistant by speech. If, however, conditions are not favorable for accurate speech recognition, for example, there is background noise or signal quality on a wireless handset is low, the user may elect to enter a choice prompt mode, as described above. As mentioned above, the user could selectively enter choice prompt mode by pressing a predetermined key, such as the star key, on a telephone keypad.
[0921] A choice prompt is a prompt, that is, output, from the virtual assistant that prompts the user to indicate a choice or take some specific action. As shown in FIG. 37 , the choice prompt is divided into active segments, which correspond to the choices that are selectable by the user. User input during a particular active segment indicates that the user desires to select the choice being provided during the active segment of the choice prompt. For example, as illustrated in FIG. 37 , the choice prompts could be, “Would you like to send your message (prompt 1 ) 440 , review your message (prompt 2 ) 442 , or discard your message (prompt 3 ) 444 ?” The corresponding active segments are 450 , 452 and 454 , respectively. The user can depress a predetermined key on the telephone keypad, or speak a predetermined utterance, during the active segment that corresponds to the desired choice. Thus, by pressing the star key, or saying “Yes,” while prompt 1 440 is being spoken would signify the user has selected “send the message.” Similarly, by pressing the star key, or saying “Yes,” while prompt 2 442 is being spoken would signify the user has selected “review the message.” Finally, by pressing the star key, or saying “Yes,” while prompt 3 444 is being spoken would signify the user has selected “discard the message.” It should be noted that saying “Yes” or pressing the star key would have no selective effect outside of the active window of the choice prompt stream.
[0922] Once in choice prompt mode, the virtual assistant could be configured to accept only DTMF input. In other words, voice input would not be possible because the speech recognition engine would not interpret spoken utterances. Similarly, the ability of a user to “barge in” would be disabled. Thus, no sounds, whether spoken or extraneous background noises, would interrupt the virtual assistant. The only acceptable input would be the predetermined DTMF.
[0923] Alternatively, a user could select to enter a choice prompt mode where only specific voice commands, such as “yes” and “no” would be interpreted by the speech recognition engine. The user could selectively exit choice prompt mode by pressing the star key again.
[0924] Alternatively, the virtual assistant could be configured to permit the user to exit the voice interface and enter the choice prompt mode to complete a specific task. Then, once the specific task is complete, the user would automatically exit the choice prompt mode and re-enter the voice use interface for further interaction with the virtual assistant by speech.
[0925] In an alternative embodiment, the default option is the first option recited by the VA. If the user knows that its intends to choose the default option, the user can press the star key twice (**), which enables the Star mode and chooses the default option in one step.
[0926] A user can use a combination of voice and keypad commands to perform a task.
[0927] The above description of the preferred embodiments detail many ways in which the present invention can provide its intended purposes. Programmers skilled in the art are able to produce workable computer programs to practice the teachings set forth above. While several preferred embodiments are described in detail hereinabove, it is apparent that various changes might be made without departing from the scope of the invention, which is set forth in the accompanying claims.
|
A computer-based virtual assistant includes a virtual assistant application running on a computer capable of receiving human voice communications from a user of a remote user interface and transmitting a vocalization to the remote user interface, the virtual assistant application enabling the user to access email and voicemail messages of the user, the virtual assistant application selecting a responsive action to a verbal query or instruction received from the remote user interface and transmitting a vocalization characterizing the selected responsive action to the remote user interface, and the virtual assistant waiting a predetermined period of time, and if no canceling indication is received from the remote user interface, proceeding to perform the selected responsive action, and if a canceling indication is received from the remote user interface halting the selected responsive action and transmitting a new vocalization to the remote user interface. Also a method of using the virtual assistant.
| 6
|
This application is a continuation of Ser. No. 09/296,921, now U.S. Pat. No. 6,515,413 B1 filed on Apr. 22, 1999.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to light filter systems and more particularly, but not by way of limitation, to infrared light filter systems for fluorescent lighting.
2. Description of the Problem and the Related Art
Existing night vision systems collect light that cannot be seen by the human eye and focus that light on an image intensifier. Inside the image intensifier, a photo cathode absorbs the collected light energy and converts it into electrons. These electrons are then drawn through a microchannel plate (which multiplies the electrons thousands of times) to a phosphor screen. When the multiplied electrons strike the phosphor screen, they cause the screen to emit light that the human eye can see. Because the phosphor screen emits light in exactly the same pattern and degrees of intensity as the collected light, the bright, nighttime image viewable on the phosphor screen corresponds precisely to the outside scene being viewed.
The night vision industry has progressed through three stages or “generations”: generation I, II and III. Although generation I technology is generally obsolete, generations II and III are in widespread use. Generation II technology, for instance, intensifies light up to 20,000 times, which means that this technology is effective in ¼ moonlight. The newest technology, generation III technology, however, provides a substantially higher intensification than does generation II technology. Furthermore, generation III technology, unlike generation I and II, is sensitive to near-infrared light, i.e., light in the 600-900 nanometer region. The ability of generation III technology to intensify light at and near the infrared region is important because most natural backgrounds reflect infrared light more readily than visible light. Thus, when infrared reflectance differences between discernable objects are maximized, viewing contrast increases and potential terrain hazards and other objects are distinguishable. Generation III technology's infrared capabilities complement this phenomenon and, accordingly, produce a sharp, informative image of an otherwise unviewable nighttime scene.
Furthermore, generation III technology can be modified to incorporate filters that substantially block visible light. These types of systems, known as aviator night vision systems, amplify light only in the near infrared and infrared region. Thus, aviator night vision systems allow the user to more clearly view terrain hazards and the like without interference from visible light.
Aviator night vision systems are useful in environments containing generated light such as light generated by an incandescent bulb. For example, a pilot of a search and rescue helicopter can require night vision capabilities to locate victims at night. The pilot needs to see not only the terrain being searched, but also the lighted helicopter instrument display. Furthermore, others aboard the helicopter may need internal lighting to perform their individual tasks, e.g., navigation. With standard generation III technology, the pilots ability to see the terrain would be greatly hampered by the visible light produced by the display and the lights used by others in the helicopter. In other words, standard generation III technology can pick-up and intensify the relatively high-intensity visible light produced inside the helicopter rather than pick-up and intensify the relatively low-intensity light on the surrounding terrain. In fact, in many cases the standard generation III night vision system could become momentarily inoperable because too much visible light reaches the collector and in effect, shuts down the entire night vision system. The pilot is thus left to fly blind or at least without night vision capabilities. Either option is likely unacceptable.
Aviator night vision systems, unlike standard generation III technology, filter out the visible light and leave only infrared light to stimulate the viewable phosphor screen. Accordingly, the visible light produced by displays or other lights inside the helicopter will not interfere with aviator night vision systems. The pilot wearing an aviator night vision system, thus, can watch the night terrain and attempt to locate victims without interference from visible light produced inside the helicopter.
Light sources, however, generally produce both visible light and infrared light. Thus, the helicopter display and any other light source used in the helicopter can produce infrared light that will interfere with even aviator night vision systems. For most light sources, however, infrared light can be filtered out, thereby minimizing its affect on aviator night vision systems. For example, existing displays and incandescent bulbs can be filtered so that the emit very little infrared light. Thus, if a search and rescue helicopter was equipped with infrared filtered lighting, the pilot could use an aviator night vision system without interference from the lighted display or any other internal lighting.
Although infrared light can be filtered from many light sources, infrared light, has not previously been effectively filtered from conventional type fluorescent lighting. Accordingly, an invention is needed that effectively filters infrared light from fluorescent lighting. Furthermore, an invention is needed that effectively filters infrared light from fluorescent lighting and that is easily adapted to typical fluorescent lighting and assemblies. One skilled in the art can appreciated that such an invention would have application anywhere that night vision systems are used or anywhere that infrared needs to be blocked. For example, the present invention even can be used to prevent the detection of fluorescent lights by night vision systems.
SUMMARY OF THE INVENTION
To remedy the deficiencies of existing systems and methods, the present invention provides a method and apparatus that effectively filters infrared light from fluorescent lighting and that is easily adapted to typical fluorescent lighting and assemblies.
One exemplary embodiment of the present invention includes a transparent tube for receiving a fluorescent lamp wherein the transparent tube includes a first end, a second end, an inner surface and an outer surface. This embodiment further includes an infrared block located adjacent to the inner surface of the transparent tube. The infrared block is for substantially blocking infrared light from passing through the transparent tube. Furthermore, this embodiment includes a first cap for capping the first end of the transparent tube and a second cap for capping the second end of the transparent tube.
BRIEF DESCRIPTION OF THE DRAWINGS
Various objects and advantages and more complete understanding of the present invention will become apparent and more readily appreciated by reference both to the following Detailed Description and to the appended claims when taken in conjunction with the accompanying Drawings wherein:
FIG. 1 a is an exploded, frontal perspective view of an exemplary filter assembly in accordance with the present invention;
FIG. 1 b is a cross-sectional view of a filter layer used with the filter assembly of FIG. 1 a;
FIG. 2 illustrates a frontal view of an alternate embodiment of a filter assembly in accordance with the present invention; and
FIG. 3 illustrates a frontal view of a fluorescent fixture including a filter cover in accordance with the present invention.
DETAILED DESCRIPTION
Although the present invention is open to various modifications and alternative constructions, preferred exemplary embodiments shown in the drawings are described herein in detail. It is to be understood, however, that there is no intention to limit the invention to the particular forms disclosed. One skilled in the art can recognize that there are numerous modifications, equivalences and alternative constructions that fall within the spirit and scope of the invention as expressed in the claims.
Accordingly, to overcome the deficiencies of existing technology and to fill a long-felt commercial need, the present invention provides an effective infrared filter for fluorescent lighting. Furthermore, the present invention provides an effective infrared filter for fluorescent lighting that is easily adapted to typical fluorescent lighting. Additionally, the present invention can filter light in accordance with MIL Specification MIL-L-85762A, which is incorporated herein by reference.
Referring now to FIG. 1 a , there is illustrated an exploded, frontal perspective view of an exemplary filter assembly 100 in accordance with the present invention. The filter assembly 100 includes a transparent, cylindrical tube 110 with a diameter and length slightly greater than those of the fluorescent tube 105 , which can be of any size or type. The filter assembly also includes a cap 115 placed on each end of the tube 110 . Although both caps 115 may be removable, it is only necessary that one cap 115 be removable. As long as one cap 115 is removable, that cap 115 can be removed and the fluorescent tube 105 can be inserted into or removed from the tube 110 . Furthermore, if one cap 115 is not removable, that cap 115 can be used to properly align the fluorescent tube 105 once placed inside tube 110 .
Each cap 115 is perforated to receive the electrical contacts 120 of the fluorescent tube 105 . The electrical contacts 120 pass through the cap 115 and can engage the electrical connections of a fluorescent fixture (not shown). Gaskets 125 are placed between the caps 115 and the ends of the fluorescent tube 105 and prevent light from escaping through the perforations in the cap 115 . Furthermore, the gaskets 125 can slide over the electrical contacts 120 and thereby form a very effective light seal.
Because of the light seal formed by the caps 115 and the gaskets 125 , all light generated by the fluorescent tube 105 must pass through the tube 110 . However, a filter layer 130 (which can be flexible) is located between the tube 110 and the fluorescent tube 105 . Therefore, all light produced by the fluorescent tube 105 must pass through the filter layer 130 where infrared light and near infrared light produced by the fluorescent tube 105 are blocked. Thus, all light emitted from the filter assembly 100 will be essentially infrared free and will not interfere with aviator night vision systems.
The filter assembly 100 can also include an opaque light blocker 135 that is preferably made of a scratch resistant material. The opaque light blocker 135 focuses the light emitted by the fluorescent tube 105 into a particular pattern. Furthermore, the opaque light blocker 135 can prevent light emitted from the filter assembly 100 from striking particular objects. For example, the opaque light blocker 135 can prevent light emanating from the filter assembly 100 from striking the interior portion of the fluorescent fixture (not shown) holding the filter assembly. Directing light away from the interior portion of a fluorescent fixture is important because even the filtered light emanating from filter assembly 100 will generate infrared light if it strikes red paint. Although the interior of most fluorescent fixtures are painted white, most white paint contains traces of red that can reflect infrared light. Thus, the opaque light blocker 135 can prevent the filtered light from striking areas, such as the interior of a fluorescent fixture, that will reflect infrared light and interfere with aviator night vision systems.
As can be appreciated, the present invention permits typical fluorescent lamps to easily and quickly be converted to only emit infrared-free light. For example, a typical fluorescent tube 105 can be converted to a non-infrared light emitting fluorescent source by merely removing one of the caps 115 from the tube 110 . Next, gaskets such as gaskets 125 are placed over the electrical contacts 120 on both ends of the fluorescent tube 105 . The fluorescent tube is then inserted into the tube 110 and aligned so that the electrical contacts 120 pass through the perforations in the non-removed cap 115 . Next, the previously-removed cap 115 is placed onto the tube 110 such that the electrical contacts 120 pass through the perforations in the cap 115 . Finally, the entire filter assembly, including the fluorescent tube, can be inserted into a standard fluorescent fixture.
Referring now to FIG. 1 b there is illustrated a cross-sectional view of a filter layer 130 used with the filter assembly 100 of FIG. 1 a . The filter layer 130 can include four individual layers, all of which can be flexible. Going from outside to inside, the layers are green filter 140 , infrared block 145 , green filter 150 and green filter 155 . Because infrared block 145 can be sensitive to heat, in this embodiment, it is not placed directly adjacent to the fluorescent tube 105 .
Furthermore, the individual filter layers do not necessarily need to cover the entire surface area of the tube 105 as is illustrated in FIGS. 1 a and 1 b . Rather, in one embodiment, particular ones or even all of the layers of filter layer 130 cover only that portion of the tube 110 that is not covered by the opaque light blocker 135 .
Although particularly good results have been obtained by using the above-described four layers, a significant portion of infrared light produced by the fluorescent tube 105 can be blocked by using just the infrared block 145 and either one green filter or two green filters, which can be various shades of green, such as green filter 155 . Furthermore, although any effective infrared block can be used with the present invention, particularly good results have been obtained by using infrared block number 577-1086 produced by Hoffman Engineering, which is located at 22 Omega Drive, 8 Riverbend Center, P.O. Box 4430, Stamford, Conn. 06907-0430.
Green filter layers, such as green filter layer 155 , can be added or removed to alter the transmission characteristics of filter assembly 100 . As one skilled in the art can appreciate, if more light should be emitted, a green filter layer can be removed. Alternatively, if less light should be emitted, an additional green filter layer can be added. Furthermore, the transmission characteristics of the filter assembly 100 can also be altered by changing the size of the opaque light blocker 135 . For example, if the opaque light blocker 135 is enlarged to cover 75% of the outside surface area of the tube 110 , less light will be emitted than when the opaque light blocker 135 only covers 50% of the outside surface area of the tube 110 .
In another embodiment of the present invention, the multiple layers of filter layer 130 are combined so that the same filtering and transmission properties can be obtained with a single layer filter or at least fewer layers. Furthermore, the filter layer 130 can be eliminated as a distinct element by incorporating the properties of the filter layer directly with the tube 110 . In this embodiment, the infrared block and transmission reducers, if necessary, are formed directly into the tube 110 .
Referring now to FIG. 2, there is illustrated a frontal view of an alternate embodiment of a filter assembly in accordance with the present invention. This embodiment includes a filter assembly 200 that filters infrared light from fluorescent tube 205 . The filter assembly 200 includes a transparent cover 210 that fits over the fluorescent tube 205 . The filter assembly 200 also includes a cap 215 (which can be opaque or clear) that is perforated to receive the electrical connectors 220 of the fluorescent tube 205 . The electrical connectors 220 pass through the cap 215 and thereby can engage a fluorescent fixture (not shown). Gaskets 225 prevent unfiltered light from escaping through the perforations in the cap 215 .
Additionally, the cover 210 can include an integrated infrared filter and transmission reducer (not shown). Alternatively, a flexible filter layer similar to filter layer 130 of FIG. 1 can be placed between the fluorescent tube 205 and the cover 210 .
Referring now to FIG. 3, there is illustrated a frontal view of a fluorescent fixture including a filter cover in accordance with the present invention. This embodiment includes a fluorescent fixture 300 such as would be suspended from a ceiling. The fluorescent fixture 300 includes a base 310 for receiving the fluorescent tube 305 and a cover 315 for blocking the infrared light generated by the fluorescent tube 305 .
The cover 315 comprises an integrated infrared filter and, if needed, an integrated transmission reducer. For example, the cover 315 can be formed of a plastic or plastic-type material that incorporates infrared filters and transmission reducers. Alternatively, a filter layer, such as filter layer 130 (shown in FIG. 1) or an equivalent single layer, can be attached to the cover 315 such that the fluorescent fixture 300 emits only filtered light.
In summary, the present invention provides an effective infrared filter for fluorescent lighting. Furthermore, the present invention provides an effective infrared filter for fluorescent lighting that is easily adapted to typical fluorescent lighting. Additionally, the present invention can filter light in accordance with MIL Specification MIL-L-85762A.
Those skilled in the art can readily recognize that numerous variations and substitutions may be made in the invention, its use and its configuration to achieve substantially the same results as achieved by the exemplary embodiments described herein. Accordingly, there is no intention to limit the invention to the disclosed exemplary forms. Many variations, modifications and alternative constructions will fall within the scope and spirit of the disclosed invention as expressed in the claims.
|
A method and apparatus that effectively filters infrared light from fluorescent lighting and that is easily adapted to typical fluorescent lighting and assemblies. A transparent tube is provided for receiving a fluorescent lamp wherein the transparent tube includes a first end, a second end, an inner surface and an outer surface. An infrared block is located adjacent to the inner surface of the transparent tube. Furthermore, a first cap is provided for capping the first end of the transparent tube and a second cap is provided for capping the second end of the transparent tube.
| 7
|
CLAIM OF PRIORITY UNDER 35 U.S.C. §120
The present Application for Patent is a continuation-in-part of U.S. patent application Ser. No. 13/567,154, entitled “EXTENDING CONTROL PLANE FUNCTIONS TO THE NETWORK EDGE IN AN OPTICAL TRANSPORT NETWORK,” filed Aug. 6, 2012, pending, assigned to the assignee hereof, and expressly incorporated herein by reference in its entirety. The present non-provisional patent also claims the benefit of priority of co-pending Indian Patent Application No. 1500/DEL/2012, filed on May 16, 2012, and entitled “EXTENDING CONTROL PLANE FUNCTIONS TO THE NETWORK EDGE IN AN OPTICAL TRANSPORT NETWORK,” the contents of which are incorporated in full by reference herein.
FIELD OF DISCLOSURE
The present application relates generally to management of optical communications networks, and more specifically, to methods of extending control plane functions to the network edge in an optical transport network.
BACKGROUND
FIG. 1A schematically illustrates the logical architecture of an Optical Transport Network (OTN) in accordance with ITU-T recommendation G.8080/Y.1304, entitled Architecture for the Automatically Switched Optical Network (ASON), the entire content of which is incorporated herein by reference. As may be seen in FIG. 1A , the network 2 is logically divided into a transport plane 4 and a control plane 6 .
The Transport Plane 4 comprises a plurality of switches 10 interconnected by Physical Interfaces (PIs) 12 , and is responsible for transporting subscriber traffic via end-to-end connections provisioned through the network. The Control Plane 6 comprises an Optical Connection Controller (OCC) 14 associated with each switch 10 of the transport plane 4 , and is responsible for resource and connection management within the transport plane 4 . In the illustrated architecture, one OCC 14 is associated with a respective one switch 10 for clarity. In fact, the ASON permits an OCC 14 to manage multiple switches 10 , if desired. Each OCC 14 is connected to its corresponding switch 10 of the transport plane 4 via a Connection Controller Interface (CCI) 16 which enables the respective OCC 14 to implement control plane functionality for its corresponding switch 10 . Within the Control Plane 6 , the OCCs 14 are interconnected via Network to Network Interfaces (NNIs) 18 , and provide a set of network resource and connection management functions. These functions may, for example, include: network topology discovery (resource discovery); address assignment; path computation, connection set-up/tear-down; connection protection/restoration; traffic engineering; and wavelength assignment. Other management functions can be implemented by the control plane 6 , as desired.
A physical node of the network will typically incorporate both a Transport Plane switch 10 and its corresponding Control Plane OCC 14 , although this is not essential. In some cases, a Transport Plane switch 10 and its corresponding Control Plane OCC 14 may be provided in separate physical machines. For example, the respective OCCs 14 of one or more switches 10 may be hosted on a server (not shown).
Client premised equipment (CE) 20 , which may be a server or a router, for example, can send and receive packets that contain information for both the Transport Plane 4 and the Control Plane 6 . For this purpose, the CE may be connected to a switch 10 of the Transport Plane 4 via a PI 12 , and to its corresponding OCC 14 via a User Network Interface (UNI) 22 .
FIG. 1B presents a simplified view of the network architecture of FIG. 1A , in which the switches 10 and their associated OCCs 14 are represented by network nodes 24 connected by inter-node links 26 (each of which includes a PI 12 and its corresponding NNI 18 ). Similarly, the CE 20 is represented as being connected to a network node 24 via an access link 28 which, in the illustrated embodiment, includes a PI 12 and a UNI 22 .
Referring to FIG. 2 , it is customary to extend the architecture of FIG. 1B to implement access gateways (AGs) 30 between the CEs 20 and the network 2 . An access gateway 30 may also be referred to as an access server or an aggregation server. The function of the access gateway 30 is to provide an interface between one or more CEs 20 and the network 2 . Among other things, an AG 30 enables a service provider to aggregate traffic flows to and from multiple CEs 20 , which increases the number of CEs 20 that can access the network 2 , while making better use of the bandwidth capacity of the access links 28 to the network 2 . The use of an AG 30 also simplifies the implementation of dual-homed connections to the network 2 , which has a benefit of removing a single point of failure in the path to and from the CEs 20 . In the example of FIG. 2 , AG- 1 is dual homed to the network 2 via respective access links 28 to network nodes A and B, while AG-m is single-homed to the network 2 via an access link 28 to node B.
It would be desirable to extend the control plane 6 to include the AGs 30 . This would be beneficial in that, among other things, each AG 30 would then be able to participate in topology discovery, path computation, connection set-up/tear-down and failure recovery functions offered by the OTN control plane 6 . As is known in the art, topology discovery requires the exchange of link state messages between each of the OCCs 14 of the control plane 6 , and the use of such state messages to accumulate a respective topology database for each OCC 14 . Such topology database can then be used by an OCC 14 to compute connection routes through the network 2 . Open Shortest Path First (OSPF) is a well-known protocol which defines various types of Link State Advertisement (LSA) messages that may be used for this purpose. Other protocols are also known, which also use inter-OCC messaging for topology discovery and route computation. For ease of description in this application, explicit reference will be made to LSA messages, it being understood that such references are also intended to encompass other message types and protocols that may be used in the control plane to implement topology discovery and route computation functions for the network 2 .
In a full-mesh network, both the volume of LSA traffic and the size of the topology database increases with N 2 , where N is the number of nodes participating in the control plane 6 . In a network environment in which there are a large number of AGs 30 , extending the control plane 6 to include the AGs 30 can lead to a proliferation of LSA traffic and require a very large topology database, both of which may degrade the topology discovery, route computation, and failure recovery functions of the control plane 6 .
Techniques that enable extension of the OTN control plane 6 without unduly degrading control plane performance remain highly desirable.
SUMMARY
An aspect of the present disclosure provides a method of extending control plane functions to the network edge in an optical transport network having a transport plane for carrying subscriber traffic within end-to-end connections, and a control plane for managing at least a portion of resources of the transport plane allocated to the connections.
An exemplary embodiment provides a method for resource and connection management in a network with a core domain and at least one metro domain in communication with the core domain. The exemplary embodiment may include designating a first set of control-plane enabled nodes of the core domain as core nodes, each core node being operable to route subscriber traffic between a pair of neighbor core nodes in the core domain; designating a second set of control-plane enabled nodes of a metro domain as metro nodes, each metro node being operable to route subscriber traffic between a pair of neighbor metro nodes in the metro domain; designating a core node that is connected to a metro node as a host node; assigning summary information to each metro node; and advertising the summary information to core nodes in the network.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings are presented to aid in the description of embodiments of the invention and are provided solely for illustration of the embodiments and not limitation thereof. Further features and advantages of the present invention will become apparent from the following detailed description, taken in combination with the appended drawings, in which:
FIGS. 1A and 1B are block diagrams schematically illustrating the logical structure of an Automatically Switched Optical Network (ASON) known in the prior art;
FIG. 2 is a block diagram schematically illustrating extension of the ASON structure of FIG. 1A to include access gateways between the ASON and Customer premised equipment;
FIG. 3 is a block diagram schematically illustrating a network implementing a first representative embodiment of the present invention; and
FIG. 4 is a block diagram schematically illustrating a network implementing a second representative embodiment of the present invention.
FIG. 5 is a block diagram depicting an exemplary embodiment of the disclosure of a core network connected to a plurality of metro networks.
FIG. 6 depicts an exemplary embodiment showing a unique metro network identifier.
FIG. 7 depicts an exemplary embodiment showing visibility of a node.
FIGS. 8A and B depict an exemplary embodiment of a hierarchical metro architecture.
FIG. 9 depicts an exemplary embodiment of a two level hierarchical architecture.
FIG. 10 depicts an exemplary embodiment of a two level Hierarchical Metro Reachability architecture.
FIG. 11 depicts an exemplary embodiment of a two level Hierarchical Visibility architecture.
It will be noted that throughout the appended drawings, like features are identified by like reference numerals.
DETAILED DESCRIPTION
Aspects of the invention are disclosed in the following description and related drawings directed to specific embodiments of the invention. Alternate embodiments may be devised without departing from the scope of the invention. Additionally, well-known elements of the invention will not be described in detail or will be omitted so as not to obscure the relevant details of the invention.
The word “exemplary” is used herein to mean “serving as an example, instance, or illustration.” Any embodiment described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments. Likewise, the term “embodiments of the invention” does not require that all embodiments of the invention include the discussed feature, advantage or mode of operation.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention. As used herein, the singular forms “a,” “an,” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises”, “comprising,” “includes,” and/or “including,” when used herein, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Further, many embodiments are described in terms of sequences of actions to be performed by, for example, elements of a computing device. It will be recognized that various actions described herein can be performed by specific circuits (e.g., application specific integrated circuits (ASICs)), by program instructions being executed by one or more processors, or by a combination of both. Additionally, these sequence of actions described herein can be considered to be embodied entirely within any form of computer readable storage medium having stored therein a corresponding set of computer instructions that upon execution would cause an associated processor to perform the functionality described herein. Thus, the various aspects of the invention may be embodied in a number of different forms, all of which have been contemplated to be within the scope of the claimed subject matter. In addition, for each of the embodiments described herein, the corresponding form of any such embodiments may be described herein as, for example, “logic configured to” perform the described action.
For the purposes of the present disclosure, a distinction is made between the core nodes and tail nodes, based on the type of transport plane traffic forwarding that can be supported by each node. For the purposes of the present disclosure, a “core node” is considered to be a node through which transport plane traffic can be routed between two adjacent core nodes. The set of core nodes within the network may be taken together as defining a “core network” or, equivalently, a “network core”. In contrast, a “tail node” is considered to be a node that cannot operate to route transport plane traffic between two adjacent core nodes, but rather is limited to sourcing (and sinking) traffic to (and from) the network and routing traffic between its directly subtending CEs. In addition to these definitions, it is convenient to identify each core node through which a tail node may obtain access to the network. Such core nodes may be referred to as “host nodes”.
In the example of FIG. 2 , each node 24 represents a core node, because it can route subscriber traffic between two neighbor core nodes 24 within the core network 32 . For example, node A can route subscriber traffic between neighbor (core) nodes D and B. On the other hand, each AG 30 is an example of a tail node, because it only operates to forward traffic between its connected CE(s) 20 and a core node 24 of the network 2 . As such, an AG 30 can only source (and sink) subscriber traffic flows into (and from) the network 2 , or route subscriber traffic flows between two CEs 20 connected to itself Even in the case of dual homed AG- 1 , subscriber traffic cannot be routed between neighbor (core) nodes A and B (e.g. via access links 28 a and 28 b ). Any traffic arriving at AG- 1 from core node A, for example, must either be passed to a CE 20 , or must be dropped; it cannot be forwarded to core node B.
It should be noted that tail nodes are not limited to AGs 30 hosting CEs 20 . A tail node can be any node that operates solely to source and sink transport plane traffic to and from the network 2 . Thus, for example, a CE 20 which is directly connected to a core node 24 can be treated as a tail node, if desired. Similarly, a gateway between two networks (or sub-networks) can be a tail node if it serves only as a transit point for traffic flows originating in one network, and terminating in the other network (and so is seen as a traffic source or sink in any given one of the involved networks).
As may be appreciated, the distinction between tail nodes and core nodes is based on the role that each node plays in the network, rather than its physical construction or location. Thus it is possible for a tail node and a core node to be physically identical, if desired, in which case the difference between the two types of nodes would lie in their respective control software. Similarly, there is no requirement for core nodes and tail nodes to be installed at geographically dispersed locations, although it is contemplated that this will normally be the case.
In a conventional Optical Transport Network (OTN) in accordance with ITU-T recommendation G.8080/Y.1304, the span of the control plane 6 is limited to core nodes, so that the control plane 6 can provide (inter alia) topology discovery, route computation, connection set-up/tear-down and protection/restoration functions for subscriber traffic flows within the network. Because the number of tail nodes can be very large (e.g. reaching 10000 or more in a large network), tail nodes are excluded from the control plane 6 , so as to avoid proliferation of control plane messaging and exponential growth of control plane messaging and topology databases, both of which may tend to degrade control plane performance.
The Applicants have discovered that the control plane 6 can be extended to provide control plane functionality to tail nodes, by implementing conventional OCC functionality in each tail node, and suitably controlling the size and propagation of LSAs through the host nodes.
Referring to FIG. 3 , there is shown a representative embodiment in which a set of three control-plane enabled tail nodes 34 (AG- 1 , AG- 2 and AG- 3 ) are logically associated with an area 36 and connected to a host node 24 H via respective access links 28 . A topology database 38 associated with the area 36 is populated with topology information of the network 2 , and thus can be used in a conventional manner to enable the tail nodes 34 to compute end-to-end routes through the network 2 using conventional methods. Typically, the topology database 38 used by a given control plane enabled tail node 34 is maintained by the OCC 14 associated with that tail node 34 . Where two or more tail nodes 34 are managed by a common OCC 14 , those tail nodes 34 will share a common topology database 38 . On the other hand, when tail nodes 34 are not managed by a common OCC 14 , then each tail node 34 will utilize its own topology database 38 .
The set of tail nodes 34 may be geographically dispersed or may be physically co-located, as desired. In the case of geographically dispersed tail nodes 34 , each tail node 34 may maintain a respective instance of the topology database 38 . On the other hand, co-located tail nodes 34 may share a common instance of the topology database 38 , if desired. Connections over the access links 28 between tail nodes 34 and the host node 24 H may utilize either User-Network-Interface (UNI) or Network-Network-Interface (NNI) connections in the control plane, as desired.
The logical allocation of tail nodes 34 to the area 36 may be based on any suitable criteria. In the embodiment of FIG. 3 , the chosen criterion is connection to the host node 24 H, such that the area 36 encompasses all of the tail nodes 34 connected to the host node 24 H. Other criteria may be used, as will be apparent from the following description.
The area 36 is preferably referenced using a unique area identifier 40 , which may be defined in any suitable manner. In the embodiment of FIG. 3 , the area identifier 40 is derived from respective addresses of the involved tail nodes 34 . In particular, the area 36 encompasses three tail nodes 34 , namely AG- 1 , AG- 2 and AG- 3 , whose addresses are “1.2.3.1”, “1.2.3.2” and “1.2.3.3”, respectively. All of these addresses contain a common prefix portion “1.2.3”, which may conveniently be used as the area identifier 40 as shown in FIG. 3 . In an alternative embodiment, the area identifier 40 may be derived from the respective address of the host node 24 H. Since every core node 24 in the network has a unique network address, derivation of the area identifier 40 from the host node address enables the host node 24 H or a management server (not shown) in communication with the host node 24 H to independently derive an area identifier 40 that is unique within the network 2 . This arrangement is advantageous in that it eliminates the need for a network service provider to manually provision area identifiers 40 while at the same time ensuring that each area identifier 40 is unique across the network 2 .
The host node 24 H is preferably provided with a network topology database 42 . The network topology database 42 may be populated in a convention manner based on LSAs received by the host node 24 H from the other core nodes 24 in the network 2 , and so may be used in a convention manner for computation of routes through the network 2 . As will be described in greater detail below, the network topology database 42 may also be populated based on LSAs received from the tail nodes 34 connected to the host node 24 H, and used to enable computation of routes between the host node 24 H at its attached tail nodes 34 .
It is a simple matter to implement OCC functionality for each tail node 34 , which thereby enables the upgraded tail node 34 to participate in the control plane 6 . Consequently, each upgraded (i.e. control-pane enabled) tail node 34 is capable of exchanging LSAs with its connected host node 24 H, populate its topology database 38 , and compute routes through the network 2 in a conventional manner.
The host node 24 H is configured (for example operating under suitable software control) to implement different LSA forwarding rules, for example depending on whether LSA messages are received from one of its attached tail nodes 34 or from neighboring core nodes 24 in the network 2 .
In some embodiments, LSAs received by the host node 24 H from a neighboring core node 24 are forwarded to its attached tail nodes 34 in a conventional manner. With this arrangement, a tail node 34 will receive LSAs originating from core nodes 24 in the network 2 , and so can populate its topology database 38 with information enabling it to calculate end-to-end routes through the network 2 .
In other embodiments, LSAs received by the host node 24 H from a neighboring core node 24 are not forwarded to its attached tail nodes 34 . With this arrangement, tail nodes 34 are not capable of calculating end-to-end routes through the network 2 , and must therefore interact with the host node 24 H to calculate end-to-end routes through the network 2 . Known techniques such as, for example Path Computation Element (PCE) and loose hop routing mechanisms may be used for this purpose.
On the other hand, LSAs received by the host node 24 H from its attached tail nodes 34 are not propagated into the network 2 in a conventional manner, but rather are used to derive summary information which is then advertised into the network 2 . The advertisement of summary information enables other nodes in the network 2 to populate their topology databases and compute end-to-end routes through the network 2 , while at the same time limiting the propagation of tail node originated LSAs into the network 2 .
In some embodiments, the summary information advertised by the host node 24 H comprises a summary address 44 which is based on the area identifier 40 of the area 36 to which each tail node 34 is allocated.
For example, in the embodiment of FIG. 3 , the summary address 44 is a four byte address comprising the three-byte area identifier 40 “1.2.3” concatenated with a one byte suffix portion populated with wildcard character (“x” in FIG. 3 ) to define a four-byte address that summarizes the respective addresses of the tail nodes 34 . Alternatively, the summary address may be comprised of only the three-byte area identifier 40 “1.2.3”, since the wildcard suffix is implicit. Advertisement of the summary address 44 into the network 2 by the host node 24 H ensures that connections destined for any of one of the tail nodes 34 will be routed through the host node 24 H.
As may be appreciated, each tail node 34 will be represented in the network 2 by a respective tail node address that conforms to the summary address 44 , but with the suffix portion populated with a node identifier that uniquely identifies a respective tail node 34 within its area 36 .
For ease of compatibility with link state messaging protocols being used in the network 2 , it is convenient to define the format of the summary address 44 in conformance with the addressing scheme of the network 2 . However, this is not essential. In general, any address format that enables the summary address 44 to be advertised into the network 2 , and which enables computation of routes to desired tail nodes 34 may be used. For example, other summarizable area identifier formats that can be used include those based on IPv6 or Network Service Access Point (NSAP).
As may be appreciated, the advertisement of summary address information into the network 2 by the host node 24 H means that a single LSA message and topology database entry can be used to represent a plurality of tail nodes 34 , thereby reducing control plane messaging relative to conventional methods. A further reduction in control plane messaging can be obtained by limiting the frequency with which the host node 24 H advertises changes in the state affecting its tail nodes 34 . In particular, under conventional control plane protocols, any change in state affecting a node immediately triggers a corresponding LSA message notifying the other nodes of the change. However, because tail nodes 34 are not critical for traffic routing in the network 2 , the host node 24 H may defer advertising tail node 34 state changes into the network 2 .
In some embodiments, the host node 24 H may advertise the state affecting its connected tail nodes 34 on a predetermined schedule, such as, for example once every half hour. Thus, for example, the host node 24 H may accumulate information of state changes affecting its tail nodes 34 during a given interval of time, and then generate a single LSA message containing a summary of changes accumulated during that interval, or simply the latest states affecting the tail nodes 34 .
In some embodiments, the host node 24 H may advertise the state affecting its connected tail nodes 34 after a predetermined number of changes have occurred. Thus, for example, the host node 24 H may accumulate information of state changes affecting its tail nodes 34 until a predetermined number of state changes have been recorded, and then generate a single LSA message containing a summary of the accumulated state changes, or simply the latest states affecting the tail nodes 34 .
In the embodiment of FIG. 3 , each of the tail nodes 34 is single-homed on core node A, acting as host node 24 H. FIG. 4 illustrates an embodiment in which the tail nodes 34 are dual-homed on host nodes A and B of the network 2 . Both of the host nodes 24 H can operate in a manner similar to that described above to advertise summary information of their attached tail nodes 34 into the network 2 . However, in embodiments in which the area identifier 40 is automatically derived by the host node 24 H, the algorithm implemented in each host node 24 H should operate to ensure that a single area identifier 40 is adopted and used by both host nodes 24 H, so that each tail node 34 is consistently identified in the network 2 . In embodiments in which the area identifier 40 is derived from the tail node addresses, this result will automatically be obtained simply by implementing the same algorithm in each host node 24 H.
Additionally, for each tail node 34 , one of the access links 28 may be disabled or blocked in a known manner. In FIG. 4 , this disabled/blocked state is indicated by an “X” in each of the affected access links 28 . Thus, in the example of FIG. 4 , tail node AG- 1 is currently connected to the network 2 via its access link 28 to core (host) node B, while tail nodes AG- 2 and AG- 3 are currently connected to the network 2 via their respective access links 28 to core (host) node A. It would be desirable to efficiently advertise this connectivity information to other nodes in the network 2 .
One method by which the host nodes 24 H can advertise connectivity information is to define a connectivity vector 46 , which may take the form of a binary sequence in which each bit position represents a respective one of the tail nodes 34 in the area 36 , and the binary value of that bit position represents whether or not that tail node 34 can be reached through the advertising host node 24 H. In use, each host node 24 H can derive a respective connectivity vector 46 based on the status of its inter-connecting links 28 to each tail node 34 in a given area 36 , and advertise the connectivity vector 46 along with the address summary 44 described above. Based on this information, other nodes in the network 2 can determine which of the host nodes 24 H can be used to reach a desired tail node 34 , and so compute routes to the desired tail node 34 via the appropriate one of the host nodes 24 . In the example of FIG. 4 , host node A advertises summary information 44 comprising summary address 44 “1.2.3.x” and connectivity vector 46 “0.1.1”, indicating that tail node addresses “1.2.3.2” and “1.2.3.3” (i.e. “1.2.3.x”; where x=2 and x=3) can be reached via host node A. Conversely, host node B advertises summary information comprising summary address 44 “1.2.3.x” and connectivity vector 46 “1.0.0”, indicating that tail node address “1.2.3.1” (i.e. “1.2.3.x”; where x=1) can be reached via host node B. By this means, other nodes in the network 2 can use the summary information to identify the host node 24 through which a desired tail node 34 can be reached, and compute a route through the network 2 to the desired tail node 34 through that host node 24 .
This approach is beneficial in that it increases the likelihood that routes can be successfully set up to desired tail nodes 34 on the first attempt, and thereby avoid undesirable control plane signaling associated with trying to find the appropriate host node 24 through which to route by “trial and error”, at a cost of advertising only one additional bit for each tail node 34 in a given area 36 and the summary area identifier 40 .
In some embodiments, each bit position of the connectivity vector 46 may be resolvable to determine the tail node address of a corresponding tail node 34 . In the example of FIG. 4 , the area identifier 40 “1.2.3” can be combined with the bit position of the connectivity vector 46 to obtain the tail node address of a specific one of the tail nodes 34 . Thus resolved, the tail node address can be used to calculate a route and set up a connection through the network 2 to the appropriate host node 24 , which can then use the tail node address to extend the connection through to the appropriate one of the tail nodes 34 .
In the foregoing examples, an area identifier 40 is used as a means to reference a set of one or more associated tail nodes 34 in the network 2 . In some embodiments, the association between the tail nodes 34 may simply be that they are connected to a given host node 24 . Alternatively, areas may be defined such that all of the tail nodes 34 within a given area 36 (and so assigned a given area identifier 40 ) have identical connections to the network 2 . Thus for example, the set of tail nodes 34 single homed on one host node 24 shown in FIG. 3 may be assigned to a first area 36 , while the set of tail nodes 34 dual-homed on host nodes 24 A and B in FIG. 4 may be assigned to a second area 36 . With this arrangement, a differentiation can be made between single-homed and dual-homed tail nodes 34 , which may, for example, be treated differently. For example, the use of a connectivity vector 46 is primarily useful for dual-homed tail nodes 34 . Thus, in some embodiments, the summary information advertised by a host node 24 may only include the connectivity vector 46 for those tail nodes 34 that are dual homed.
In the foregoing examples, the connectivity vector 46 is provided as a binary sequence in which each bit position represents a respective one of the tail nodes 34 in the area 36 , and the binary value of that bit position represents whether or not that tail node 34 can be reached through the advertising host node 24 H. This arrangement is beneficial in that it facilitates route computation with minimal overhead, as noted above. However, in some cases, it may be desirable to advertise connectivity information with a finer granularity than is possible with a single bit. Accordingly, if desired, the connectivity vector 46 may be formatted such that each tail node 34 is associated with a respective set of two of more bit positions, which may be used alone or in combination to convey information regarding connectivity between the advertising host node 24 and the involved tail node 34 .
For example, consider a network in which access links 28 may be configured in any one of four different bandwidths, including: zero (i.e. no bandwidth); Optical channel Data Unit (ODU)- 0 (i.e. 1.24416 Gbit/s); ODU- 1 (i.e. 2× ODU- 0 or approximately 2.49877 Gbit/s); and ODU- 2 (i.e. 4× ODU- 1 or approximately 10.03727 Gbit/s). This connectivity information may be conveyed by a connectivity vector 46 formatted to provide a set of two bit positions for each tail node 34 , with the binary value represented by the 2-bit set indicating a respective one of the four possible bandwidth states of the access link 28 between the advertising host node 24 and the relevant tail node 34 . Thus, for example, a value of “00” may indicate that the respective tail node 34 is not reachable; a value of “01” may indicate that the respective tail node 34 is reachable for connections up to an ODU- 0 bandwidth; a value of “10” may indicate that the respective tail node 34 is reachable for connections up to an ODU- 1 bandwidth; and a value of “11” may indicate that the respective tail node 34 is reachable for connections up to an ODU- 2 bandwidth. Other formats of the connectivity vector 46 and the meanings will become apparent to those of ordinary skill in the art, and may be used without departing from the intended scope of the appended claims.
Based on the foregoing description, it will be seen that the present technique utilizes a summary address 44 and connectivity vector 46 to advertise reachability of tail nodes 34 in the network. This arrangement offers numerous benefits over the conventional mechanisms by which information about tail nodes 34 and links 28 inter-connecting tail nodes 34 and host nodes 24 may be advertised in the network 2 . More particularly, if it was desired to advertise information about tail nodes 34 and access links 28 in the conventional manner then: a) each tail node 34 would advertise a Nodal LSA. At minimum this includes the address of the tail node 34 which is similar in size to the summary address 44 , i.e. 4 bytes; and b) For each link 28 inter-connecting a tail node 34 to a host node 24 , the tail node 34 would advertise a Link LSA, and the host node 24 would advertise a Link LSA also. Information in both Link LSAs would be pretty much the same (except local and remote information would be reversed) and such information can easily reach 100 bytes in some implementations (e.g.: OSPF-TE). So, in conventional methods, for each tail node 34 there would be advertisement of one Nodal LSA and two Link LSAs per each link 28 interconnecting tail node 34 to host node 24 . If tail nodes 34 are interconnected to host nodes 24 via many links 28 then 2 Link LSAs are advertised per each link 28 .
By contrast, in the present technique, these three (or more) LSAs are replaced by a single summary address 44 and a connectivity vector 46 . In practice, the summary address 44 advertised by the host node 24 is approximately equivalent in size to a single Nodal LSA, but a savings is obtained in that a single summary address 44 is advertised representing N tail nodes 34 . Further (and significant) savings are obtained by replacing the two (or more) link LSAs with a connectivity vector 46 comprising a single bit (or a set of two or more bits for more granular information) for each tail node 34 .
Information in conventional Link LSAs includes bandwidth availability on the link, link's attributes such as admin weight or cost, its color or resource class, and many other attributes typically used in the route computation to enable appropriate steering/discrimination of routes. For example, a link's admin weight or cost is conventionally used to calculate the most optimal (cheapest) end-to-end route of a connection. However, the present Applicants have recognized that links 28 inter-connecting tail nodes 34 and host nodes 24 must always be used by the tail node 34 to gain access to the core network 32 and thus cannot be avoided/discriminated. For example, if the cost of using a given tail-to-host link 28 is X dollars then the cost of an end-to-end route to the tail node 34 attached to that link must be at least X dollars, independently of the route taken through the core network 32 . Therefore, link attributes such as cost are of limited value for links 28 between tail 34 and host 24 nodes, as such links 28 are not used to tandem traffic/connections not destined for the particular inter-connected tail node 34 , and must always be used to gain access to the core network 32 .
FIG. 5 depicts an exemplary embodiment of the disclosure. As shown in FIG. 5 , a core network 532 may be connected to a plurality of metro networks 536 . The core network may include a plurality of core nodes 524 that route subscriber traffic between two neighbor core nodes 524 within the core network 532 . Each metro network 536 may include a plurality of metro nodes 534 . The metro networks 536 communicate with core network 532 to pass traffic between the metro domains and the core similar to tail nodes and core nodes noted above.
As may be appreciated, the distinction between metro nodes and core nodes is based on the role that each node plays in the network, rather than its physical construction or location. Thus it is possible for a metro node and a core node to be physically identical, if desired, in which case the difference between the two types of nodes would lie in their respective control software. Similarly, there is no requirement for core nodes and metro nodes to be installed at geographically dispersed locations, although it is contemplated that this will normally be the case.
The Applicants have discovered that the core control plane 6 can be extended to provide control plane functionality to metro nodes, by implementing conventional OCC functionality in each metro node, and suitably controlling the size and propagation of LSAs through the host nodes.
FIG. 6 depicts an exemplary embodiment. For example, the metro reachability is shown in FIG. 6 . The metro network 636 is preferably referenced using a unique metro network identifier, which may be defined in any suitable manner. For example, a unique Prefix.Suffix address may be assigned to each Metro Node, e.g.: 1.1 or 5.3, such that all nodes in the same metro have the same Prefix. The suffixes may be sequential. All nodes 634 in a metro can be summarized by a Metro Reachability Summary Address of Prefix.x, e.g.: 1.x, 5.x, etc. Each Core Node 624 connecting to a metro 636 is that metro's Home Node 624 H.
Home Nodes 624 H may flood Metro Reachability Summary Addresses and optionally a Metro Reachability Bit Vector to indicate reachability to a particular Metro Node 634 .
One bit may indicate Reachable versus Non-Reachable nodes. More bits may be defined to represent the cost of reachability and for which payload sizes, etc. If a Metro Reachability Bit Vector is not flooded or contains insufficient detail/granularity then a PCE like mechanism may be used for path computations, otherwise each Metro Node 634 can calculate its own routes. Home Nodes 624 H do not flood metro's 136 topology (nodes+links) into Core 632 , while Core nodes 624 do flood their topology into metros 636 .
Routing Scalability—each Core Node 624 may know only the detailed topology of the Core 632 and Metro Reachability Summary Addresses for all Metros 636 and optionally may also know the Metro Reachability Bit Vectors. Each Home Node 624 H may know the detailed topology of the Core 632 and its Metro 636 , and Metro Reachability Summary Addresses of all other Metros 636 and optionally may also know the Metro Reachability Bit Vectors. Thus, Routing Topology Databases associated with the networks contains no more than few hundred nodes instead of thousands of nodes if the entire network was treated flat as a single area/domain.
FIG. 7 depicts an exemplary embodiment. For example, the visibility of a node is shown in FIG. 7 . By way of illustration, an example of SNC from 1.4 to 50.2 will now be described. This example assumes the most simple of implementations where a Metro Reachability Bit Vector is advertized/flooded with a single bit representing reachability/non-reachability to a Metro Node 734 . Steps:
User issues ENT-SNC against source Metro Node 734 (1.4)
ENT-SNC::SNC-1-1:C:::RMTNODE=“50.2”, . . . ;
Optical Signaling and Routing Protocol (OSRP) calculates a route to destination node 50.2
On source Metro Node 1.4 OSRP determines that nodes E, F, G can reach 50.2 so it calculates routes to each and chooses the “best” one. Assume the route is via node E: DTL={<1.4,link>, <1.8,link>, <C,link>, <D,link>, <E,0>} Note that route through E may not be the best end-to-end route but with Metro Reachability Bit Vector with only a single bit, this may be the consequence. More bits may be used to indicate some level of cost, e.g.: high, medium, low.
OSRP signals SNC with the computed DTL and destination of 50.2 SNC SETUP arrives at node E (final hop in the DTL) where OSPR determines E is not the final destination so it calculates a route from E to destination 50.2 and extends the DTL. Assume the extended DTL is:
DTL={<1.4,link>, <1.8,link>, <C,link>, <D,link>, <E, link>, <50.1,link>, <50.2,0>}
SNC SETUP is allowed to continue along the DTL and arrives at destination Metro Node 50.2 and CONNECT is launched back to source Metro Node 1.4 SNC setup completes once the CONNECT is received by source Metro Node 1.4
Another example will now be described wherein a metro reachability bit vector is not advertized/flooded. If a Metro Reachability Bit Vector is not advertized/flooded then a PCE type of mechanism may be utilized to perform path computations. The following are the steps for SNC setup from Metro Node 1.4 to 50.2 using a Backward Recursive PCE (BR-PCE):
User issues ENT-SNC against source Metro Node 1.4
ENT-SNC::SNC-1-1:C:::RMTNODE=“50.2”, . . . ;
OSRP uses BR-PCE to calculate a route to destination node 50.2 as follows:
On source Metro Node 1.4 OSRP determines that nodes E,F,G can reach 50.2 so it sends a BR-PCE request to either E,F,G to calculate a “best” route from E,F,G to 50.2. Assume 1.4 chooses E and sends the BR-PCE request to it On Home Node E OSRP calculates “best” routes from each of E,F,G to 50.2. Assume the “best” routes are as follows:
DTL E->50.2 ={<E,link>,<50.1,link>,<50.2,0>} at cost of 30 DTL E->50.2 ={<F,link>,<50.4,link>,<50.7,link>,<50.2,0>} at cost of 50 DTL G->50.2 ={<G,link>,<50.3,link>,<50.1,link>,<50.2,0>} at cost of 60 Home Node E returns the routes DTL E->50.2 , DTL F->50.2 , DTL G->50.2 back to source Metro Node 1.4 as part of BR-PCE reply
On source Metro Node 1.4 OSRP calculates best routes to each of E, F, G. Assume the best routes are as follows:
DTL 1.4->E ={<1.4,link>,<1.8,link>,<C,link>,<D,link>,<E,0>} at cost of 100 DTL 1.4->F =<1.4,link>,<1.8,link>,<C,link>,<H,link>,<E,link>, <F,0>} at cost of 130 DTL 1.4->G ={<1.4,link>,<1.8,link>,<C,link>,<H,link>,<G,0>} at cost of 80 Metro Node 1.4 now combines the best routes DTL 1.4->E , DTL 1.4->F , DTL 1.4->G with corresponding best routes DTL E->50.2 , DTL F->50.2 , DTL G->50.2 to obtain the end-to-end best route from 1.4 to 50.2; DTL 1.4->50.2 =DTL 1.4->E and DTL E->50.2 ={<1.4,link>,<1.8,link>,<C,link>,<D,link>,<E,link>,<50.1,link>, <50.2,0>} at a cost of 100+30=130
OSRP signals SNC with the computed DTL 1.4->50.2
Note that the described PCE mechanism may be in-skin and its topology database may be OSRP's routing database, i.e. PCE is a component riding on top of OSRP routing and PCE communication (request+reply) may be done OOB or IB.
FIGS. 8A and B depict an exemplary embodiment. For example, a hierarchical metro architecture is shown in FIGS. 8A and B. There may be a desire to deploy metros in a hierarchical way when not all metros are connected to a core, i.e. when more than one metro may need to be traversed to get to another metro via a core. For example, core 832 may be connected to a plurality of metro networks 836 as shown in FIG. 8A . Such configurations can be generically thought of as a hierarchy where the core is the root as shown in FIG. 8B .
FIG. 9 depicts an exemplary embodiment. For example, a two level hierarchical architecture with core and metro networks is shown in FIG. 9 . FIG. 10 depicts an exemplary embodiment. For example, a two level Hierarchical Metro Reachability architecture is shown in FIG. 10 . FIG. 11 depicts an exemplary embodiment. For example, two level Hierarchical Visibility architecture is shown in FIG. 11 .
With reference to FIG. 11 , by way of illustration, an example of SNC from 2.M.x to 1.1.3 will now be described.
User issues ENT-SNC against source Metro Node 2.M.x
ENT-SNC::SNC-1-1:C:::RMTNODE=“1.1.3”, . . . ;
OSRP uses PCE to calculate a route to destination node 1.1.3 as follows:
On source Metro Node 2.M.x OSRP determines that nodes A, B, C can reach 1.1.3 so it sends a BR-PCE request to either A,B,C to calculate a route from A,B,C to 1.1.3. Assume 2.M.x chooses A and sends the BR-PCE request to it On Home Node A OSRP determines that nodes 1.1,1.2,1.3 can reach 1.1.3 so it sends a BR-PCE request to either 1.1,1.2,1.3 to calculate a route from 1.1,1.2,1.3 to 1.1.3. Assume A chooses 1.1 and sends the BR-PCE request to it On Home Node 1.1 OSRP calculates “best” routes from each of 1.1,1.2,1.3 to 1.1.3. Assume the “best” routes are as follows: DTL 1.1 → 1.1.3 ={<1.1,link>,<1.1.4,link>,<1.1.3,0>} at cost of 30 DTL 1.2 → 1.1.3 ={<1.2,link>,<1.1.4,link>,<1.1.3,0>} at cost of 20 DTL 1.3 → 1.1.3 ={<1.3,link>,<1.1.2,link>,<1.1.1,link>,<1.1.3,0>} at cost of 60 Home Node E returns the routes DTL 1.1 → 1.1.3 , DTL 1.2 → 1.1.3 , DTL 1.3 → 1.1.3 back to Home Node A as part of BR-PCE reply On Home Node A OSRP calculates “best” routes from each of A,B,C through 1.1,1.2,1.3 to 1.1.3 considering the routes DTL 1.1 → 1.1.3 , DTL 1.3 → 1.1.3 received in BR-PCE reply. Assume the “best” routes are as follows: DTL A → 1.1.3 ={<A,link>,<1.3,link>,<1.1.link>,<1.1.4,link>,<1.1.3,0>} at cost of 70 DTL B → 1.1.3 ={<B,link>,<1.7,link>,<1.3,link>,<1.1,link>,<1.1.4,link>,<1.1.3,0>} at cost of 90 DTL C → 1.1.3 ={<C,link>,<1.8,link>,<1.6,link>,<1.5,link>,<1.2,link>,<1.1.4,link>, <1.1.3,0>} at cost of 100 Home Node A returns the routes DTL A → 1.1.3 , DTL C → 1.1.3 back to source Metro Node 2.M.x as part of BR-PCE reply On source Metro Node 2.M.x OSRP calculates “best” routes to 1.1.3 through A,B,C considering the routes DTL A → 1.1.3 , DTL B → 1.1.3 , DTL C → 1.1.3 received in BR-PCE reply. Assume the “best” routes are as follows: DTL 2.Mx → A → 1.1.3 ={<2.M.x,link>,<2.6,link>,<2.5,link>,<2.4,link>,<D,link>,<A,link>, <1.3,link>,<1.1.link>, <1.1.4,link>, <1.1.3,0>} at cost of 170 DTL 2.M.x → B → 1.1.3 ={<2.M.x,link>,<2.6,link>,<2.5,link>,<2.4,link>,<D,link>,<A,link>, <B,link>,<1.7,link>,<1.3,link>,<1.1,link>,<1.1.4,link>,< 1 . 1 . 3 , 0 >} at cost of 200 DTL 2.Mx → C → 1.1.3 ={<2.M.x,link>,<2.6,link>,<2.2,link>,<2.1,link>,<C,link>,<1.8,link>, <1.6,link>,<1.5,link>,<1.2,link>,<1.1.4,link>,<1.1.3,0>} at cost of 150 Metro Node 2.M.x chooses the “best” route from 2.M.x to 1.1.3 via C, i.e. DTL 2.M.x → C → 1.1.3 : DTL 2.M.x → 1.1.3 ={<2.M.x,link>,<2.6,link>,<2.2,link>,<2.1,link>,<C,link>,<1.8,link>, <1.6,link>,<1.5,link>,<1.2,link>,<1.1.4,link>,<1.1.3,0>} at cost of 150
OSRP signals SNC with the computed DTL 2.M.x → 1.1.3
A number of options may be available for hierarchical network structures. For example, BR-PCE may be used to calculate the end-to-end route if the destination node is not in the source node's topology database. Also, the number of recursions may depend on the hierarchical level of metros, i.e. N-level hierarchy->(N−1) recursions. Also, Metro reachability information (Metro Reachability Summary Address) may be explicitly provisioned on Home Nodes leading to a metro or dynamically discovered via OSRP routing. Also, the outermost metro (from perspective of the core) may always have the largest view in terms of the network topology. The Core may have the smallest view and may only know which Home Nodes can reach which metros. This may be beneficial as the core may be busy processing all control plane signaling messages resulting from mesh restorations, etc. This processing may require a processor and thus not over-burdening the core with routing details may be beneficial. The further away from a core, i.e. metros, the less processor time may be required for control plane signaling (less connections) and thus more processor time may be afforded to handling routing details/updates. In addition, metro-to-metro shortcuts may be used. In addition, multiple levels of “tails” and metros may be used.
Those of skill in the art will appreciate that information and signals may be represented using any of a variety of different technologies and techniques. For example, data, instructions, commands, information, signals, bits, symbols, and chips that may be referenced throughout the above description may be represented by voltages, currents, electromagnetic waves, magnetic fields or particles, optical fields or particles, or any combination thereof.
Further, those of skill in the art will appreciate that the various illustrative logical blocks, modules, circuits, and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both. To clearly illustrate this interchangeability of hardware and software, various illustrative components, blocks, modules, circuits, and steps have been described above generally in terms of their functionality. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the overall system. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The methods, sequences and/or algorithms described in connection with the embodiments disclosed herein may be embodied directly in hardware, in a software module executed by a processor, or in a combination of the two. A software module may reside in RAM memory, flash memory, ROM memory, EPROM memory, EEPROM memory, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art. An exemplary storage medium is coupled to the processor such that the processor can read information from, and write information to, the storage medium. In the alternative, the storage medium may be integral to the processor.
Accordingly, an embodiment of the invention can include a computer readable media embodying a method for management of communications networks. Accordingly, the invention is not limited to illustrated examples and any means for performing the functionality described herein are included in embodiments of the invention.
While the foregoing disclosure shows illustrative embodiments of the invention, it should be noted that various changes and modifications could be made herein without departing from the scope of the invention as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the embodiments of the invention described herein need not be performed in any particular order. Furthermore, although elements of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
|
A method of extending the control plane to a metro sub-domain for a network having a transport plane for carrying subscriber traffic within end-to-end connections, and a control plane for managing at least a portion of resources of the transport plane allocated to the connections. A first set of control-plane enabled nodes of the network is designated as core nodes, each core node being operable to route subscriber traffic between a pair of neighbor core nodes in the network. A second set of control-plane enabled nodes of the network is designated as metro nodes, each metro node being connected to a core node and operating as a sub-domain of the network. Each core node that is connected to at least one metro node is designated as a host node. The host node is controlled to advertise summary information of its connected metro nodes to other core and metro nodes in the network, thus making it possible to extend control plane function to the metro nodes that can calculate connection routes, set-up/tear-down connections and perform connection failure recovery functions.
| 7
|
TECHNICAL FIELD
[0001] The present disclosure relates generally to seats and shelves used in showers, baths and the like, and more particularly, relating to a preformed structural support for use in the construction of seats for new and existing ceramic tile surfaces where the preformed structural support is site customizable to conform to the irregularities of the shower or bath wall structure.
BACKGROUND
[0002] Seats and shelves are desired fixtures in showers, baths and the like for providing architectural decoration, a place for sitting, a foot rest or a horizontal surface to store bathing related articles. In constructing such fixtures, it is important to preserve the waterproofing of the bath or shower, provide an appealing finished product, and also ensure the fixture can support loading, such as, for example, when a person sits or uses the fixture as a foot rest.
[0003] One usual method of constructing these fixtures includes a site-built wood frame structure that is attached to the rough frame of a shower or tub wall and/or floor. The wood frame structure is then waterproofed with one of several methods and then reinforced with expanded metal, wire mesh or other means. A sub-base or mortar is applied to all of the exposed surface areas, and then tile is placed over the mortar by means of a suitable bonding agent, such as thinset. Although this provides an appealing finished look it is problematic and has many draw backs. First, the construction method is very labor intensive, time consuming and requires a degree of skill that most general construction labors do not have. Further, if the waterproofing is not done correctly or is compromised the construction is prone to failure due to water penetration. Water damage in this area can lead to extensive repair costs. Further yet, the wood frame is likely to shrink and the wood frame members are likely to shift overtime resulting in cracking of the tile and grout finish and damaging the waterproofing.
[0004] A second usual method of constructing these fixtures includes building a support structure of concrete blocks during either the rough-in of the bath or shower or after waterproofing the bath or shower construction. The concrete blocks are individually arranged to form a perimeter wall that is then filled with concrete or a mortar mix to form a top horizontal surface. The surface of the concrete blocks and top horizontal surface are prepared for the application of tile using the typical various methods. Although this method attempt to eliminate the shrinking and shifting of the wood members experienced by the first method, this method also has many drawbacks. In this regard, it is more labor intensive, results in a heavier construction, and requires additional skills even over the first method.
[0005] One attempt to provide a better construction method and device for constructing such fixtures in showers and baths is disclosed in U.S. Pat. No. 5,542,218 (“the '218 patent”), issued to Rompel on Aug. 6, 1996. The '218 patent describes a corrosion-resistant self-supported frame of a pre-form shape, to which a mortar substrate and ceramic tile is applied, in order to produce corner seats and trays.
[0006] While the pre-form of the '218 patent provides a ready made support structure for use in constructing corner seats and trays in showers or baths it requires the use of penetrating fasteners, such as, a threaded fastener to attach the pre-form to the shower or bath wall framing members, which requires penetrating the waterproofing of the shower or bath. Any penetration of the waterproofing can lead to water damage resulting in costly repairs. Additionally, the pre-form may not be capable of conforming to irregularities of the shower or bath walls. It is very common for abutting vertical walls in a building structure, such as, a bath or shower to not be perfectly square or plumb. The addition of surface tile can further add or exaggerate the wall irregularities. The pre-form of the '218 patent is constructed with the expectation of the walls being square and plumb. However, if this is not the case during installation, gaps can result between the pre-form and the walls or the pre-form can be damaged by over tightening of the penetrating fasteners in attempt to close the gaps, either of which is likely to result in failure. An additional possible drawback of the pre-form of the '218 patent, is the pre-form is designed to be elevated above the floor of the bath or shower and installed in a cantilever fashion. In some installations, it is desirable to have the seat extend down to the floor of the bath or shower, and the pre-form of the '218 is not capable of providing this.
[0007] An additional attempt to provide a better construction method and device for constructing such fixtures in showers and baths is provided by T. Clear Corp. in their PreFormed™ tile ready shower seat which is lightweight, does not require wood framing and its installation does not compromise the waterproofing of the shower or bath. However, T. Clear Corp. instructs the walls to which the seat is to be installed against must be square and plumb and you must not cut the seat or otherwise damage the exterior coating of the seat. These requirements makes utilization of the seat less practical as most walls are not square or plumb and the seat can not be cut to conform to the irregularities of the walls. Further, it is likely during the tiling process tools or tiles will be dropped, and in this event, if the tools or tile impact the seat this may damage the exterior coating requiring costly replacement of the seat.
[0008] The disclosed preformed structural support for use in the construction of seats for new and existing ceramic tile surfaces is directed to overcoming one or more of the problems set forth above and other problems present in the art.
SUMMARY OF THE INVENTION
[0009] In general, in one aspect, a preformed structural support for ceramic tile for use in constructing a horizontal support surface, such as a seat or a foot rest in a shower or the like installation environment having structural surfaces for attachment of the preformed structural support thereto is provided. The preformed structural support includes a base unit having a plurality of inward facing sides, and plurality of outward facing sides, wherein at least one of the plurality of inward facing sides includes a lip at least partially around and projecting from the periphery thereof. Each lip having an interface surface for abutment with at least one structural surface, and wherein each of the plurality of outward facing sides is adapted for the application of tile thereon.
[0010] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood and in order that the present contribution to the art may be better appreciated.
[0011] Numerous objects, features and advantages of the present invention will be readily apparent to those of ordinary skill in the art upon a reading of the following detailed description of presently preferred, but nonetheless illustrative, embodiments of the present invention when taken in conjunction with the accompanying drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of descriptions and should not be regarded as limiting.
[0012] As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
[0013] For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there is illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The invention will be better understood and objects other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
[0015] FIG. 1 is a front perspective view of the preformed structural support shown installed in a typical installation environment, such as a shower;
[0016] FIG. 2 is a rear perspective view of the preformed structural support constructed under the principals of the present invention;
[0017] FIG. 3 is a front perspective view of the preformed structural support constructed under the principals of the present invention;
[0018] FIG. 4 a is a partial cross-sectional view taken along line 4 a - 4 a in FIG. 3 showing the preformed structure support is shown installed as “new construction”;
[0019] FIG. 4 b is a variation of FIG. 4 b , where the preformed structural support is shown installed as “old construction”;
[0020] FIG. 5 is a partial cross-sectional view of two outward facing sides with tile applied to the sides;
[0021] FIG. 6 is a cross-sectional view taken along line 6 - 6 in FIG. 2 showing a hollow interior configuration of the preformed structural support with internal reinforcement;
[0022] FIG. 7 a is a top plan view of the preformed structural support with an alternate configuration;
[0023] FIG. 7 b is a top plan view of the preformed structural support with an alternate configuration; and
[0024] FIG. 7 c is a top plan view of the preformed structural support with an alternate configuration.
[0025] Similar reference characters denote corresponding features consistently throughout the attached drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0026] With reference to FIG. 1 of the drawings, there is shown a perspective view of a preformed structural support 10 for use in the construction of seats for new and existing ceramic tile surfaces constructed in accordance with the principals of the present invention installed in a typical installation environment 100 such as a shower or bath. The preformed structural support 10 is positioned in a corner formed by two vertical walls 12 and 14 and a horizontal floor surface 16 , herein referred to as structural surfaces.
[0027] With reference now to FIGS. 1-3 , the preformed structural support 10 includes a base unit 18 of a desired size and shape constructed of a non-corrosive, rigid material. It is contemplated the base unit 18 being constructed of a plastic through injection molding or otherwise. It is further contemplated, the base unit 18 being constructed of a high-density plastic. A suitable high-density plastic may be ABS. The plastic material also may include a reinforcement material. A suitable reinforcement material may be a fibrous material, such as, for example, glass or carbon fibers.
[0028] The base unit 18 , with reference to the installation positioning, includes a plurality of inward facing sides 20 - 24 and a plurality of outward facing sides 26 and 28 . The base unit 18 is generally constructed to have a polygonal horizontal cross-sectional shape with two opposed and attitudinally spaced horizontal surfaces and a number of vertical surfaces equal to the number of sides of the polygon extending between the two horizontal surfaces. The desired installation position of the base unit 18 with respect to the installation environment's structural surfaces determines the number of inward facing sides and the number of outward facing sides. In one aspect, the base unit 18 includes at least one inward facing side and at least one outward facing side. In another aspect, the base unit 18 includes at least two inward facing sides and at least two outward facing sides. As illustrated, the base unit 18 includes two vertical inward facing sides 20 , 22 and a horizontal side inward facing side 24 , and a vertical outward facing side 26 and a horizontal outward facing side 28 . The inward facing sides 20 - 24 may be continuous surfaces. The outward facing sides 26 , 28 may be continuous surfaces.
[0029] A lip 30 extends at least partially around the periphery 32 of each inward facing side 20 - 24 . The lip 30 may extend from at least two peripheral edges of each inward facing side 20 - 24 . The lip 30 may extend from at least three contiguous peripheral edges of each inward facing side 20 - 24 . Each lip 30 includes an interface surface 34 for abutting with a structural surface of the installation environment 100 , which will be further explain in more detail below. The lip 30 may extend from the periphery 32 of its respective inward facing side 20 - 24 such that the interface surface 34 is at a spaced distance from the inward facing side. The 30 may extending from the periphery 32 of its respective inward facing side 20 - 24 such that the interface surface 34 is at a spaced distance from and generally parallel to the inward facing side. In one aspect, the lip 30 extends about 0.5 inches from the periphery 30 of its respective inward facing side 20 - 24 . In another aspect, the lip 30 extends less than about 0.5 inches from the periphery 30 of its respective inward facing side 20 - 24 . In another aspect, the lip 30 extends about 0.5 inches from the periphery 30 of its respective inward facing side 20 - 24 and if of a thickness of about 0.5 inches. In another aspect, the lip 30 extends less than about 0.5 inches from the periphery 30 of its respective inward facing side 20 - 24 and is of a thickness of about or less than 0.5 inches.
[0030] The lips 30 can be trimmed to conform to the irregularities and/or angles of the structural surfaces in relation to the adjacent structural surfaces to which the base unit 18 is to be installed against. For example, very often, the corner formed by two vertical walls abutting one another is rarely perfectly square forming, thus forming a ninety degree angle. Additionally, the floor surface of the installation environment is typically formed to have a slight slant towards a drain formed through the floor. In either of these events, it is impractical to first measure these angles and then request a manufacture to construct and ship a pre-formed seat structure having interface surfaces formed to match the measured angles. As such, being able to trim the lips 30 permits on-site customization of the base unit 18 to fit the intersections of the abutting structural surfaces, the irregularities of the structural surfaces and the angles of the structural surfaces.
[0031] The preformed structural support 10 can be installed as “new construction” meaning before the application of tile to the structural surfaces to which the base 18 is to be installed, as shown in FIG. 4 a , or “old construction” meaning after application of tile to the structural surfaces as shown in FIG. 4 b.
[0032] With particular reference to FIG. 4 a , there is shown a partial, elevation sectional view of the preformed structural support 10 as shown in FIG. 1 . While the below discussion is made in reference to only one vertical inward facing side, the same applies to the remaining vertical inward facing sides. The base 18 is installed with the vertical inward facing side 22 against a structural vertical wall or structural surface 12 and the horizontal inward facing surface 24 against the floor or structural surface 16 of the installation environment 100 . The base 18 is showing being installed as “new” construction meaning before the application of tiles to the structural surfaces. The vertical wall 12 includes a waterproofed outer surface 102 supported by wall framing 104 . The floor 16 is waterproofed and is a sub-base of the shower or bath. The interface surfaces 34 of the lips 30 of the inward facing sides 22 and 24 are shown trimmed and in contact with the surface 102 and floor 16 respectively. Note, the lip 30 of the inward facing side 24 has been trimmed to conform to the slight slope of the floor 16 ensuring a continuous contact between the interface surface 34 and the floor. A suitable adhesive 36 (partially cutaway to illustrate lips) is applied between the structural surfaces 102 and 16 , the inward facing sides 22 and 24 , and the interface surfaces 34 to secure the base 18 to the structural surfaces. A suitable adhesive may be a mortar mix or the like. Another suitable adhesive may be a single or multipart epoxy compound. The use of an adhesive as opposed to mechanical fasteners insures the integrity of the waterproofing of the structural surfaces.
[0033] With reference to FIG. 4 b , the base 18 is showing being installed as “old” construction meaning after the application of tiles to the structural surfaces. Like above, vertical wall 12 includes a waterproofed outer surface 102 supported by wall framing 104 and additionally includes a layer of tiles 104 . The floor 16 is waterproofed and is a sub-base of the shower or bath. While not shown, the floor 16 could also have a layer of tiles. The interface surfaces 34 of the lips 30 of the inward facing sides 22 and 24 are shown trimmed and in contact with the layer of tiles 104 and floor 16 respectively. Note, the lip 30 of the inward facing side 24 has been trimmed to conform to the slight slope of the floor 16 ensuring a continuous contact between the interface surface 34 and the floor. A suitable adhesive 36 (partially cutaway to illustrate lips) is applied between the structural tile layer 104 and 16 , the inward facing sides 22 and 24 , and the interface surfaces 34 to secure the base 18 to the structural surfaces. A suitable adhesive may be a mortar mix or the like. Another suitable adhesive may be a single or multipart epoxy compound. The use of an adhesive as opposed to mechanical fasteners eliminates the need to penetrate the structural surfaces and insures the integrity of the waterproofing of the structural surfaces and prevents the requirement of drilling through the tile layer 104 .
[0034] With reference to FIG. 5 , there is shown a partial cross-sectional view of base unit 18 with a plurality of tiles 38 applied to the outward facing surface 26 , 28 . The outward facing sides 26 , 28 may be textured or otherwise treated to permit the direct application of tile 38 with a suitable adhesive 40 to the outward facing sides. A suitable adhesive 40 for attaching tile 38 to the outward facing sides 26 , 28 may be a thinset compound. In one aspect, the outward facing sides 26 , 28 may have a plurality of recessed pockets 42 . The pockets 42 capture and retain the adhesive 40 for application of the tile 38 . The pockets 42 can be arranged in desired patterns on the outward facing sides 26 , 28 .
[0035] Turning now FIG. 6 , which is a horizontal cross sectional view of the base unit 18 , to reduce weight and manufacturing costs, the base unit may be constructed to have a hollow interior 44 that is defined by the sides 20 - 28 . An internal reinforcement 46 may be provided to support the sides of the base. In one aspect, the internal reinforcement 46 is provided in the form webbing that extends across the vertical sides 20 , 22 , 26 between the horizontal sides 24 , 28 . The webbing 46 may be formed into any desired pattern that affords the most structural support while reducing weight and manufacture costs. In one aspect, as shown, the webbing 46 is generally rectangular. In another aspect, the webbing 46 may be honeycomb shaped.
[0036] While the above description of the preformed structural support 10 was made in reference to a base unit 18 having a triangular horizontal cross-sectional shape, the base unit 18 is generally constructed to have a polygonal horizontal cross-sectional shape with two opposed and attitudinally spaced horizontal surfaces and a number of vertical surfaces equal to the number of sides of the polygon extending between the two horizontal surfaces. For example, with reference to FIGS. 7 a , 7 b and 7 c , the base unit 18 is shown of various different shapes. In FIG. 7 a , the base unit 18 has a polygonal shape generally of a quarter circle and includes two horizontal sides (one not shown) and three vertical sides. In FIG. 7 b , the base unit 18 has a polygonal shape generally of a truncated square, and includes two horizontal sides and five vertical sides. Likewise, in FIG. 7 c , the base unit 18 has a polygonal shape generally of a square, and includes two horizontal sides and four vertical sides. The shape of the base unit 18 of the preformed structural support 10 should not be limited to the examples discussed herein, as the base unit may be constructed to have numerous shapes.
[0037] In use, the preformed structural support 10 is first dry fit to the structural walls to which it is to be attached, including any vertical walls and floor. The lip 30 of each inward facing side is trimmed by a plane, saw, knife or otherwise so as to shape the interface surface 34 thereof to conform to the irregularities and angles of the respective wall/floor. The lips 30 are trimmed also to ensure each interface surface 34 makes even contact with the surrounds walls/floor so the base unit 18 does not rock. Once the preformed structural support 10 is dry fit, a suitable adhesive is applied to the inward facing sides and interface surfaces and the base unit 18 is set into place. Once the adhesive is cured, tile is applied to the outward facing surfaces using known methods.
[0038] A number of embodiments of the present invention have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the invention. Accordingly, other embodiments are within the scope of the following claims.
|
A preformed structural support for ceramic tile for use in constructing a horizontal support surface, such as a seat or a foot rest in a shower or the like installation environment is provided. The preformed structural support includes a base of a corrosion-resistant material that can be trimmed to conform to the irregularities of the structural walls to which it is to be installed against. The base includes tile receiving sides that are textured and are ready for the application of tile using a suitable adhesive, such as a thinset compound. The preformed structural support is installed without the use of penetrating fasteners, thereby preserving the integrity of the waterproofing of the shower.
| 4
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to emission control of internal combustion engines. In particular, the invention relates to on-board monitoring of an efficiency of a Three Way Catalytic converter (TWC) installed on a vehicle to minimize emission from an engine.
2. Prior Art
It is known in the field that catalytic conversion relates to a catalytic oxygen storage capability. A properly operating TWC converter dampens exhaust gas component fluctuations in the exhaust stream. One proposed system (see SAE paper 900062, Detection of catalytic efficiency loss using on-board diagnostic) employs two exhaust gas oxygen (EGO) sensors, one upstream and one downstream of the converter, to detect those changes in oxygen content before and after the converter. The system further employs test signals in a form of an air-fuel ratio swing on both sides of stoichiometry at predetermined rates or frequencies caused by fuel control system perturbations. By comparing the change in response patterns between pre- and post-converter EGO sensors, a determination can be made about catalytic efficiency. A deficiency of that method is that during the test the fuel control system operates in an open loop control mode, and air-fuel ratio tends to shift from stoichiometry. Test results also depend on two EGO sensors with different characteristics due to manufacturing tolerances or aging which may lead to additional errors. Further, the particular selected air-fuel ratio swing and frequency greatly influence results of the test. The problem and disadvantages discussed above are overcome by this invention.
SUMMARY OF THE INVENTION
This invention provides a system for on-board catalytic converter efficiency monitoring by measuring parameters of a converter.
A method and apparatus for converter monitoring employs an air-fuel ratio closed loop control system. This control system uses, as a main control input, one EGO sensor located downstream of the converter. The control system operates in a limit cycle mode, and frequencies of the limit cycles are changed by changing parameters of a system controller. A limit cycle is defined as the cycle of variation in air fuel ratio control signal from a rich limit to a lean limit and back to the rich limit again. Parameters of the converter are defined based on such limit cycle frequencies. These parameters are matched with experimentally developed functions to estimate catalytic converter efficiency.
In one particular aspect of the invention, the method includes the steps of: initiation of a closed loop air-fuel ratio control system using an EGO sensor located downstream of the catalytic converter; measuring the frequency of the limit cycle; changing, one or more times, operating or structural parameters of a system controller to generate different limit cycle frequencies; measuring the frequency of each limit cycle; solving a system of equations which relate the limit cycle frequencies to the catalytic converter parameters; and estimating the catalytic converter efficiency using stored experimental data.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects and advantages described herein will be more fully understood by reading the description of the preferred embodiment with references to the drawings wherein:
FIG. 1 is a schematic diagram of an internal combustion engine with converter and control system in accordance with an embodiment of this invention;
FIG. 2 is a block diagram of the control system which is used for catalytic converter efficiency monitoring in accordance with an embodiment of this invention;
FIG. 3 is a block diagram of the control system as described in the invention;
FIGS. 4 and 4A is a flowchart illustrating various process steps performed by a portion of the embodiment shown in FIG. 2;
FIG. 5 is a graphical representation of a catalyst efficiency as a function of TWC converter parameters T d (transport time delay) and T c (time constant);
FIG. 6 is a flowchart illustrating various process steps performed by a portion of the flowchart shown on FIG. 4 to calculate a limit cycle period in accordance with an embodiment of this invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
An example of the embodiment in which the invention claimed herein is used to advantage is now described with reference to attached figures.
First referring to FIG. 1, an internal combustion engine 1 produces exhaust gases which pass through an exhaust manifold and associated piping 2, to a TWC converter 3 and are discharged through exhaust piping 4. The efficiency of converter 3 is measured in accordance with this invention. Two EGO sensors 5 and 6 upstream and downstream, respectively, of the converter are connected to an engine control computer (ECC) 7. It should be noted that either a single upstream EGO sensor 5 control system or a dual EGO sensor control system using both EGO sensors 5 and 6 may be used in accordance with this invention. ECC 7 also receives various engine operating parameters which are advantageous for proper operation of the fuel control system. These parameters include, but are not limited to, engine speed, vehicle speed, air flow, crankshaft position, cooling water temperature and inlet air temperature. Based on a plurality of such engine operating parameters, ECC 7 calculates a fuel pulse width which is delivered to fuel injectors 8. The fuel pulse width is trimmed in accordance with inputs provided by EGO sensors so that limit cycle operation is initiated. This is operation wherein an indication of lean air fuel ratio by an EGO sensor causes the fuel control system to increase the richness of the air fuel ratio until there is an indication of rich air fuel ratio by the EGO sensor, where the fuel control system drives the air fuel ratio leaner. The proposed invention will work with either single or multiple fuel injectors, and only one injector is shown for clarity. Fuel is supplied to fuel injectors through a fuel line 9.
It is noted that many conventional engine components necessary for proper engine operation, such as an ignition system, are not shown. Those skilled in the art will also recognize that the invention may be used to advantage with engines having different number of cylinders or exhaust banks.
The following is a theoretical explanation of the proposed method.
A vehicle exhaust system, having fuel as an input and exhaust gas oxygen concentration as an output, includes engine cylinders, an exhaust mainfold, connecting piping, a TWC converter, and an EGO sensor after a converter. In terms of a control system, the vehicle exhaust system may be described as a transport time delay T d and a set of first order low pass filters connected in series. The physical nature of the transport time delay T d is due to an exhaust gas propagation time from a time of delivering fuel to an engine cylinder to a time exhaust gas reaches a EGO sensor. The physical nature of the first order low pass filter time constants T ci are due to a catalytic converter oxygen storage damping of exhaust gas fluctuations, response rate of EGO sensor, and to a minor extent due to physical mixing and chemical reactions in the exhaust manifold and associated piping 2. In a form of Laplace transform, the transfer function of the exhaust system is ##EQU1## where W sys (s) is a transfer function of the exhaust system; T d (transport time delay), and T ci (low pass filter time constant) are unknown parameters which are to be determined during a test.
Conventional fuel controller is a Proportional/Integral (PI) controller with calibratable gain H and integral G, commonly known as a jumpback and ramp. Its transfer function W cont (s) in a form of Laplace transform is
W.sub.cont (s)=H+G/s (Eqn 2)
It should be mentioned that any more sophisticated controller, for example, a controller with a differential term may be used with the proposed method.
The EGO sensor output is connected to a controller input through a comparator which has the output +1 or -1 depending on what side of stoichiometry the EGO sensor is sensing. A block diagram of the fuel control system is shown on FIG. 2, where numerical 21 refers to the exhaust system in accordance with Eqn 1, numerical 22 refers to a comparator, and numerical 23 refers to a controller described, for example, by Eqn 2.
Calculations of the limit cycle period T li of the control system is known from the art, and equal to ##EQU2## which has (n+1) unknown parameters T d , T ci , c 0 =G (controller ramp), and c i is a known function of a controller jumpback H and time constants T ci .
In order to solve Eqn 3 to find out all (n+1) unknown parameters, it is necessary to generate (n+1) equations similar to Eqn 3. To achieve this objective, the ramp G, jumpback H, or both of them simultaneously should be changed n times, and (n+1) limit cycles T li corresponding to each controller parameter setting should be measured. Then set of (n+1) algebraic equations may be solved using any known numerical method. Those skilled in the art may use known or develop new methods for solving a set of Eqn 3 which are the best fit for their computing environment.
The above theoretical explanation of the proposed method refers to a general description of the control system. In practice, filtering effects of the exhaust manifold and associated piping 2 may be neglected, and therefore, no time constants are assigned to them.
For simultantiously monitoring catalytic converter efficiency and downstream EGO sensor 6 monitoring, two time constants T c1 and T c2 characterizing EGO sensor response rate and converter oxygen storage damping are required. Fuel control is turned over to downstream EGO sensor in the case of a conventional fuel control arrangement with one upstream EGO sensor. A control signal from upstream EGO sensor is disabled in the case of a dual EGO fuel control system (see, for example, copending patent application number 07/724,394). Then three limit cycle frequencies are generated by changing, for example, jumpback H to achieve full or 100% jumpback, half or 50% jumpback, and 0% or no jumpback.
For monitoring only catalytic converter efficiency, the time constant of the downstream EGO sensor may be lumped together with a converter time constant, so only one time constant is be required. The above mentioned sequence using three settings of fuel the controller can be simplified to use only two settings. In some cases, transport time delay T d may be estimated or measured by other known means. In such a case, only one limit cycle frequency is needed to solve Eqn 3, thus providing further simplification in monitoring converter efficiency. For clarity of explanation without losing any generality, the proposed invention will be described below with a reference to a control system to monitor only catalytic converter efficiency. Hence only transport time delay T d and catalytic converter time constant T c will be determined.
A block diagram of the control system is shown in FIG. 3, where numeral 31 refers to the converter, numeral 33 refers to the controller, and numeral 32 refers to the comparator. Corresponding transfer functions are also shown on the FIG. 3.
The operation of ECC 7 in controlling air-fuel ratio in a manner to estimate the efficiency of a converter is now described with particular reference to the flowchart shown on FIGS. 4 and 4A and an associated experimentally developed TWC converter efficiency function shown in FIG. 5.
At the start of the process in step 4010, engine parameters are read. They include, but are not limited to, parameters which define test conditions and EGO switching. In this description, parameters are read using a constant sampling rate, for example 10 msec. However, in an interrupt driven computer system, different counters which will be described later, may be substituted by timers. This may also require additional steps in the flowchart. In step 4020, test conditions are verified. It may be desirable to initiate a catalytic converter efficiency test at a constant vehicle speed, for example between 20 and 50 MPH, moderate load, and after engine operations are stabilized. Only one converter efficiency test may be desired for a given driving cycle. If the test conditions are satisfied, the test may be started, otherwise at step 4030 the test subroutine is exited. It should be noted that step 4030 will also terminate and reset the test if entry conditions change during test. Step 4040 checks if a catalytic converter monitoring test has already been started. If this is the first entry into the test, step 4050 sets a test in progress flag. In step 4060, the control system is switched to a control signal supplied by downstream EGO sensor 6. Controller jumpback is set to a desired value, for example 100% full jumpback is a typical value. Step 4070 sets a flag indicating that the first limit cycle period is to be measured. Then the test subroutine exits the test at step 4080.
In the following sampling intervals, if test conditions in step 4020 continue to be satisfactory and the test in progress flag is set in step 4050, logic flow goes to step 4090 which checks if this is a measurement of the first limit cycle period. Steps 4100 and 4110 provide a certain time delay to settle possible transient conditions associated with the change of the controller input. Step 4110 represents a counter which is incremented each sampling interval to provide a constant sampling rate counter content proportional to elapsed time. Step 4100 verifies that this time has elapsed. After this entry delay is completed, step 4120 starts calculations, in the following sampling intervals, first limit cycle period T 11 . Complete operation of step 4120 will be explained later. Step 4120 sets flags for steps 4090 and 4130, indicating completion of measurements of the first limit cycle period, and a flag for step 4140, indicating completion of catalytic converter monitoring test. If conditions in steps 4130 or 4140 are not met, subroutine is exited through a return in step 4080. When both limit cycle periods T 11 and T 12 are measured as indicated by a flag in step 4140, step 4150 solves equations 3 to calculate transport time delay T d and converter time constant T c . Step 4160 generates a function f(T d ,T c ) which is an input to the experimental TWC converter efficiency function shown in FIG. 5. Step 4170 makes a determination if the converter has passed the efficiency test.
After the first limit cycle period is determined, the first cycle flag in step 4090 is reset and logic flow proceeds to step 4180. If a second cycle flag in step 4180 is not set and measurement of the second limit cycle period has not been started, new controller parameters are set in step 4190. For example, jumpback is set to 0%. This means that the original PI controller is changed in this example to an I controller, and another limit cycle, longer than a limit cycle with the PI controller, will be initiated. Step 4200 sets the second cycle flag to start second limit cycle period measurement. Steps 4210 and 4220 provide an entry time delay, similar to one described in steps 4100 and 4110, to settle possible transient conditions associated with the change in the controller parameters. After this entry time delay is completed, step 4210 directs the subroutine logic flow to step 4120 which will measure the second limit cycle period.
Referring to FIG. 6, step 4120 is common to all limit cycles. Step 5010 checks if this is the first entry for any limit cycle period measurement. If this is the first entry, logic flow goes to step 5020 to check for the first EGO sensor switch. If there is no EGO switch, logic flow goes to step 5050. After the first EGO sensor switch is detected, step 5030 sets a first entry flag for step 5010, and resets test and period counters. Test counter N t is incremented in step 5060 during each sampling interval after the first entry flag is set. If an EGO sensor switch is detected in step 5070, period counter N p is incremented for each EGO sensor switch. When a preselected number of limit cycle periods, as counted by period counter N p , is detected in step 5090, step 5100 calculates, an average period T li for a given limit cycle, and stores it in memory for future use. Step 5110 resets the first entry flag for use in step 5010, thus preparing step 4120 for measuring another limit cycle period. Next step 5120 resets the first cycle flag used in steps 4090 and 4130, thus allowing measurement of the second limit cycle period in step 4180. The second cycle flag which is set in step 4180 is checked in step 5130 after measurement of the second limit cycle is completed. Step 5140 sets a test complete flag which allows step 4140 to proceed to step 4150, as described above. If the third limit cycle is required as in the case of a downstream EGO sensor time constant calculations, one more branch should be added to the flowchart similar to steps 4180 through 4220. Controller jumpback will be set to a new value, for example, 50% jumpback.
Various modifications and variations will no doubt occur to those skilled in the art to which this invention pertains. For example, the particular feedback gain or operating parameters used to vary frequency may be varied from that disclosed herein. These and other variations which basically rely on the teachings through which this disclosure has advanced the art are properly considered within the scope of this invention.
This concludes the description of the preferred embodiment. It is intended that the scope of the invention be limited to only the following claims.
|
An on-board catalytic converter efficiency monitoring system uses an exhaust gas oxygen sensor downstream of a converter to enable closed loop air-fuel ratio control. The period of the air-fuel limit cycle is used to determine a time constant parameter of the feedback loop. A parameter in the fuel controller is changed to induce another air-fuel limit cycle frequency. The period of this new air-fuel limit cycle provides additional information with respect to the time constant of the feedback loop. Because it is possible to make other changes to the parameters of the fuel controller, different frequencies can be induced and additional parameters of the feedback loop time constant can be determined. With n different frequencies produced by n different fuel controller parameters it is possible to solve for n different time constants. The system can be used with either one or two EGO sensors depending upon the desired parameter to be solved. It is particularly advantageous to use one EGO sensor downstream of a converter to determine the catalytic efficiency.
| 5
|
BACKGROUND
[0001] This invention relates to a twin fabric hybrid forming section for use in a paper making machine. In a hybrid forming section the stock jet is ejected from a headbox slice onto a first forming fabric that is travelling in a horizontal plane in the machine direction over a series of dewatering boxes comprising a conventional open surface single fabric forming section. A second forming fabric is then brought into intimate contact with the exposed upper sheet surface at the beginning of the hybrid two fabric forming section. The partially formed sheet and the undrained stock is sandwiched between two forming fabrics; drainage then occurs through both forming fabrics. The second forming fabric is separated from the upper surface of the formed sheet at the end of the hybrid two fabric forming section and the sheet is conveyed to the press section on the first forming fabric. This invention is concerned with that portion of the hybrid two fabric forming section between the locus at which the first and second forming fabrics come together to sandwich the stock between them and the locus at which the first and second forming fabrics separate with the sheet continuing on the first forming fabric. Although the forming section described here includes a single second forming fabric section this invention is not so limited. It is common to have more than one hybrid two fabric forming section, and to have a second headbox delivering a second layer of stock onto the first forming fabric ahead of the second hybrid two fabric forming section.
[0002] In a hybrid type forming section the two forming fabrics do not follow a linear path. The fabrics together pass over a sequence of rolls and dewatering boxes which are located on alternate sides of the two fabrics and thus define the sinuous path of the two fabrics. Each dewatering box has a curved surface, which carries a group of fabric support elements, such as blades, which are in contact with the machine sides of the forming fabrics. Each dewatering box may also be connected to a source of controlled vacuum. These curved surfaces cause the moving forming fabrics to follow the desired sinuous path. The application of a controlled level of vacuum to the dewatering boxes has two effects: it promotes the removal of water from the stock between the two moving forming fabrics, and it deflects the path of the two moving forming fabrics into the gaps between the fabric support elements. This deflection of the two moving forming fabrics generates a positive pressure pulse within the stock layer sandwiched between them that creates fluid movement within the stock in the machine direction; this causes a shearing action within the stock which serves to break up fibre flocs.
[0003] The actual magnitude of each pressure pulse generated by the deflection angle of the moving forming fabrics at the edges of each fabric support element has a significant impact on the quality of the final sheet produced. The strength of the pressure pulse generated by each fabric support element should be chosen to match the stock conditions and properties at that fabric support element. Hence, there exists a need to be able to modify the strength and/or magnitude of the pressure pulses as more water is drained from the stock and the incipient paper web is formed.
[0004] Poor control of the fabric deflection within the forming section has been found to have an adverse effect on the formation process, which will in turn have a negative impact on the quality of the paper product being made.
[0005] The actual fabric deflection angle at the edge of each fabric support element in an operating twin fabric forming section has been found to be controlled by several factors. These include:
[0006] 1. the geometric layout of the physical components used in the construction of the forming zone; including the element-to-element pitch for the fabric support elements, the machine direction width of the fabric support elements, and the radius of curvature of the surfaces to which the fabric support elements are attached;
[0007] 2. the level of vacuum applied to the dewatering boxes which controls the degree to which the moving forming fabrics are deflected into the gaps between the fabric support elements; and
[0008] 3. the amount of machine direction tension applied to each of the two moving forming fabrics.
[0009] As used herein, then following terms are to be taken to have the following meanings:
[0010] (i) the term machine direction, or MD, refers to a direction generally parallel to the direction of movement of the forming fabrics away from a headbox slice;
[0011] (ii) the term “pitch” refers to the centre to centre spacing of successive fabric support elements in the machine direction; and
[0012] (iii) the terms “fabric support element” and “fabric support elements” refer:
[0013] either to moving surfaces such as rolls over which a forming fabric moves in rolling contact,
[0014] or to static surfaces such as blades, foils or the like over which a forming fabric moves in sliding contact.
[0015] In the initial stages of sheet formation, when the level of vacuum applied to the machine side of the forming fabric, and consequently to the incipient paper web, is low, the predominant factors controlling forming fabric deflection are the geometry of the forming section and the tension applied to both of the forming fabrics. Further, although the tension applied to the two forming fabrics is usually the same, two different tension levels can be used. The two tensions are set, within the overall pattern of adjustments, to obtain the desired level of pressure pulses within the stock sandwiched between the two moving forming fabrics.
[0016] From the point at which the stock is first sandwiched between the two moving forming fabrics until the point at which the two forming fabrics separate, the consistency of the stock is continually increasing as water is drained from the incipient paper web. At the same time as the stock consistency increases, there is also a corresponding decrease in individual fiber mobility within the stock. These changes require a stronger pressure pulse to provide beneficial fiber movement which will improve the sheet properties in the incipient paper web. However, the incipient paper web eventually reaches a consistency at which no further beneficial fiber movement can occur. From that point onwards until the two moving forming fabrics separate the pressure pulse strength must be controlled by careful selection of the required vacuum level so that drainage continues, and by careful selection of the radius, fabric support element pitch and fabric support element width so that the pressure pulse strength is controlled to a level which will not act to impair formation of the incipient paper web.
[0017] During the initial sheet forming period where beneficial fiber movement can still occur, the need for a larger pressure pulse may increase at a faster rate than can be achieved by control of the vacuum level applied to the forming fabrics alone. This is because the vacuum level must be limited to a value which does not cause excessive drainage which will both reduce fiber mobility and set the sheet properties before the desired formation benefits can be achieved. It is therefore essential to obtain a larger pressure pulse by causing a higher deflection of the forming fabrics at the edges of the fabric support elements by utilizing a wider pitch between them and/or by utilizing a higher radius of curvature in the structure to which the fabric contacting fabric support elements are attached, and/or by utilizing opposed fabric support elements, such as blades, located to increase fabric deflection into the gaps between the fabric support elements.
SUMMARY
[0018] It is thus apparent that there is a matrix of variables which must be considered in order to optimise the quality of the sheet product. The present invention is based on the realization that the following factors must to be taken into account in the creation of an improved twin fabric hybrid type forming section for paper making machine:
[0019] (a) the pitch of the fabric support elements should decrease progressively in the machine direction;
[0020] (b) the level of vacuum applied to the forming fabrics through the dewatering boxes should increase in the machine direction;
[0021] (c) the two forming fabrics together with the stock sandwiched between them should traverse at least four separate and distinct vacuum zones within the forming section as they proceed in the machine direction;
[0022] (d) the level of vacuum applied to the last of the at least four separate and distinct vacuum zones must be higher than the level of vacuum applied to the first of the separate and distinct vacuum zones;
[0023] (e) the level of vacuum applied to the at least four separate and distinct vacuum zones must follow a preselected profile; and
[0024] (f) the dewatering boxes carrying the fabric support elements should be arranged so that the fabric support elements are located in an alternating sequence on the machine sides of both of the forming fabrics.
[0025] Thus in a first broad embodiment this invention seeks to provide a two fabric hybrid type forming section for a paper making machine having a first forming fabric and at least one second forming fabric, such that:
[0026] (i) each of the forming fabrics has a paper side and a machine side;
[0027] (ii) the forming fabrics move together in close proximity with each other in the machine direction with a layer of stock sandwiched in between;
[0028] (iii) the forming fabrics are supported by a series of rolls and/or a series of static fabric contacting fabric support elements over which the machine sides of each of the forming fabrics pass in sliding contact, the fabric support elements being supported on a sequence of dewatering boxes, the dewatering boxes each having a curved fabric support element supporting surface; and
[0029] (iv) the dewatering boxes provide separate drainage zones at least some of which are connected to a source of vacuum to provide separate vacuum zones,
[0030] wherein:
[0031] (a) the forming zone comprises that portion of the forming section between the locus at which the forming fabrics come together to sandwich the stock between them and the locus at which the two forming fabrics separate with the stock continuing on one of them;
[0032] (b) the dewatering boxes provide at least four separate and distinct vacuum zones within the forming section;
[0033] (c) either: the radii of curvature of the curved surfaces located over those dewatering boxes which are connected to a source of vacuum supporting the fabric supporting elements decreases progressively in the machine direction,
[0034] or: the radii of curvature of the curved surfaces located over those dewatering boxes which are connected to a source of vacuum supporting the fabric support elements decreases on successive support surfaces in the machine direction;
[0035] (d) either: the pitch of the fabric support elements within each vacuum zone is constant, and the pitch of the fabric support elements on successive vacuum zones decreases in the machine direction;
[0036] or: the pitch of successive fabric support elements within each vacuum zone decreases in the machine direction.
[0037] (e) the dewatering boxes supporting the fabric support elements are constructed and arranged to locate the fabric support elements in contact with the machine sides of the first forming fabric and the second forming fabric in an alternating sequence in the machine direction;
[0038] (f) on all of the dewatering boxes:
[0039] either: all of the fabric support elements are the same width in the machine direction;
[0040] or: all of the fabric support elements are not the same width in the machine direction.
[0041] Preferably, the fabric support element pitch within each vacuum zone is constant, and the fabric support element pitch within successive vacuum zones decreases in the machine direction. Alternatively, the fabric support element pitch within each vacuum zone is not constant, and the fabric support element pitch within each successive vacuum zone decreases in the machine direction.
[0042] Preferably, the radii of curvature of the curved surfaces supporting the fabric support elements on successive vacuum zones decreases in the machine direction. Alternatively, the radii of curvature of the curved surfaces supporting the fabric support elements on successive vacuum zones decrease progressively in the machine direction.
[0043] Preferably, each dewatering box provides at least one vacuum zone. More preferably, at least one dewatering box provides at least two vacuum zones. Most preferably all of the dewatering boxes provide more than one vacuum zone.
[0044] Preferably, the ratio of the width of the fabric support elements to the width of the gap between them varies from about 1:10 down to about 1:0.5.
BRIEF DESCRIPTION OF THE DRAWINGS
[0045] The invention will now be described with reference to the attached figures in which:
[0046] FIG. 1 shows schematically a two fabric hybrid type forming section according to first embodiment of the invention;
[0047] FIG. 2 shows schematically in more detail the hybrid forming zone of FIG. 1 ;
[0048] FIG. 3 shows schematically an alternative construction to FIG. 2 ; and
[0049] FIG. 4 shows schematically a further alternative construction to that shown in FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0050] Referring first to FIG. 1 , a two fabric hybrid type forming section 1 is shown. The forming section 1 is arranged substantially horizontally; the arrow A indicates the horizontal direction.
[0051] In the forming section of this invention, the formation zone 60 where the sheet is formed on the first forming fabric 2 extends from the breast roll 50 to the couch roll 57 . A layer of stock 7 is ejected from the headbox slice 8 onto the first forming fabric 2 . Within this zone 60 the two fabric hybrid forming section extends from the locus where the first forming fabric 2 carrying the layer of stock 7 contacts the second forming fabric 4 at lead-in box 53 sandwiching the stock 7 between them, to the locus of the turning roll 9 and transfer box 55 where the first and second forming fabrics separate. The sheet continues towards the press section on the first forming fabric 2 . The two forming fabrics move together through the hybrid forming section 1 so that the sheet moves in the machine direction as indicated by arrow A.
[0052] Although the hybrid forming section 1 shown in FIG. 1 includes a single so-called “top wire” forming unit 61 , located on the first forming fabric 2 , other arrangements are possible. For example more than one own headbox delivering additional stock onto the first forming fabric 2 . Each additional unit 61 can also be provided with its own headbox delivering additional stock onto the first forming fabric 2 .
[0053] In the operation of the formation zone 60 , a jet of stock is ejected from the headbox slice 8 to provide a layer 7 of very aqueous stock on the open surface portion 2 A of the first forming fabric 2 . The first forming fabric 2 and the stock layer 7 move together in the machine direction shown by arrow A, over in sequence a forming board 51 , and a series of dewatering boxes and other sundry dewatering devices indicated generally as 52 . The first forming fabric 2 carrying the stock layer 7 then enters the top wire unit 61 of the hybrid forming section 1 . The second forming fabric 4 is brought into contact with the stock layer 7 at this point, so that it becomes sandwiched between the first and second forming fabrics 2 and 4 (see FIG. 2 for more details). The first forming fabric 2 and the second forming fabric 4 , with the stock layer 7 sandwiched between them, then pass with their respective machine sides in contact with a sequence of units. These are: a lead-in dewatering box 53 , a multi-chambered dewatering box 10 , an opposed fabric support element unit 54 and a transfer box 55 . The multi-chambered dewatering box 10 is located with its fabric support elements in contact with the machine side of the second forming fabric only (see FIGS. 2, 3 and 4 ). At the end of the unit 61 the second forming fabric 4 wraps around a turning roll 9 and is thereby taken out of contact with the stock layer 7 . The stock layer 7 carried by the first forming fabric 2 then passes over further dewatering boxes 56 and finally is transferred after the couch roll 57 at the end of the forming section 61 to the press section (not shown) for further processing.
[0054] FIG. 2 shows a more detailed schematic view of the lower part of the two fabric hybrid forming section 1 shown in FIG. 1 . In FIG. 2 the second forming fabric 4 partially wraps around the forming roll 3 with the result that the stock 7 , which is conveyed in the machine direction as indicated by the arrow A, becomes sandwiched between the first forming fabric 2 and the second forming fabric 4 . The two forming fabrics 2 and 4 with the stock layer 7 sandwiched between them then pass over several dewatering devices. The machine side of the first forming fabric 2 passes in sliding contact over the lead-in dewatering box 53 , an opposed fabric support element box 54 and a transfer box 55 . At the same time, the machine side of the second forming fabric 4 passes in sliding contact with the opposed fabric support elements 73 located on the multi-chambered dewatering unit 10 . Box 54 is optional, and the support elements 71 need not all be in contact with the machine side of the fabric 2 . The two forming fabrics 2 and 4 thus pass together in sequence past these four dewatering units in the sequence box 53 , unit 54 , unit 10 and box 55 . After box 55 the second forming fabric 4 wraps around the turning roll 9 and is carried away out of contact with the stock 7 . The stock 7 is carried by the first forming fabric 2 towards the press section (not shown).
[0055] In FIG. 2 , dewatering box 53 , which is referred to as a lead-in box, as shown is provided with two vacuum chambers 63 , 64 . Box 55 , which is referred to as a transfer box, which ensures the transfer of the stock 7 from the second forming fabric 4 to the first forming fabric 2 , as shown is provided with a single vacuum chamber. Either or both of these dewatering boxes 53 and 55 may be internally divided to provide two, or more, separate vacuum chambers each of which is connected to a separate controlled vacuum supply (not shown). A further embodiment is shown in FIG. 4 , in which Box 53 comprises a single vacuum chamber and Box 55 comprises two vacuum chambers 101 , 102 .
[0056] In Box 53 , forming fabric support elements 70 are mounted on the continuously curved fabric support element supporting surface 90 . Box 54 is an opposed fabric support element unit, which is a gravity drainage box. Water removed from the machine side surface of the first forming fabric 2 drops into the box 54 , and is removed therefrom. The box 54 includes fabric support elements 71 , which are mounted on the surface 91 . As this box 54 is on the outside of the convex curve of the two fabrics 2 , 4 , formed by the box 10 , the fabric support elements 71 can be mounted on flexible, adjustable mountings such as those disclosed by McPherson in U.S. Pat. No. 6,361,657. Box 55 is provided with a plurality of fabric support elements 72 supported by the continuously curved surface 96 .
[0057] FIG. 2 also shows a multi-chambered dewatering unit 10 . As shown, unit 10 includes four distinct vacuum zones 80 , 81 , 82 and 83 , each of which is provided with a separate controlled vacuum supply (not shown). Located beneath each of the separate vacuum zones 80 , 81 , and 82 is a set of fabric support elements, as at 73 . The fabric support elements 73 are supported on the curved surfaces 92 , 93 and 94 .
[0058] There are several possibilities for the radii of curvature of the three surfaces 92 , 93 and 94 .
[0059] (i) The three radii of curvature can be the same, so that all three surfaces 92 , 93 and 94 together form a single constant radius curve.
[0060] (ii) At least one of the three radii can be different, or all three can be different. If this arrangement is adopted, then the radius of curvature of each of the surfaces 92 , 93 and 94 must decrease in the machine direction, so that the radius of curvature of the surface 94 is always the smallest of the three.
[0061] It also apparent from FIG. 2 that the pitch of the fabric support elements 73 on the multi-chambered dewatering unit 10 is not constant. The pitch decreases in the machine direction.
[0062] In FIG. 2 , fabric support element 74 which is the first element of the set 73 , is located on the upstream side of zone 80 towards the headbox slice and is a so-called autoslice blade, also known as a skimmer blade. When in use, the autoslice blade 74 skims excess water from the machine side of the second forming fabric 4 as it passes in the machine direction in sliding contact with the element 74 .
[0063] FIG. 3 is similar to FIG. 2 , with the exception that on box 53 the radius of curvature of the curved fabric support element supporting surface 90 is not constant. The surface 90 is broken into successive portions having radii of curvature R 1 , R 2 and R 3 . The radius of curvature for each portion decreases in the machine direction, so that R 1 is the largest radius of curvature. By decreasing the radius of curvature of the supporting surface 90 for the fabric support elements 70 located on the lead-in box 53 so as to increase sequentially the amount of wrap of the first and second forming fabrics 2 , 4 the stock 7 is subjected to increasingly stronger pressure pulses, which induce shearing actions within the stock 7 , at each edge of the fabric support elements 70 as the forming fabrics 2 , 4 pass over them in the machine direction. This feature is also shown in each of the dewatering boxes 53 , 54 , 10 and 55 .
[0064] FIG. 4 is also similar to FIG. 2 except that the individual or discrete fabric support elements 70 of the lead-in box 53 are replaced by the continuous curved surface 100 mounted on support surface 90 , as described by Buchanan et al. in US 2003/017438. In addition, the transfer box 55 has been internally portioned to provide two separate vacuum zones 101 and 102 , each of which is provided with its own controlled vacuum supply (not shown).
[0065] In the drawings the fabric support elements are all shown schematically to have the same width in the machine direction. In practise, the fabric support element width may not be the same for all of the dewatering boxes. Some dewatering boxes may require a different width fabric support element just to accommodate the volume of white water which is being drained from the forming fabrics at that location. It is also possible that a different width fabric support element may be required in order to obtain the desired level of pressure pulse within the stock at a given location. Experience shows that the ratio of the machine direction width of fabric support elements to the width of the gap between them should be from about 1:10 to about 1:0.5.
[0066] In the drawings dewatering boxes are shown which have more than one chamber to each of which a controlled level of vacuum is applied. If the vacuum levels in adjacent chambers or dewatering boxes are not the same, it is desirable that the surface curvatures, and possibly also the corresponding fabric support element pitch, also should not be the same. Furthermore experience shows that it is desirable that the vacuum level in a sequence of dewatering boxes or chambers should increase relatively smoothly in the machine direction. Although the vacuum level can remain constant in two adjacent dewatering boxes or chambers it should not decrease in the machine direction, and furthermore spikes of radically different pressure should be avoided. In other words, all of the variables do not necessarily change smoothly in a step wise fashion; adjacent zones can have the same values for at least some of the variables.
|
A twin fabric hybrid forming section for paper making machine is described in which: the pitch of the fabric support elements decreases progressively in the machine direction; the level of vacuum applied to the forming fabrics through the dewatering boxes increases in the machine direction; the two forming fabrics together with the stock sandwiched between them traverse at least four separate and distinct vacuum zones within the forming section as they proceed in the machine direction; the level of vacuum applied to the last of the at least four separate and distinct vacuum zones is higher than the level of vacuum applied to the first of the separate and distinct vacuum zones; the level of vacuum applied to the at least four separate and distinct vacuum zones follows a preselected profile; and the dewatering boxes carrying the fabric support elements are arranged so that the fabric support elements are located in an alternating sequence on the machine sides of both of the forming fabrics.
| 3
|
This is a continuation of co-pending application Ser. No. 07/087,555 filed on Aug. 20, 1987, now U.S. Pat. No. 4,837,907.
BACKGROUND OF THE INVENTION
This invention relates to rolls for processing travelling web material, such as paper being made on a papermaking machine. More particularly, this invention relates to a so-called self-loading controlled deflection roll wherein pressure means is located within the roll to exert force against the inner peripheral surface of the roll shell at one or more locations to control the deflection of the roll shell along a longitudinally-extending line on its surface to be straight, or curved upwardly or downwardly, a controlled amount, as desired. Still more particularly, this invention relates to a self-loading controlled deflection roll wherein the roll shell is capable of being driven while simultaneously being moved laterally, or transversely, relative to its longitudinal axis.
Self-loading controlled deflection rolls are known. Examples are shown and described in U S. Pat. Nos. 3,885,283, 4,048,701 and 4,520,723. There are also many arrangements for driving controlled deflection rolls. These designs are often complicated due to the fact that the roll shell must be driven relative to its stationary support beam. This is further complicated by the fact that the roll shell must accommodate some flexing which occurs during operation of its controlled deflection structure, and the roll surface must be capable of moving into, and out of, nip engagement with a mating roll.
Prior self-loading controlled deflection rolls utilize self-aligning bearings on either end to accommodate the small, but significant, flexule motion of the roll shell about an axis transverse to its axis of rotation. Prior self-loading controlled deflection rolls also utilize a drive gearbox which requires its own bearings to support it independent of the roll shell.
Some prior self-loading controlled deflection rolls utilize sliding collars, or yokes, on which the inner race of the bearings on which the roll shell is rotatably mounted are in turn mounted to the sliding yokes to provide the lateral movement of the roll shell relative to the stationary roll shaft, or support beam. Such an arrangement is shown and described in the Biondetti, U.S. Pat. No. 3,885,283. This arrangement requires close tolerances for accurate operation, but these same close tolerances require costly accurate finishing of the surfaces brought into sliding engagement. On the other hand, loose tolerances can permit undesirable vibration.
Prior arrangements for driving a controlled deflection roll are very complex due to the need to support the stationary roll support beam while providing driving force to the roll shell. These arrangements often necessitated the use of triple-race bearings which are extremely expensive. Finally, controlled deflection rolls driven by any prior drive which is concentric with the longitudinal axis of the support beam can't accommodate lateral movement of the roll shell relative to the support beam.
SUMMARY OF THE INVENTION
This invention provides apparatus which permits self-loading of the roll shell into nipping engagement with a mating roll without having to move the support beams of either roll. It also provides controlled deflection operation of the roll where the entire roll shell can move laterally relataive to its longitudinal axis of rotation. Finally, it provides both the self-loading and controlled deflection operations of the roll while simultaneously providing direct drive of the roll shell relative to the stationary support beam.
In this invention, the roll shell is mounted to an end assembly which is supported in a bearing housing on non-self-aligned bearings, such as tapered roller bearings. This establishes and maintains a rigid alignment between the roll shell and the bearing housing.
At one end of the roll, a ring gear comprises part of the end assembly and is also thereby rigidly aligned with the bearing housing at that end. A driveshaft having a drive gear is rotatably mounted in this bearing housing with the drive gear in engagement with the ring gear to provide rotational drive for the roll shell. Since the driveshaft is mounted in the same bearing housing as the ring gear driving the roll shell, alignment of the drive gear and ring gear is established and maintained under all operating conditions.
The bearing housings at either end of the roll are pivotally-attached to support stands at a location offset from the longitudinal axis of the roll. The center support beam of the roll is also pivotally-supported in these same support stands. This arrangement allows for movement of the bearing housings and roll shell surface relative to the center shaft.
Within the controlled deflection roll is one or more pressure elements, such as shoes, which are actuated by one or more pistons to provide lateral movement of the roll shell and/or deflection control, as desired, which is independent of any movement of the roll support beam This permits the support stands at either end of the roll to be mounted directly to the support stands, or bearing housings, of a roll to be mated in nipping engagement with the self-loading controlled deflection roll.
Accordingly, when it is desired to open or close the nip between mating rolls, or to control the deflection of the controlled deflection roll, the forces exerted between the support beam and roll shell are taken up entirely by the connections between the support stands of the two rolls and no nip loading forces are transmitted to the machine framework supporting either of the rolls.
Since non-self-aligned bearings are used to support the roll shell, rigid alignment of the roll shell relative to the bearing housing is maintained and the bearing housings can, therefore, be used as a gear box. This permits the driveshaft and drive gear to be mounted in the same bearing housing as the ring gear which drives the roll shell.
Accordingly, it is an object of this invention to provide a self-loading controlled deflection roll wherein the roll drive is combined with the shell bearing mounting and housing.
Another object of this invention is to provide a self-loading controlled deflection roll wherein the roll shell is not supported by self-aligning bearings.
Still another object of this invention is to provide a self-loading controlled deflection roll wherein the function of the gearbox bearings and the shell rotatable support bearings are combined.
A feature and object of this invention is the provision of a controlled deflection roll wherein the bearings maintain rigid alignment between the roll shell and the bearing housings.
Another feature of this invention is the provision of a self-loading controlled deflection roll having bearing housings which are externally pivoted.
Yet another feature and advantage of the invention is the provision of a self-loading controlled deflection roll which is simple in construction and which can use external pressure cylinders to either lift the roll into, or out of, nipping engagement, or to apply edge pressure at the edges of mating rolls.
These, and other, objects, features and advantages of the invention will be readily apparent to those skilled in the art upon reading the following description of the preferred embodiments in conjunction with the attached drawings and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an end elevational view of the self-loading controlled deflection roll mounted beneath a mating roll and having pressure cylinders attached to each bearing housing.
FIG. 2 is a side elevational view of one end of the roll couple shown in FIG. 1.
FIG. 3 is an end elevational view of the self-loading controlled deflection roll and mating roll similar to the apparatus shown in FIG. 1, but without the pressure cylinders between the bearing housings and support stands.
FIG. 4 is a top sectional view of the self-loading controlled deflection roll.
FIG. 5 is a side elevational view, partially in section, of the apparatus shown in FIG. 2.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With particular reference to FIGS. 4 and 5, a self-loading controlled deflection roll 4 is shown which has a stationary support beam 10 and its end journals 11 pivotally mounted into support stands 13 at either end. A hollow, cylindrical roll shell 12 is disposed about the support beam. One or more bearing support shoes 42, which operate according to either the well known hydrostatic or hydrodynamic principles, and supported by one or more pistons 40 mounted in corresponding cavities in the support beam 10, are disposed in the space between the support beam and the inner surface of the roll shell to provide support elements of the roll shell on the beam. At either end of the roll shell is a roll end assembly 14 which includes a circular flange 17 that is attached with capscrews 8 so as to be concentric with the roll shell about its longitudinal axis 6. Securely attached in the roll end assembly at the front end of the roll is a bearing ring 18. Similarly, attached in the roll end assembly at the back end of the roll is a ring gear 20. Thus, the roll end assemblies comprise flanges 14 and bearing ring 18 or ring gear 20.
At the front end of the roll is a front bearing housing 22 and at the rear end of the roll is a rear bearing housing 23. The roll bearing ring 18 and ring gear 20 of the end assemblies are rotatably mounted in the bearing housings by tapered roller bearings 16. These tapered roller bearings are non-self-aligning bearings. The significance of this fact is that tapered roller bearings do not permit any pivotal motion between their inner and outer races about an axis transverse to their axis of revolution. Thus, the bearing ring 18 and ring gear 20 also cannot move about an axis transverse to the axis of roll shell rotation.
Referring to FIGS. 1-3, the bearing housings 22,23 are, in turn, pivotally mounted to the support stands 13 with pivot arms 24 in which spherical bushings 26 are mounted to rotate about shafts or pins 27. These bearing housing pivots are located in a plane 34 (FIGS. 1 and 3) which is essentially horizontal and which is perpendicular to plane 36 which extends through the axes of rotation 6,3 of the self-loading controlled deflection roll 4 and its mating roll 2, respectively, shoe 42 and the nip line N of contact therebetween.
Referring to FIG. 5, a driveshaft 28 is mounted in back bearing housing 23 with driveshaft bearings 30 near either end to rotate about its longitudinal axis 5 which is parallel to axis 6 about which roll shell 12 rotates. A drive gear 32 is secured to the driveshaft and engages the ring gear 20. Since the driveshaft 28 and ring gear 20 are both secured in the same bearing housing 23, rigid alignment of drive gear 32 and ring gear 20 is maintained since the ring gear bearings 16 are not self-aligning bearings. In other words, the tapered roller bearings maintain rigid alignment of their inner and outer races, and corresponding alignment of the ring gear in the bearing housing.
In another embodiment, shown in FIG. 1, pressure cylinders 38 are mounted between the support stands 13 and front and back bearing housings 22,23 to provide pivotal movement of the self-loading controlled deflection roll 4 about their pivot shafts 27. When the controlled deflection roll is mounted in the lower position relative to a mating roll 2, as shown in FIG. 1, these pressure cylinders 38, which typically take the form of hydraulic cylinders actuated by pressurized hydraulic fluid, can be operated to increase or decrease the loading applied to the edges of the roll due to the proximity of their attachment to the bearing housings through their pivot arms 24. In the manufacture of paper, regardless of whether the controlled deflection roll is used in the press or calender sections of a papermaking machine, such control of the edges of the paper web travelling through the machine is vital to ensure uniformity of paper caliper and finish in the cross-machine direction.
When the controlled deflection roll is mounted in the upper position relative to its mating roll 2, such as if the embodiment shown in FIG. 1 were rotated 180°, pressure cylinders 38 could be actuated to raise roll 4 upwardly and away from nipping engagement with its mating roll 2. This would avoid the necessity of otherwise providing some internal apparatus, such as a pressurized piston and shoe arrangement mounted in the controlled deflection roll shaft opposite the piston 40 and shoe 42. In this upper position, pressure cylinders 38 can also be used to effect changes in pressure applied to the edges of the nip line of contact N between the mating rolls and, thereby, control the web caliper and finish at these locations.
In operation, with reference to FIGS. 4 and 5, controlled deflection roll 4 is pivotally secured into its stand 13 by its journals 11. Its roll shell 12 is rotatably mounted on its non-self-aligned bearings, such as tapered roller bearings 16, within front and back bearing housings 22,23 which are pivotally mounted to stands 13 by pivot shafts 27. Driveshaft 28 is linked with a flexible drive (not shown) to a source of power, such as a motor which also is not shown, and rotates drive gear 32 which engages ring gear 20 to rotate the roll shell.
A supply of pressurized fluid, such as hydraulic oil 44, in the controlled deflection roll is urged against the bottom of one or more pistons 40 to cause one or more shoes 42 to apply force to the inner surface of roll shell 12 beneath nip line N and either control its deflection or produce a crown in the surface of the roll shell along its nip line of contact N with mating roll 2. The manner in which the controlled deflection roll applies force to the inner side of the roll shell is well known in the art, and, therefore, it will not be discussed in further detail. In this regard, reference is made to U.S. Pat. No. 3,276,102 whose teaching is incorporated herein by reference. One or more pistons, with one or more corresponding shoes, can be used as the support elements to support the roll shell 12 relative to the roll shaft 10. Similarly, the operation of the shoes can be according to either the well known hydrostatic or hydrodynamic principles.
Actuation of the shoe and piston support elements cause the roll shell 12 to move laterally, or transversely, relative to the longidutinal axis 6 as shown by double-headed arrow 9. Since the support beam 10 is secured by its journals in stands 13, the actuation of the piston and consequential transverse movement of the roll shell causes the front and back bearing housings 22,23 to rotate upwardly, with reference to FIG. 3, about pivot shafts 27. In this upwardly extended, or loaded, position, the roll axis of rotation 6 is no longer coincident with the longitudinal axis of the roll through its journals. There is no skewing or relative motion between the driveshaft 28, gears 32, 20 and the roll shell 12 since they all move with back bearing housing 23. The roll is thus self-loading in that the roll shell 12 is moved laterally into nipping engagement with a mating roll 2 by actuation of the internal support elements of the roll itself. The reaction forces on the support beam 10 may cause some downward deflection of the beam. This deflection is accommodated by the spherical bushings 15 on journals 11 in the support stands 13 on either end of the roll. Mating roll 2 is held into engagement with the controlled deflection roll 4 by having its bearing housings 7 and support stands 46, which can be integral, secured to the support stands 13 by bolts 48. All nip loading and reaction forces are taken up by the support stands and the bolts holding them together. No loads are transmitted to any swing arms since there aren't any, or to any of the papermaking machine framework.
After the rolls have been loaded into nipping engagement, further actuation of the piston, or pistons, can be effected to control the deflection of the roll shell along its nip line of contact in a manner well known in the art.
When it is desired to unload the rolls from nipping engagement, the piston, or pistons, are deactuated and the roll shell 12 pivots downwardly about its pivot shafts 27 to create a gap between rolls 2 and 4.
In the embodiment shown in FIG. 1, the operation is essentially the same as described above, however, pressure cylinders 38 pivotally link the bearing housings 22,23 with the support stands 13. The pressure cylinders can be used to effect, or augment, the loading and unloading of the controlled deflection roll, if desired.
Thus, a self-loading controlled deflection roll which achieves the objectives and includes the features and advantages set forth has been disclosed. Variations in the specific structures disclosed in the preferred embodiments may be made without departing from the spirit and scope of the invention as claimed. For example, while tapered roller bearings have been recited in the preferred embodiment, this is by way of example only and any other bearing which can maintain rigid alignment between the ring gear and roll shell can be used.
Also, while the bearing housings have been shown and described in the preferred embodiment as being pivotally-supported and linked in the support stands, other means for supporting and linking the bearing housings with the support stands, such as by sliding pins and stops are contemplated and intended to be within the scope of the invention.
|
A self-loading controlled deflection roll is rotatably mounted with non-self-aligning bearings at either end to bearing housings which, in turn, are pivotally-mounted to support stands. The stationary support beam extending through the roll is pivotally-mounted in the same support stands. At one end of the roll, a drive shaft having a drive gear engaging a ring gear which is mounted on the end of the roll shell concentric with its surface is provided to rotatably drive the roll shell while simultaneously permitting lateral movement of the roll shell relative to the support beam during the self-loading phase of roll oepration.
| 5
|
BACKGROUND OF THE INVENTION
The invention relates to a textile web, especially a textile-covered web for a paper-making machine, which, viewed from a transverse direction, is provided with several web sections that extend parallel to one another in a lengthwise direction and are aligned adjacent to one another, with their lateral edges being attached to one another via fasteners.
Textile webs of the type described above are used primarily to transport paper webs through a paper-making machine (GB-A-975 750; EP-B-0 464 258; U.S. Pat. No. 5,360, 656). They are comprised of web sections extending lengthwise across the web, with the width of the sections being considerably narrower than the actual width of the textile web. The web sections extend primarily in a lengthwise direction along the textile web, sometimes at a slight angle to it. The textile web is thus designed such that one or more strips of textile are progressively wound in a lengthwise direction to the textile web, and spirally, crosswise to it.
The web sections may be comprised of structural fibers, for example in the form of a woven fabric. The structural fibers may, however, also form a support base, to which a carded fibre batt tissue is needle-punched on one or both sides, so that the final textile web forms a felt. Such felts are suited especially for use in guiding the paper web in the pressing section of a paper-making machine.
With known textile webs of this type, the individual web sections do not overlap one another, they actually push up against one another along their lateral edges. In such cases, in order to ensure adequate lateral stability, the lateral edges are connected to one another. In the abovementioned documents, it is, therefore, proposed that the lateral edges be sewn together via a zigzag stitch, that they be fused or welded, for example, by ultrasonic welding. As an alternative, the above mentioned documents propose that the lateral edges be provided with seam loops and the connection be made via a wire pushed through the seam loops.
In EP-0 947 623, a connection for the web sections is proposed, which consists of cross thread sections that project beyond the lateral edges of the web sections and overlap, interlocking with one another, and of a joining thread that is bonded to these sections. The establishment of such a connection is not without problems, however, and difficulties arise in matching the porosity of the area around the lateral edges to the porosity of the remaining areas of the web sections. In a paper-making machine it is important, however, that the porosity of the textile web be even over the entire width of the web. A further requirement is that the connection of the web sections one over the other be as firm as possible both in a crosswise and in a lengthwise direction.
SUMMARY OF THE INVENTION
The object of the present invention is to design a method for connecting the lateral edges of the web sections in a textile web of the type described at the beginning, such that it is easier to produce and possesses a high degree of stability, but its porosity does not deviate substantially from the porosity of other areas of the textile web.
This object is attained in accordance with the invention in that the adjacent lateral edges of the web sections follow a meandering course, with alternating projections and recesses, and the web sections are interlocked with one another via these projections and recesses, and in that the fasteners connect the projections to one another, in that they extend preferably in a lengthwise direction and are designed to be continuous, to the greatest extent possible.
Thus, the basic premise of the invention is that the lateral edges of the web sections are not straight—as in the current state of the art—but meander, with interlocking projections and recesses, as with toothed gears, and the connection of the adjacent web sections is accomplished via the fasteners used to connect the projections. This type of connection is relatively simple in comparison with known types of connections, and can be machine-produced. It has been found that a connection that is very firm both in a lengthwise and in a crosswise direction can be produced, without the porosity of the area around the lateral edges of the textile web deviating substantially from the porosity of other areas.
The fasteners may be designed, for example, as sewn seams, which preferably extend parallel to the lengthwise direction of the web sections, with several parallel sewn seams being provided per connection. Instead of, or in combination with, such sewn seams, sections of adhesive tape may be used, which cover the area of the projections and recesses partially or, preferably, completely, and may even extend beyond this area. In special cases, the sections of adhesive tape may contain heat-bonding adhesive, or be composed thereof. The heat-bonding adhesive may be activated via heat and pressure once the sections of adhesive tape have been put in place. In order to keep the porosity in this area from being substantially reduced, the sections of adhesive tape should be designed to be porous, in other words they should contain holes, which will ensure sufficient open crosswise surface area.
The sections of adhesive tape may be designed in many different ways. For instance, bonding sheets provided with an adhesive coating may be used, wherein the adhesive coating may consist of a suitable adhesive, such as the above mentioned heat-bonding adhesive. In order to ensure adequate porosity, the bonding sheets should be perforated.
Instead of the above, or in combination with it, the sections of adhesive tape may also be designed as spunbonded tissue, preferably equipped with heat-bonding adhesive fibers. The advantage of using such sections of adhesive tape is that they can be cut to fit, such that they will not seriously affect the porosity of the area in question, and such that their structure will correspond to the structure of the other areas. By activating the heat-bonding fibers via heat and pressure, a firm connection between the interlocking projections is produced. The heat-bonding fibers may consist entirely of heat bonding adhesive, in which case it is advantageous for them to be present only proportionally in the non-woven tissue that forms the section of adhesive tape. They may, however, also be designed as bicomponent fibers, in which heat-bonding adhesive is proportionally present.
Regarding the meandering design of the lateral edges, various shapes are possible, for example wave-type or zigzag shapes. The projections, however, may also be trapezoidal or rectangular in shape. Other shapes for the lateral edges are also possible.
The web sections may be provided with a support base, as is known in the art, or may even be composed thereof, wherein the support base takes up the lengthwise and crosswise forces that act upon the textile web. To the extent that the textile web is to be designed as a felt, such as a press felt designed specifically for use in the pressing section of a paper-making machine, the supports may be needle-punched with spunbonded tissues, so that a felt-like surface is formed on both sides.
Suitable support bases include woven fabrics, knitted fabrics, or even reinforced spunbonded tissues, wherein the woven fabrics, knitted fabrics or spunbonded tissues are used in several layers, and may even be used in combination with one another.
Synthetic netting—in single or multiple layers, alone or in combination with the above mentioned types of support bases—may also be provided, as is described, for example, in EP-B-0 285 376, EP-A-0 307 182, WO 91/02642, or WO 92/17643. The advantage of synthetic netting is that it will edges, and thus offers a firm hold on the fasteners that extend over the projections. For this reason it is immaterial whether the individual webs of synthetic netting extend in a lengthwise or crosswise direction, or run diagonally. The synthetic netting may be produced as described in the above-named documents. One particularly efficient method for producing synthetic netting of this type consists in using extrusion technology, as is described, for example, in U.S. Pat. Nos. 4,123,491, 3,917,889, and 3,767,353.
The width of the area comprising the projections and recesses may be determined in accordance with given stability requirements. Advantageously, an area of up to 50 cm in width is suitable, with areas ranging from 10 to 20 cm being preferred.
BRIEF DESCRIPTION OF THE DRAWING
In the diagrams, the invention is described in greater detail using exemplary embodiments. These show:
FIG. 1 an overhead view of a device used in producing a textile web with web sections;
FIG. 2 an overhead view of two web sections connected by a first type of connection;
FIG. 3 an overhead view of two web sections connected by a second type of connection;
FIG. 4 an overhead view of the interlocking area between two web sections, connected by a third type of connection;
FIG. 5 an overhead view of the interlocking area, with a fourth type of connection;
FIG. 6 an overhead view of the interlocking area with a fifth type of connection;
FIG. 7 an overhead view of a web section of a textile web with woven support base and needle-punched spunbonded tissue;
FIG. 8 an overhead view of a web section of a textile web with a knitted support base and needle-punched tissue and
FIG. 9 an overhead view of a web section of a textile web with netting support base and spunbonded tissue.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The device 1 illustrated in FIG. 1 is equipped with two separate rollers 2 , 3 driven in the same direction. A strip of textile 5 is drawn from a supply roll 4 . The supply roll 4 is set at a slight angle, and when the strip of textile is drawn from it, it moves in the direction of the arrow A, in other words in a crosswise direction. This causes the strip of textile to be wound spirally onto the two rollers 2 , 3 , until a desired width has been reached. In this, the advance in the direction of the arrow A is calculated such that web sections—indicated here by the number 6 —form, adjacent to one another, such that their lateral edges push up against one another.
The spiral rolling of the strip of textile 5 may also be performed in a number of layers, in that the supply roll 4 , upon reaching the final width, is moved back, with the angle of discharge being adjusted accordingly. This is described in detail in EP-B-0 464 258 and U.S. Pat. No. 5,360,656. However, it is also possible for two loops having positive and negative angles of inclination to be positioned one above the other.
In the representation illustrated in FIG. 1, the lateral edges of the web sections 6 are shown straight for purposes of increased clarity. In FIGS. 2 through 5, various examples of lateral edge shapes are illustrated, in accordance with the invention.
FIG. 2 shows two adjacent web sections 7 , 8 , whose lateral edges 9 , 10 , or 11 , 12 are wave-like in shape, so that projections—indicated here by the number 13 —and recesses—indicated here by the number 14 —are produced. The web sections 7 , 8 are positioned adjacent to one another such that the projections 13 and recesses 14 become interlocked with one another, in other words such that each projection 13 fits into the recess 14 the lies opposite it.
The two web sections 7 , 8 are connected via three seams that run parallel to one another, extending lengthwise along the web sections 7 , 8 over the projections 13 , connecting them to one another. The course of the seams 15 , 16 , 17 ensures that the two web sections 7 , 8 are firmly joined to one another.
In the exemplary embodiment illustrated in FIG. 3, the same web sections 7 , 8 are used, in other words they also have wave-shaped lateral edges 9 , 10 , 11 , 12 , in which projections 13 and recesses 14 are formed. In this case, instead of seams 15 , 16 , 17 , the sections are connected via a section of adhesive tape 18 , which extends in a lengthwise direction along the web sections 7 , 8 , and covers the area of the projections 13 , 14 and the immediately adjacent areas. The section of adhesive tape 18 consists of a spunbonded tissue equipped with heat-bonding adhesive. Through the effects of heat and pressure, the heat-bonding fibers are activated, so that, once cooled, a firm connection is established between the two web sections 7 , 8 .
FIG. 4 shows a further embodiment of adjacent web sections 19 , 20 . The shape of their lateral edges 21 , 22 is such that trapezoidal projections—indicated here by the number 23 —and recesses—indicated here by the number 24 —are formed, wherein the projections 23 become narrower as they move away from the lateral edges 21 , 22 to which they are attached.
As with the exemplary embodiments illustrated in FIGS. 2 and 3, the web sections 19 , 20 are positioned adjacent to one another such that the projections 23 and recesses 24 become interlocked. Two parallel seams 25 , 26 extend over these projections 23 , running in a lengthwise direction along the web sections 19 , 20 , and connecting the web sections 19 , 20 .
In the exemplary embodiment illustrated in FIG. 5, two web sections 27 , 28 are provided, whose lateral edges 29 , 30 are designed such that both trapezoidal projections—indicated by the number 31 —and trapezoidal recesses—indicated by the number 32 —are formed, however the width of the projections and recesses is narrower toward the lateral edges 29 , 30 of the web, in contrast to the exemplary embodiment illustrated in FIG. 4 . In this case as well, the web sections 27 , 28 are positioned adjacent to one another such that the projections 31 and recesses 32 become interlocked. The connection is produced via two parallel seams 33 , 34 , which extend approximately along the center of the projections 31 , joining them to one another.
In the exemplary embodiment according to FIG. 6, two web sections 32 , 33 are envisioned whose lateral edges 34 , 35 extend in such a way that rectangular projections—indicated here as an example with the number 36 —and recesses—indicated here as an example with the number 37 —are produced. The web sections 32 , 33 are positioned adjacent to one another is such a way that the projections 36 and recesses 37 become interlocked with one another. Three parallel seams 38 , 39 , 40 extend over these projections 36 , running in a lengthwise direction along the web sections 32 , 33 and connecting them.
It goes without saying that the connection shown in the embodiments illustrated in FIGS. 4, 5 and 6 may also be produced via a section of adhesive tape, in the manner illustrated in FIG. 3 .
FIGS. 7, 8 and 9 show sections of web sections 41 , 42 , 43 in an overhead view. The web sections have a support base 44 , 45 , 46 to which the spunbonded tissue is needle-punched. The spunbonded tissues 47 , 48 , 49 were omitted in part in order to reveal that support bases 44 , 45 , 46 located beneath them.
In the exemplary embodiment according to FIG. 7 the support base is woven from longitudinal threads—indicated here as an example with the number 50 —and cross threads—indicated here as an example with the number 51 —as a basket weave. The exemplary embodiment according to FIG. 8 demonstrates a support base that is knitted from a multitude of threads—indicated here as an example with the number 52 . In the exemplary embodiment according to FIG. 9 the support base 46 is comprised of an extruded netting with longitudinal wires—indicated here as an example with 53 —and cross wires—indicated here with the number 54 —that are connected to one another with self-substance and consisting of a suitable plastic, e.g. polyamide.
Furthermore, the present invention is not limited to spirally rolled strips of textile. The individual web sections may also be made of individual pieces positioned adjacent to one another, such that they extend not at a slight angle but precisely in a lengthwise direction.
|
The invention relates to a textile web, especially a textile-covered web for a paper-making machine, which, viewed from a transverse direction, is provided with several web sections ( 6, 7, 8, 19, 20, 27, 28 ) that extend parallel to one another in a lengthwise direction and are aligned adjacent to one another, with their lateral edges ( 9, 10, 11, 12, 21, 22, 29, 30 ) being attached to one another via fasteners ( 15, 16, 17, 18, 25, 26, 33, 34 ). This textile web is characterized in that the adjacent lateral edges ( 10, 11, 21, 22, 29, 30 ) follow a meandering course with alternating projections ( 13, 23, 31 ) and recesses ( 14, 24, 32 ), and the web sections ( 6, 7, 8, 19, 20, 27, 28 ) are interlocked with one another via these projections ( 13, 23, 31 ) and recesses ( 14, 24, 32 ), and in that the fasteners ( 15, 16, 17, 18, 25, 26, 33, 34 ) connect the projections ( 13, 23, 31 ) to one another.
| 3
|
BACKGROUND OF THE INVENTION
The present invention relates to methods for improving cheese production by utilizing plasmin-regulating agents to maintain plasmin in the animal's milk at levels less than 0.2 mg/l milk. All animals whose milk is used to produce cheese benefit from the administration of the plasmin-affecting agents of the present invention. For instance, milk from cows, sheep, goats or even buffalo, to name a few, is used in cheese production. One such compound is bovine somatotropin (hereinafter referred to as BST).
Plasmin is a component of an animal's blood and appears to be involved with fibrinolysis primarily. However, plasmin also has been implicated in cell migration and differentiation, involution of the uterus and mammary gland. Often times, plasminogen activator is synthesized by the target tissue in order to generate localized plasmin production.
Plasmin interacts with milk and cheese in a very particular manner. It seems that milk plasmin increases in late lactation resulting in the increased formation of gamma caseins from the proteolysis of alpha-s and beta casein (Donnelly, 1983). Observed at the same time is an increase in plasminogen activator during natural mammary gland involution or during hormonally induced involution in cell culture. Such an increase in plasminogen activators may be speculated to increase plasmin concentrations with a subsequent degradation of milk proteins.
Recently, an increase in bovine milk plasmin has been observed in late lactation. Further, bovine milk also fluctuates in milk plasmin concentrations depending on the season of the year. Generally, in the spring plasmin and plasminogen are lower, and in the winter plasmin and plasminogen seem to be higher. Additionally, during mastitis or during periods of elevated somatic cell counts, milk plasmin seems to be increased. The decrease in the integrity of the alveslar epithelia within the mammary gland results in an increased transfer of blood plasminogen/plasmin to milk.
Proteolysis of kappa-casein is necessary in cheese production. However, excess non-specific proteolyisis reduces firmness when cheese is being produced. In the more neutral pH cheeses, such as swiss cheese, plasmin is highest, and it is lowest in the acid cheeses such as cheshire cheese. Plasmin degrades beta casein into three components. Also, plasmin has been reported to induce gelation of ultra high temperature pasteurized milk. The formation of amino acids during cheddar cheese ripening yields production of bitter flavors in milk and dairy products and decreasing cheese yield and quality. If milk is incubated with plasmin longer than four hours there is a resulting increase in time necessary to form a rennet clot which is necessary in cheese production.
Difficulties in cheese production from milk exposed to increased levels of plasmin concentration are observed due to seasonal calving in some parts of the world, and therefore, a method to increase cheese production is desireable and will allow cheese manufacture help in such areas of cheese shortages. If milk is processed 1 to 3 days after it is collected from the cow, obviously a high level of plasmin coupled with long incubation time will degrade the alpha-s and beta caseins thereby reducing cheese yield. External modulators which can minimize fluctuation in plasma concentration over lactation or prevent plasmin increases during diseases (mastitis) have tremendous potential in insuring consistent milk for cheese processing and results.
Surprisingly, it has been observed that with injections of recombinant bovine somatotropin (BST), as an example of a plasmin-regulating agent, milk plasmin concentrations observed in late lactations revert to those of early lactation, i.e., the milk plasmin concentration decreases. Thus, a method to improve cheese production yields by administering compounds which decrease milk plasmin levels is provided herein.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1: Relationship between milk plasmin concentration and milk yield in control and rBST-injected cows. Plasmin concentration shown in circles for milk from control ( ) or rBST-injected cows ( ). -Daily milk yield shown in squares for milk from control (□) or rBST-injected cows ( ). All values represent least squares means.
FIG. 2: Effect of rBST-injections on milk plasminogen and plasmin concentration through lactation and 3 days after drying off. Plasmin concentrations are represented for control cows ( ) and rBST-injected cows ( ). Milk plasminogen concentrations are shown for control cows (□) and rBST-injected cows ( ). All values represent least squares means.
FIG. 3A-3B: Relationship between daily milk yield and milk plasmin concentration (mean, n=4) during cessation and resumption of rBST treatment in late lactation. Dark areas on the X axis indicate daily rBST injections. Light areas on the Y axis indicate cessation of rBST injections.
SUMMARY OF THE INVENTION
The present invention, therefore, provides methods for improving cheese production yields by administering to a milk-producing animal, a plasmin-affecting amount of a plasmin-regulating agent. Specifically, plasmin levels maintained in milk used to produce cheese of less than 0.2 mg/l of milk (0.2 mg/l to 0.001 mg/l) provide the beneficial improvement in cheese production.
The plasmin-regulating agents of the present invention include exogenous animal somatotropins, such as bovine somatotropin, ovine somatotropin, caprine somatotropin, and even buffalo somatotropin. Also, included as another example of a plasmin-regulating agent useful in the present invention is epsilon-amino caproic acid.
It is an object of the present invention, therefore, to provide methods for improving cheese production by administering a plasmin-regulating agent to an animal whose milk is used in cheese production in order to provide milk that is more suitable and increases cheese quality and/or production. Further, it is an object of the present invention to provide methods for increasing cheese production by utilizing milk that has been derived from cows administered such agents. One such agent is recombinantly derived bovine somatotropin (rBST). Another such component is episilon-amino caproic acid. These and further objects of the invention will become obvious by the more detailed description of the invention provided hereinafter.
DETAILED DESCRIPTION OF INVENTION
The following examples are provided as illustrative of the present invention and not limitative thereof.
EXAMPLE 1
Experimental Animals - Efficacy
Seventy-seven Holstein cows are used in the experiments. Forty-two cows are assigned to groups of 14 animals each. Each group is injected with either 10.3 mg animal - 1 day - 1 BST subcutaneously, 175 mg or 350 mg BST animal - 1 14 days - 1 in a sustained-release preparation injected subcutaneously. Injections commence at 35 d postpartum for the entire lactation. The remaining 35 cows, serving as controls, receive placebo injections. Cows are fed total mixed rations formulated for National Research Council (1978) requirements for production. Ration ingredients are alfalfa haylage, dry ground corn, high moisture ear corn, roasted soybeans and a vitamin-mineral premix. One thousand two hundred milk samples are collected at two-week intervals from fall into spring. Milk samples are defatted and the skim milk centrifuged at 100,000 ×g for lh at 4° C. to resolve the milk serum fraction from the casein pellet. Daily milk yield is also recorded Injection of BST increases milk yield, and yield of major components in a dose-dependent, linear fashion. This increase is relatively instantaneous, and occurs through an increase in feed intake and improved efficiency of converting feed into milk. Lactation curves generally show improved persistency of production.
EXAMPLE 2
Compositions and Doses of BST
The exogenous animal somatotropins of the present invention are illustrated hereinbelow, but include chemically synthesized, naturally purified from pituitary glands and/or recombinantly-derived.
Recombinantly-derived animal somatotropins without the additional Asp-Gln substitutions or with other substitutions are used in accordance with the present invention, as well. Further, animal somatotropins with deletions in amino acid chain length, additions to amino acid chain length, replacement of amino acids, fragments with the active portion and the like all within the scope of the present invention. Numbering of amino acid residues herein relates to the Met-Asp-Gln analogues, but numbering is altered accordingly by one skilled in the art. ##STR1## wherein R 1 , R 1a , R 2 and R 2a of said recombinant animal somatotropins each independently represent amino acid residues selected from arginine, lysine, aspartic acid, glutamic acid, asparagine, glutamine, histidine, alanine, glycine, isoleucine, leucine, valine, phenylalanine, tryptophan, tyrosine, methionine, serine, threonine, proline or cystine; additionally R 1 , R 1a or, R 2 and R 2a in the above illustrated somatotropins, represents an amino acid residue other than cysteine.
Compositions
In practice, the compositions useful in the present invention are generally administered to the animals by injection in the form of biologically active parenteral compositions. Among the parenteral compositions useful for administration of the animal somatotropins of this invention are gels, pastes, microspheres, microcapsules, implants and the like. As such, there is considerable interest in providing dosage forms of biologically active substances which release the substance in a controlled manner and thus, reduce the frequency of administration.
The compositions useful for this type of administration are prepared by dissolving the animal somatotropin in dilute ammonium hydroxide and then adding a solution of an alkali metal benzoate, laurate, carbonate or the like thereto. A nonionic surfactant is thereafter admixed with the solution and the resulting mixture spray dried. The thus formed solids are then admixed with molten fat or wax or a mixture thereof and the resulting molten mixture sprayed through an air/liquid spray nozzle equipped with a heated jacket to maintain the incoming air and the molten phase at a temperature above the melting point. The microspheres are formed as the molten droplets cool. These are collected on a series of sieves in the desired size range of about 45 to 180 microns and retained for use. Microspheres which are not of the desired size range are recycled. Alternatively, the homogeneous mixture is fed onto a centrifugal disc and the microspheres thus formed collected as above, or the molten mixture are cooled and milled to the desired average particle size range.
The biologically active microspheres are then dispersed in a pharmaceutically and pharmacologically acceptable liquid vehicle for injection into the animal. The microsphere-liquid composition is generally administered by subcutaneous injection under the skin of the animal usually in the vicinity of the head, neck or ears.
The animal somatotropins of the present invention also are prepared as biocompatible implants which are injected under the skin of the animal using a conventional pellet implant gun. These compositions are prepared by admixing a powdered modified or derivatized somatotropin with a wax such as castor wax or with a mixture of a copoly (glycolide/lactide), magnesium hydroxide, and a condensate of ethylene oxide prepared with a hydrophobic base formed by condensation of propylene oxide with propylene glycol. The thus formed compositions are then introduced into a pelleting press and formed into cylindrical pellets about 1/8 inch in diameter. The thus formed pellets are administered with a conventional pellet implant gun.
Preparation of the recombinant animal somatotropins in a size range suitable for incorporation in microspheres by spray drying is accomplished by dissolving the recombinant animal somatotropin in dilute ammonium hydroxide solution and then adding desired salt solutions such as sodium benzoate. A nonionic surfactant such as a block copolymer of ethylene oxide and propylene oxide is added and allowed to dissolve with constant gentle mixing. The solution is then spray-dried. A Buchi mini spray dryer, model #190 maybe used for this purpose.
A homogeneous mixture of the thus prepared active ingredient and additives in the molten fat, wax or mixture thereof is prepared and the resulting mixture sprayed through an air/liquid spray nozzle equipped with a heated jacket to maintain the incoming air and the molten phase at a temperature above the melting point. The microspheres are formed as the molten droplets cool and are collected on a series of sieves in the desired size range of about 45 to 180 microns and retained for use. Microspheres which are not of the desired size range are collected for recycling. Alternatively, the homogeneous mixture are fed onto a centrifugal disc and the microspheres thus formed are collected as above, or the molten mixtures are cooled and milled to the desired average particle size range.
Waxes and fats which are suitable for use in the compositions of this invention in general have melting points higher than 40° C. *These waxes are defined as a low-melting organic mixture or compound of high molecular weight, solid at room temperature and generally similar in composition to fats and oils except that it contains no glycerides. Some are hydrocarbons; others are esters of fatty acids and alcohols. They are classed among the lipids. Waxes are thermoplastic, but since they are not high polymers, they are not considered in the family of plastics. Common properties are water repellency; smooth texture; nontoxicity; freedom from objectionable odor and color. They are combustible, and have good dielectric properties. Soluble in most organic solvents; insoluble in water. The major types are as follows:
I. Natural
1. Animal (beeswax, lanolin, shellac wax, Chinese insect wax).
2. Vegetable (carnauba, candelilla, bayberry, sugar cane)
3. Mineral
(a) Fossil or earth waxes (ozocerite, ceresin, montan)
(b) petroleum waxes (paraffin, microcrystal-line) (slack or scale wax)
II. Synethetic
1. Ethylenic polymers and polyol ether-esters ("Carbowax," sorbitol)
2. Chlorinated naphthalenes ("Halowax")
3. Hydrocarbon type via Ficher-Tropsch synthesis
The fat may be defined as a glyceryl ester of higher fatty acids such as stearic and palmitic. Such esters and their mixtures are solids at room temperatures and exhibit crystalline structure. Lard and tallow are examples. There is no chemical difference between a fat and an oil, the only distinction being that fats are solid at room temperature and oils are liquid. The term "fat" usually refers to triglycerides specifically, whereas "lipid" is all-inclusive.
The fat is preferably long chain C 10 -C 24 fatty acid, alcohol, ester, salt, ether or mixture thereof, with mono-, di-, or triglycerides composed predominantly of stearates, palmitates, laurates, linoleates, linolenates, oleates, and residues or mixtures thereof, having melting points greater than 50° C. being most preferred. Glycerol tristearate is a most preferred fat. Additionally, lipophilic salts of fatty acids such as magnesium stearate and the like are also suitable.
The microspheres useful in the invention are dispersed in a pharmaceutically and pharmacologically acceptable liquid to obtain a slow release composition for parenteral administration. The vehicle is aqueous buffered systems or oil systems. The oil is a vegetable or an animal oil. A preferred oil is a neutral triglyceride liquid fat. A neutral oil is one containing no residual acid. Vehicles suitable for use in the compositions of this invention include aqueous systems such as buffered salines; organic solvents such as glycols and alcohols; and water immiscible liquids such as oils, depending upon the solubility of the active ingredient being administered.
Implants are prepared by weighing a sufficient quantity of the ground homogeneous mixture of the desired animal somatotropin and the desired diluents. This mixture is then compressed on a carver press at from 1000 to 5000 psig in a 3/16" or 1/8" diameter cylindrical die or on a rotary tablet press using the required punch and die. The implants thus prepared are then coated with either biodegradable or nonbiodegradable coatings as provided herein.
Clean grade silicon elastomer (10 parts) is mixed with curing agent (one part) on a watch glass with a spatula. This is deaerated in a dessicator for 30 minutes. The implants are grasped by the ends with tweezers, rolled into the silicon polymer, placed on end on aluminum foil and cured at 40° C. for five hours. One or both of the ends are removed with a razor blade leaving the "shaft" of the cylinder coated.
Alternatively, implants are dip coated with 20% to 40% of a medical adhesive, sold under the trademark SILASTIC, by Dow Corning, which has been dispersed in hexane, and dried and cured at 40° C. to 50° C. overnight before removing the coating from one or both of the base ends.
Alternatively, the polymer or copolymer (one part) is dissolved in chloroform (three to eight parts). Each implant is grasped by the ends with tweezers, dipped into the polymer solution, and then the chloroform evaporated at room temperature. Each implant is coated twice. After the coating dried overnight at room temperature, the polymer ends are removed with a razor blade, leaving the long cylindrical "shaft" coated.
______________________________________Implant formulation______________________________________ % Magnesium % ethyl % Castor% somatotropin stearate cellulose Wax______________________________________50 -- 5.0 4540 -- 5.0 5020 -- 5.0 7550 0.5 3.5 4620 0.5 3.5 76______________________________________ % glyceryl*somatotropin % cholesterol % surfactant tristearate______________________________________30 68 2 --15 41.5 2 41.5______________________________________ % stearic% somatotropin acid______________________________________50 5020 80______________________________________
Also, the recombinant animal somatotropins is blended with surfactants, buffer salts, and/or preservatives in an aqueous solution. This solution is then spray-dried in a Buchi Model 190 spray dryer giving a small particle size powder. This powder is then melt-blended with a fat or wax and molded into cylindrical implants. The implants prepared are then coated with either a biodegradable or a non-degradable polymer using the various procedures A or B.
______________________________________
______________________________________Implant Formulations % glyceryl % sodium %% somototropin tristearate benzoate surfactant______________________________________28 69.9 2.0 0.1515 82.9 2.0 0.1550 48.5 1.5 0______________________________________
Dose
In Table I, a 10.3 mg dose of a daily injectable bovine somatotropin plus two sustained release doses of bovine somatotropin are reviewed for milk yield and composition. The sustained release doses of 175 mg or 350 mg are injected every fourteen days and treatments beginning about 14 weeks after calving.
TABLE I______________________________________Parameter 0.0 10.3 175 350______________________________________Milk, kg/day 21.60 24.75 24.78 24.743.5% fat- 23.06 26.46 26.76 25.80corrected milk, kgMilk fat, % 4.12 4.21 3.98 4.02Milk protein, % 3.33 3.29 3.18 3.21______________________________________
EXAMPLE 3
BST also increases milk yield in a dose-dependent fashion when administered beginning approximately 4 weeks after calving. The following table reports average daily milk yield for cows administered 10.3 or 20.6 mg BST as a daily injection from 6 University dose-titration experiments. BST herein refers to rBST.
TABLE II______________________________________Parameter 0.0 10.3 20.6______________________________________Milk, lbs/day 60.32 68.75 72.873.5% fat- 60.11 68.13 72.16corrected milk, lbs______________________________________
EXAMPLE 4
Experimental Animals - Resumption of BST
In another experiment, the effect of cessation and resumption of BST injections on concentration of plasmin in milk and milk yield is determined. Four cows at >310 days of lactation with a history of daily BST injection are assessed for daily milk yield and milk plasmin activity. These measurements are taken 3 days prior to cessation of BST injection (end of safety-efficacy trial), for four days after cessation of BST injections and for 3 days following resumption of BST injections. In this study, daily injections contain 10.3 mg of BST in saline and are administered daily between 0930 and 1000 h in the shoulder region.
EXAMPLE 5
Plasmin and Plasminogen Analysis
Plasmin and plasminogen concentrations in milk serum or casein fractions are determined by the method of Koryoka-Dahl et al. with a slight modification. As plasmin has proteolytic sepcificity similar to trypsin, it will cleave amide bonds on the carboxy-terminal side of lysine and arginine residues. Briefly, this method involves assaying for plasmin activity by measuring the rate of hydrolysis of the chromogenic substrate (H-D-valyl-L-leucyl- L-lysine-p-nitroanilide dihydrochloride, S2251). Three amino acids are required to minimize interference from other serine proteases. Formation of p-nitroanilide resulting from substrate cleavage by plasmin is measured spectrophotometrically at 405 nm. A standard curve is prepared to convert plasmin activity to plasmin concentration by plotting change in absorbance versus concentration of plasmin over the range of 0 to 3 mg/l. This conversation is made to overcome the difficulty in comparing plasmin activity units, which are not uniform in the literature. Plasminogen is the inactive form of plasmin. In this assay a plasminogen-activating substance, urokinase, is added to quantitatively convert all of the plasminogen to plasmin. When plasmin activity is again assayed, any increase in activity can be said to be derived from plasminogen. Thus the ratio of plasminogen to plasmin is a useful index in determining the degree of activation of the system.
Least square analysis of variance is performed to examine the effect of exogenous somatotropin administration on milk plasmin and plasminogen concentrations and milk yield. The mathematical model includes lactation number, stage of lactation and treatment as fixed classification effects, the interaction between stage of lactation and treatment, log somatic cell counts (SCC) and milk yield as covariates plus a random residual term. The effect of milk yield is removed from the model when testing the significance of the other factors on milk yield. For data analysis there are five subclasses for lactation number (1, 2, 3, 4, 5). Treatment consisted of two subclasses; control and treated. All BST treated groups are grouped into one category defined as treated. This is possible as there are no statistically significant differences in response among BST treatments. Stage of lactation is classified into 10 subclasses with subclasses 1 to 9 consisting of cows in their first to ninth month of lactation, respectively. The last subclass contains samples from cows with more than 9 months in lactation.
EXAMPLE 6
Plasmin Levels in Milk Production
In FIG. 1, the relationship between milk plasmin and milk yield is presented for control cows and for those treated with exogenous BST (all levels). Increasing plasmin concentration in milk as lactation progresses has been reported previously by Politis et al. (13) and others (10). The present results show that plasmin levels remain depressed throughout lactation in cows injected with BST (FIG. 1). Similarly, the total plasmin produced (milk volume×plasmin concentration) is maintained at low levels in milk from cows injected with BST. In contrast, cows injected with placebo show a gradual increase in the total production and concentration of milk plasmin as lactation advances. The milk yield data have been superimposed to illustrate the inverse relationship between milk plasmin concentration and milk yield. The BST-injected cows have persistently higher milk yields and low milk plasmin concentration and total secretion.
Milk plasmin is influenced by the availability of precursor plasminogen and the presence of plasminogen activators and plasminogen activator inhibitors. Plasminogen is not limiting in animals injected with BST as milk plasminogen levels are not significantly different between BST-injected and control cows (FIG. 2). This continues into the dry period where at 3 days after the last milking plasminogen levels were 1.49±.08 and 1.39±.08 mg L- 1 in secretions from BST-injected and control animals, respectively. The process regulating milk plasminogen is apparently insensitive to BST. The ratio of plasminogen to plasmin is a useful index of plasminogen activation. This measurement is independent of milk volume. In milk from BST-injected cows, this ratio remains remarkably constant throughout lactation. However, 3 days after drying off, this ratio falls dramatically, indicating massive activation of plasminogen and production of plasmin (FIG. 2). In milk from control cows, the plasminogen/plasmin ratio falls from 6.3 in the first month to 3.6 at >9 months of lactation. The activation process is thus gradual throughout the lactation period.
In an effort to gain insight into the time course and reversibility of BST effects on decreased milk plasmin and increased milk yield, BST injections are abruptly ceased as cows conclude the safety-efficacy trial for 4 days then resume injections (FIG. 3). Plasmin concentrations in the milk rises during the first day and reaches the peak at the second day, while milk yield is initially unaffected, then decreases. When BST injections are resumed, plasmin concentrations decrease while milk yield continue to decrease, then increase in a lag fashion (FIG. 3). These data show that alterations in BST lead to prompt changes in milk plasmin levels prior to changes in milk yield.
EXAMPLE 7
Two cows were selected to represent extremes in milk plasmin concentrations; one late lactation, high somatic cells (#628), the other early lactation, low somatic cells (#659). Milk was collected, assayed for plasmin, plasminogen cheese total solids and cheese yield determined. Milk plasmin concentration was three fold higher in cow #628 (Table II). Cheese total solids were higher for cow #659, while milk protein levels appeared lower. Increased cheese total solids would indicate higher quality curds for cheese production, and should indicate greater cheese yield. While cheese yield was not different in this very limited experiment total protein was lower in milk containing lower plasmin. Calculating cheese yield on an equal milk protein basis would result in increased cheese yield from the cow having lower milk plasmin concentration.
TABLE III______________________________________Properties of Milk from Cows ofDiffering Milk Plasmin ConcentrationParameter #659.sup.1 #628.sup.2______________________________________Plasmin, mg/l milk .085 .253Cheese total solids, % 55.8 50.6g total solids/100 g milk 6.3 5.9Milk fat, % 3.19 3.20Milk protein, % 3.03 3.42Cheese yield, % 11.22 11.56Cheese yield/unit milk protein 3.70 3.38______________________________________ .sup.1 Early lactation, low somatic cells .sup.2 Late lactation, high somatic cells
References
1. Akers, R. M. 1985. Lactogenic hormones: Binding sites, mammary growth, secretory celldifferentiation and milk biosynthesis in ruminants. J. Dairy Sci. 68:501.
2. Baer, R. J., K. M. Treszen, D. J. Schingoethe, D. P. Casper, W. A. Eisenbeisz, R. D. Shaver and R. M. Cleale. 1989. Composition and Flavor of Milk Produced by Cows Injected with Recombinant Bovine Somatotropin. J. Dairy Science. 72:in press.
3. Bauman, D. E., P. J. Eppard, M. J. DeGeeter and G. M. Lanza. 1985. Responses of high-producing dairy cows to long term treatment with pituitary somatotropin and recombinant somatotropin. J. Dairy Sci. 68:1352.
4. Collier, R. J., R. Li, H. D. Johnson, B. A. Becker, F. C. Buonomo and K. J. Spencer. 1988. Effect of sometribove on plasma insulin-like growth factor I and II in cattle exposed to heat and cold stress. J. Dairy Sci. 71 (Suppl. 1):228.
5. Cotes, P. M., J. A. Crichton, S. J. Folley and F. G. Young. 1949. Galactopioetic activity of purified anterior pituitary growth hormone. Nature 164:992.
6. DeJong, L. 1976. Protein breakdown in soft cheese and its relation to consistency. Neth. Milk Dairy J. 30:242.
7. Disenhaus, C., L. Belair and J. Djane. 1988. Caracterisation et evolution physiologique des recepteurs pour les insulin-like growth factor I and II dans la glande mammaire de brebis. Reprod. Nutr. Develop. 28:241.
8. Donnelly, W. J. and J. Gerard Barry. 1983. Casein compositional studies. III. Changes in Irish milk for manufacturing and role of milk protease. J. Dairy Res. 50:433-441.
9. Elvinger, F., H. H. Head, C. J. Wilcox, R. P. Natzke, R. G. Eggert. 1988. Effects of administration of bovine somatotropin on milk yield and composition. J. Dairy Sci. 71:1515-1525.
10. Eppard, P. J., D. E. Bauman, J. Bitman, D. L. Wood, R. M. Akers, W. A. House. 1985. Effect of dose bovine growth hormone on milk composition: a Lactalbumin, fatty acids and mineral elements J. Dairy Sci. 68:3047-3054.
11. Gertler, A., N. Cohen and A. Macz. 1983. Human growth hormone but not ovine or bovine growth hormones exhibit galactopoietic prolactin-like activity in organ culture from bovine lactating mammary gland. Mol. Cell. Endocr. 33:162.
12. Hart, I. C., J. A. Bines, S. V. Morant and J. L. Ridley. 1978. Endocrine control of energy metabolism in the cow: Comparison of the levels of hormones (prolactin, growth hormone, insulin and thyroxine) and metabolites in the plasma of high- and low-yielding cattle at various stages of lactation. J. Endocr. 77:333.
13. Hart, I. C., J. A. Bines and S. V. Morant. 1980. The secretion and metabolic clearance rates of growth hormone, insulin and prolactin in high- and low-yielding cattle at four stages of lactation. Life Sciences 27:1839.
14. Holst, B. D., W. L. Hurley and D. R. Nelson. 1987. Involution of the bovine mammary gland. Histology and ultrastructural changes. J. Dairy Sci. 70:935.
15. Koryoka-Dahl, M., B. Ribadeau-Dumas, N. Chene and J. Marta. 1983. Plasmin activity in milk. J. Dairy Sci. 66:704.
16. Larsson, L. -T., L. Skriver, L. S. Nielsen, J. Grondahl-Hansen, P. Kristensen and K. Dano. 1984. Distribution of urokinase-type plasminogen activator immunoreactivity in the mouse. J. Cell. Biol. 98:894.
17. Ossowski, L., D. Biegel and E. Reich. 1979. Mammary plasminogen activator: Correlation with involution, hormonal modulation and comparison between normal and neoplastic tissue. Cell 16:929.
18. Pearse, M. J., P. M. Linklater, R. J. Hall, A. G. MacKinlay. 1986. Extensive degredation of casein by plasmin does not impede subsequent curd formation and syneresis. J. Dairy Res. 53:477-480.
19. Politis, I., E. Lachance, E. Block and J. D. Turner. 1988. Plasmin/plasminogen in bovine milk: A relationship with involution. J. Dairy Sci. 72:900.
20. Richard, A. L., S. N. McCutcheon and D. E. Bauman. 1985. Responses of dairy cows to exogenous bovine growth hormone administered during early lactation. J. Dairy Sci. 68:2385. 21.
21. Richardson, B. C. 1983. Variation of the concentration of plasmin and plasminogen in bovine milk with lactation. NZ J. Dairy Sci. and Tech. 18:247-252.
22. Soderholm, C. G., D. E. Otterby, J. G. Linn, F. R. Ehle, J. E. Wheaton, W. P. Hansen and R. J. Annexstad. 1988. Effects of recombinant bovine somatotropin on milk production, body composition and physiological parameters. J. Dairy Sci. 71:355-365.
23. Turner, J. D., P. Rotwein, J. Novakofski and P. J. Bechtel. 1988. Induction of messenger RNA enceding insulin-like growth factors I and II during growth hormone stimulated skeletal muscle hypertrophy. Am. J. Physiol. 255:E 513.
24. Walstra, P. and R. Jenness. Dairy Chemistry and Physics. 1989 by John Weley and Sons, N.Y., pp. 132.
|
The present invention relates to methods for improving cheese production by utilizing plasmin-regulating agents to maintain milk plasmin concentration in milk used to make cheese at that found at early lactation or at less than 0.2 mg/l milk.
| 2
|
CROSS REFERENCES TO RELATED APPLICATIONS
The present application is a continuation of co-pending U.S. application Ser. No. 10/720,851 filed on Nov. 24, 2003, which is a continuation of co-pending U.S. application Ser. No. 10/154,237 filed on May 23, 2002, which claims priority to Japanese Application No. 2001-153326 filed on May 23, 2001, all of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a manufacturing method for a semiconductor apparatus, and in detail, the present invention particularly relates to such a manufacturing method for a semiconductor apparatus, wherein a micro wiring pattern is formed.
2. Description of the Related Art
In recent years, the miniaturization of a wiring pattern has been quickly advanced in order to improve the degree of integration and the property of an LSI. The techniques for miniaturizing a gate length in order to improve the property of a transistor and for opening a contact hole smaller than that of a conventional contact hole in order to improve the degree of integration have been strongly requested. It is well known that a limit resolution (R) in an optical lithography process to determine the minimum size of the LSI is represented by the following equation (1):
R=k×λ/NA (1)
In this case, A is a wave-length of a light source, NA is the numerical aperture in a projection lens, and k is a constant having a value of about 0.5.
That is, in order to attain the lithography process having a resolution higher than that of the conventional one, it is desirable to select a light source having a shorter wave-length. Because of this reason, a photolithography machine, which uses a krypton fluorine (KrF) excimer laser having a wave-length of 248 nm as a light source, is used in a field of manufacturing an high technology device. However, NA of a current exposing apparatus is 0.68 at its maximum. Thus, even the latest KrF excimer laser photolithography machine has only a resolution of about 0.18 μm. However, the resolution derived from the equation (1) is applied to a banded pattern typically referred to as a line and space. Then, the resolution of the contact hole pattern has a limit of about 0.22 μm.
On the other hand, a technique for opening a micro contact hole, having a diameter of 0.15 μm is requested in a device of 0.13 μm generation. This is the size that can not be easily attained even by using an argon fluorine (ArF) excimer laser photolithography machine, which is expected as a next generation photolithography machine using a light source having a wave length of 193 nm.
As one method of solving this problem, a technique for carrying out an etching process so as to give a taper to a side wall of a hole 112 formed on a film 111 to be processed by using a resist mask 121 is known and thereby finishing it to a desired hole diameter at a bottom 112 b of the hole 112 , as shown in FIG. 3 .
However, as shown in FIG. 4 , in the above-mentioned conventional method, even if a desired hole diameter (a hole diameter on design) Db is obtained at the bottom 112 b of the hole 112 , a diameter Dt at an upper end (aperture) 112 t of the hole 112 becomes greater than the desired size (a size on the design). This results in a problem that a sufficient matching margin can not be obtained at a later lithography process. For example, this has a problem that a distance d from a wiring 13 I placed adjacently to the hole 112 is made narrower.
The present invention is a manufacturing method for a semiconductor apparatus proposed in order to solve the above-mentioned problems.
SUMMARY OF THE INVENTION
The manufacturing method of a semiconductor apparatus of the present invention includes the steps of: forming a mask material film made of organic insulation film on a film to be processed; forming a tapered opening pattern or aperture pattern, in which a bottom is narrower than an open side on the mask material film; and etching the film to be processed using the mask material film as a mask.
In accordance with the manufacturing method of the semiconductor apparatus, after the mask material film is formed on the film to be processed, the tapered aperture pattern that is narrower at the bottom side than at the aperture side is formed on the film to be processed, and thereby it is possible to able to form the bottom of the aperture pattern at the desired micro dimension exceeding the limit of the lithography technology. The film to be processed is then etched by applying thus-processed mask material film as a mask, thereby, the film to be processed can be vertically etched to the micro dimension exceeding the limit of the lithography technology.
As mentioned above, according to the manufacturing method of the semiconductor apparatus of the present invention, after the mask material film is formed on the film to be processed, the tapered aperture pattern in which the bottom is narrower than the aperture side is formed on this mask material film. Thus, the bottom of the aperture pattern can be formed at the desirable micro dimension exceeding the limit of the lithography technique. The thus-processed mask material film is used as the mask, and the film to be processed is etched. Hence, the film to be processed can be vertically etched to the micro dimension exceeding the limit of the lithography technique. Therefore, since the film to be processed can be processed under the excellently controlling performance with regard to the size, the matching margin is never decreased differently from the conventional direct taper etching method.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A to 1E are sectional views of manufacturing steps showing an embodiment according to a manufacturing method for a semiconductor apparatus according to the present invention;
FIG. 2 is a sectional view of a schematic configuration for describing a case in which a film to be processed has a step;
FIG. 3 is a sectional view of a schematic configuration for describing a conventional technique; and
FIG. 4 is a sectional view of a schematic configuration for describing a problem.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
One embodiment of a manufacturing method for a semiconductor apparatus according to the present invention will be described below with reference to a sectional view of manufacturing steps of FIGS. 1A to 1E .
As shown in FIG. 1A , a film 12 to be processed made of, for example, silicon oxide film is formed on a substrate 11 . Next, a first mask material film (mask material film) 13 made of an organic insulation film is formed on the film 12 to be processed. A dielectric film having low dielectric constant is used as this organic insulation film. The material referred to as the low dielectric film is the material having a lower dielectric constant than that of SiO 2 , and is originally developed in order to reduce an inter-wiring capacitance of an LSI. For example, FLARE made by Honeywell Co., Ltd., SILK made by Dow Chemical Ltd. and the like are known as such material. Those organic system materials have a high heatproof temperature of 350° C. Thus, they can be positively used even as a hard mask material in a process for manufacturing a semiconductor. Hence, they can be used to form a micro hole pattern.
Moreover, a second mask material film 14 , which serves as an etching mask to this first mask material film 13 and is made of, for example, an oxide film, is formed on the first mask material film 13 . Moreover, a resist film 15 is formed on the second mask material film 14 . The mask material film 14 is made of, for example, a silicon oxide film. With regard to this silicon oxide film, if it is the silicon oxide film serving as the etching mask to the first mask material film 13 , a silicon oxide film formed by a chemical vapor deposition, a silicon oxide film of a coating type such as SOG film and the like can be used, and accordingly the film forming method is not specified. As mentioned above, the low dielectric film has the high heatproof property although it is the organic film. Thus, it can be sufficiently endured in the process for forming the mask material film 14 made of the oxide film by using the chemical vapor deposition.
Then, as shown in FIG. 1B , the usual lithography process is carried out under this condition, and an aperture pattern 16 is formed on the resist film 15 . As mentioned above, the formable pattern size at this time is limited by the limit resolution of the lithography technique. If the defect of the lithography process causes a line width and a positional deviation to depart from a range of a specification, it is possible to apply a reproducing process through a usual resist ashing. Even if a resist reproducing process is carried out, the second mask material film 14 is formed on the low dielectric film. Thus, the low dielectric film is protected by this second mask material film 14 . Hence, the low dielectric film is never ashed in carrying out the reproducing process.
When the lithography process is completed without any trouble, the resist film 15 on which the aperture pattern 16 is formed is used as the mask, and the second mask material film 14 is etched to thereby form an aperture pattern 17 .
Next, as shown in FIG. 1C , the resist film 15 is used as the etching mask, and the first mask material film 13 made of the low dielectric film is etched. This etching is done such that in an open pattern 18 formed on the first mask material film 13 , a bottom side is narrower than an aperture side, and its side-wall becomes taper-shaped. Actually, the taper etching can be carried out by setting a temperature of the substrate to a low temperature (for example, −50° C. to 0° C.).
Usually, the deposition reaction and the etching reaction are mixed in an etching chamber. The deposition reaction is easily carried out by lowering the temperature of the substrate. Thus, it is possible to process the taper shape. Ammonia (NH 3 ), mixed gas of hydrogen (H x ) and nitrogen (N 2 ), oxygen (O 2 ) and the like are used as the etching gas for the low dielectric film. In addition, a method of etching the organic insulation film to the taper shape in an excellently controlling manner is disclosed in Japanese Patent Publication No.H7-27886. According to this method, an aperture having a desirable taper angle can be formed, for example, by changing a content of phloro-carbon gas in the etching gas.
In the above-mentioned etching process, when the first mask material film. 13 is etched, the resist film 15 is also etched and removed. Then, when the resist film 15 is perfectly removed, the second mask material film 14 serves as the etching mask, and the etching is further advanced.
Next, as shown in FIG. 1D , the first mask material film 13 is used as the etching mask, and the usual etching for the vertical processing is carried out. Consequently, an aperture pattern 19 , which is further miniaturized over the size formed by the lithography process, is formed on the film 12 to be processed. In the etching at this time, the second mask material film 14 [refer to FIG. 1C ] formed on the upper layer is desired to be formed in advance at a film thickness to be etched simultaneously with the film 12 to be processed.
After that, as shown in FIG. 1E , the first mask material film 13 made of the low dielectric film that is already unnecessary [refer to FIG. 1D ] is removed by carrying out the ashing process similar to the resist removal. As a result, the aperture pattern 19 less than the resolution limit of the lithography technique can be formed on the film 12 to be processed.
As compared with the method of reducing the hole diameter (or the slit width) at the bottom by performing the taper etching on the film itself to be processed that is typically used, the method of the present invention can carry out the vertical processing of the film 12 to be processed. Thus, for example, when the aperture pattern 19 is the hole pattern, its control of the hole diameter thereof becomes easy. The problem of the lack of the matching margin as described in the problem is never induced. Also, as shown in FIG. 2 , when the film 12 to be processed has a step S, the first mask material film 13 can function as a flattened layer. Thus, this method has the merit that the lithography step is advantageous.
When the above-mentioned manufacturing method is used to form the contact hole pattern, as the example, the lithography process is carried out to thereby form the aperture pattern 16 composed of the contact hole pattern having the diameter of 0.22 μm on the resist film 15 . Then, for the first mask material film 13 made of the low dielectiic film, the taper etching is used to finally obtain the aperture pattern 18 having the bottom diameter of 0.15 μm. When this first mask material film 13 is used as the etching mask and the film 12 to be processed is vertically etched, the aperture pattern 19 having a diameter of 0.15 μm is obtained.
A KrF excimer laser exposing apparatus (an exposure wave length=248 nm) in which NA=0.68 and σ=0.75 is used as the optical condition to expose the resist film 15 . As the resist film, for example, R11JE made by JSR Corporation is used, and its film thickness is defined as 0.4 μm. Also, a parallel flat plate type of a plasma etching apparatus is used to etch the film 12 to be processed, and ammonium (NH 3 ) is used for the etching gas, and the temperature of the substrate is set to 0°C.
As mentioned above, the case in which the optical lithography is carried out to thereby form the micro contact hole pattern is exemplified. However, the present invention can be also applied to an electron beam lithography, an ion beam lithography and an X-ray lithography. Moreover, it can be applied not only to the contact hole but also the formation of the micro slit pattern.
|
When a hole pattern is formed on a film to be processed, a matching deviation margin at a lithography step is reserved by making a diameter of a bottom of a hole substantially equal to a diameter of an aperture of the hole. The method for manufacturing the semiconductor apparatus includes the steps of: forming a (first) mask material film on a film to be processed; forming a tapered open pattern on the (first) mask material film; and etching the film to be processed by using the (first) mask material film as a mask.
| 8
|
The invention relates to an exhaust-gas turbocharger including a compressor and a turbine disposed in a housing with multiple exhaust gas supply passage of which some can be closed by adjustable shut-off flaps.
BACKGROUND OF THE INVENTION
The publication US 18 16 787 describes a multi-cylinder internal combustion engine, which is equipped with an exhaust-gas turbocharger, which comprises a compressor in the inlet duct of the internal combustion engine and an exhaust-gas turbine in the exhaust duct. The exhaust gas turbine is driven by the pressurized exhaust gases from the internal combustion engine, the rotation of the turbine being transmitted, by way of a common shaft, to the compressor, which draws in the combustion air and compresses it to an increased charge-air pressure, under which the combustion air is delivered to the cylinder inlets of the internal combustion engine. In order to be able to adjust the turbocharger output, the exhaust gas is delivered to the turbine rotor by way of three flow ducts, in each of which a valve is arranged, whose position can be adjusted by way of a common control rod as a function of the charge-air pressure, so as to compensate for pressure fluctuations. No provision is made here for any independent adjustment of the opening cross section of each flow duct, the valves in the flow ducts instead being opened or closed in a set order through the actuation by means of the control rod. In the exhaust-gas turbocharger according to US 18 16 787 no further adjustment facilities are provided other than the atmospheric pressure compensation.
Another problem is that the shut-off valves in the flow ducts are designed as pivoted flaps, the pivot axes of which extend approximately centrally through the respective flow duct, so that even in its open position the shut-off valve forms an obstacle to the flow of the exhaust gas.
Another exhaust-gas turbocharger is disclosed by the generic publication DE-AS 1 253 510. The exhaust-gas turbine of this exhaust-gas turbocharger comprises two parallel exhaust manifolds, which each open into a spiral section, which radially surrounds part of the turbine rotor. A pivotal shut-off flap, which can be pivoted between a shut-off position closing the flow inlet of the exhaust manifold and an open position exposing it is arranged in the area of the flow inlet of one of the two exhaust manifolds. In the open position, the shut-off flap is accommodated in a correspondingly shaped recess in the inside wall of the turbocharger housing, thereby avoiding any adverse effect on the flow of exhaust gas entering. No shut-off flap is provided in the area of the second exhaust manifold; the second exhaust manifold remains permanently opened.
For adjustment of the turbocharger output, the shutoff flap can be adjusted between its open position and its shut-off position, so that given an identical cross section in both exhaust manifolds the total unrestricted inlet cross section available to the exhaust gas inlet flow can be approximately doubled.
It is the main object of the invention to provide an exhaust-gas turbocharger that is variably adjustable.
SUMMARY OF THE INVENTION
In an exhaust-gas turbocharger having a compressor and an exhaust-gas turbine, which drives the compressor and comprises a multi-part exhaust gas supply duct manifold and a turbine rotor, to which pressurized exhaust gas can be delivered by way of the exhaust gas supply duct, the exhaust gas supply duct manifold includes at least three flow passages, which, except for one, are provided with shut-off flaps, which are adjustable independently of one another.
This arrangement allows a maximum number of adjustments for the admission of exhaust gas to the turbine rotor to be achieved using a minimum number of shut-off flaps. The independent adjustment of the shut-off flaps enables the existing flow ducts to be interconnected in any combination, in order to provide a greater or lesser overall cross section for the delivery of exhaust gas, at least the one flow duct having no flap being permanently open, so that a minimum of exhaust gas is delivered to the exhaust gas turbine in any operating condition of the internal combustion engine.
A further advantage lies in the simplicity of the design. In contrast to exhaust-gas turbines having a variable turbine geometry achieved, for example, by means of a guide baffle with adjustable guide vanes, so that a multiplicity of moveable components have to be adjusted, which increase the susceptibility to malfunction, in the simplest design of the exhaust-gas turbocharger according to the invention, having a total of three flow ducts, only two shutoff flaps are needed, which are arranged in two of the three flow ducts for adjustment of the unrestricted inlet cross section. This reduces the number of moving parts considerably. At the same time, however, the various possible combinations of opened and closed shut-off flaps, available even in the simplest version with three flow ducts, mean that up to four different-sized overall inlet cross sections can be set for the delivery of exhaust gas, which is usually sufficient for all operating conditions both during engine power operation and during engine braking of the vehicle.
Through an adept choice of inlet cross sections for the flow ducts—such as two flow ducts of equal cross section, one flow duct with a cross section twice as large, for example—four overall inlet cross sections, divided up in the size ratio 1:2:3:4, can be exposed for the various operating conditions of the internal combustion engine.
In an advantageous embodiment, at least two shut-off flaps are arranged in the two outer flow ducts, and supported so that they are capable of pivoting onto the inside wall of the turbine housing. In this design at least one flow duct, situated in the middle between the two outer ducts, is designed without a flap, the middle flow duct and the two outer flow ducts in each case sharing a common wall in the event of there being a total of just three flow ducts.
The shut-off flaps are advantageously designed to conform to the contour of the inside wall of the turbine housing and in the open position fit precisely against the inside wall, thereby presenting the least possible flow resistance to exhaust gas flowing in. The outside of the shut-off flap remote from the inside wall of the turbine housing and facing the flow duct may here have a flow-enhancing contour in order to further minimize the flow resistance and to obtain any desired flow effects, such as an acceleration of the flow through tapering of the unrestricted inlet cross section.
It may also be appropriate, however, to incorporate a recess, designed to conform to the shut-off flap, into the inside wall, in which recess the shut-off flap can be received in the open position. In this design the shut-off flap in the open position can be fully accommodated in the recess, thereby providing for a smooth inside wall surface.
In order to improve the flow ratios over the turbine rotor a fixed guide baffle may be provided in a duct upstream of the turbine rotor, the duct being connected to, or being part of, the exhaust manifold. In an alternative version, the guide baffle may also be variably adjustable, being axially insertable into the guide channel, for example, or equipped with adjustable guide vanes. A variable turbine geometry is thereby achieved, which permits a multiplicity of possible adjustments of the unrestricted inlet cross section.
The exhaust manifold—with or without guide baffle—is advantageously divided into a plurality of angular sections, which are hermetically separated from one another, precisely one angular section in the guide channel being assigned to each flow duct. The ratio of the angular sections advantageously corresponds to the ratio of the flow duct cross sections, so that a double angular section is also assigned to the flow duct having twice the cross section.
The invention will become more readily apparent from the following description thereof on the basis of the accompanying drawings:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a longitudinal section through an exhaust-gas turbocharger,
FIG. 2 shows an exhaust-gas turbine of an exhaust-gas turbocharger in a sectional view taken along the line II—II in FIG. 1,
FIG. 3 shows an exhaust-gas turbine comparable to FIG. 2, but with a different division of the areas of the inlet cross sections in the exhaust manifold of the turbine.
DESCRIPTION OF PREFERRED EMBODIMENTS
In the figures, identical components are provided with identical reference numbers.
The exhaust-gas turbocharger for an internal combustion engine represented in FIG. 1 comprises an exhaust-gas turbine 1 having a turbine rotor 3 , which is rotatably mounted in a turbine housing 2 , and whose rotation is transmitted, by way of a shaft 4 , to a compressor impeller of a compressor 22 for the compression of intake air. The exhaust-gas turbine 1 is suitably designed as an axial-flow impulse action turbine.
A fixed, immovable guide baffle 5 , which serves to optimize the flow ratios of the exhaust gas striking the turbine rotor, is arranged in an exhaust manifold 6 positioned axially upstream of the turbine rotor 3 , through which manifold the exhaust gas from the internal combustion engine is to be delivered axially to the turbine rotor and which is connected to a collecting chamber 13 in the turbine housing.
According to FIG. 2 the exhaust manifold 6 , positioned axially upstream of the turbine rotor 3 , is divided by means of wall plates 10 , 11 , 12 in the turbine housing 2 into a total of three flow ducts 7 , 8 , 9 . The exhaust manifold 6 is of approximately annular construction, a first flow duct 7 of the exhaust manifold 6 covering an angle range of approximately 180°, which is defined by the two wall plates 10 and 12 . A second, middle flow duct 8 , which is separated from the two outer flow ducts 7 and 9 by the wall plates 10 and 11 , extends over an angular section of approximately 90° of the exhaust manifold 6 in front of the turbine rotor. The third flow duct 9 , which, like the first flow duct 7 , is designed as an outer flow duct, is bounded by the wall plates 11 and 12 and likewise extends over an angular section of approximately 90° of the exhaust manifold. Each flow duct 7 to 9 shares one common wall plate with each of the other two flow ducts.
The collecting chamber 13 is arranged upstream of the exhaust manifold 6 . The collecting chamber 13 is likewise an integral part of the exhaust-gas turbine 1 ; the exhaust gases from the exhaust of the internal combustion engine are fed into this chamber. The collecting chamber 13 is connected to inlet cross sections 7 a , 8 a and 9 a of the flow ducts 7 , 8 and 9 , the inlet cross sections 7 a , 8 a , and 9 a lying in a common admission flow plane 20 , which separates the collecting chamber 13 from the exhaust manifold 6 . Two shut-off flaps 16 and 17 , by means of which the unrestricted inlet cross sections 7 a and 9 a of the two outer flow ducts 7 and 9 can be closed or opened, are pivotally mounted by way of articulations 18 and 19 on the inside walls 14 and 15 of the collecting chamber 13 . The inlet cross sections 8 a and 9 a of the middle flow duct 8 and of the second outer flow duct 9 are of approximately equal size and each occupy approximately one quarter of the overall flow cross section in the admission flow cross-section 20 . The inlet cross section 7 a of the first outer flow duct 7 occupies approximately half the overall inlet cross section and is therefore approximately twice as large as each of the other two inlet cross sections 8 a and 9 a.
The wall plates 10 , 11 and 12 extend essentially parallel to one another, the wall plates 10 and 11 between the middle flow duct 8 and each of the outer flow ducts 7 and 9 being situated at approximately the same height and the further wall plate 12 being arranged on that side of the turbine rotor 3 situated 180° opposite, between the two outer flow ducts 7 and 9 .
The shut-off flaps 16 and 17 can be actuated independently of one another and can each be adjusted between a shut-off position, closing the unrestricted inlet cross section 7 a or 9 a , and an open position, in which the respective inlet cross section is exposed. In the representation shown in the figure both shut-off flaps 16 and 17 are in their shut-off position, so that only the middle inlet cross section 8 a of the middle flow duct 8 is open and all exhaust gas is delivered to the turbine rotor 3 in the direction of the arrow 21 through the middle flow duct 8 . In the open position of the shut-off flap 17 of the second, outer flow duct 9 , the inlet cross section 9 a is also exposed in addition, so that the total unrestricted inlet cross section available for admission of the exhaust gas comprises the individual cross sections 8 a of the middle flow duct and 9 a of the second, outer flow duct, provided that the shut-off flap 16 of the first flow duct 7 remains in its shut-off position. If, on the other hand, the shutoff flap 16 of the first flow duct 7 is in the open position and the second shut-off flap 17 of the opposite outer flow duct 9 is in the shut-off position, the total unrestricted inlet cross section available comprises the individual cross sections 7 a and 8 a of the first, outer flow duct 7 and the middle flow duct 8 . If both shut-off flaps 16 and 17 are in their open position, a maximum inlet cross section is provided, which comprises the individual cross sections 7 a , 8 a , and 9 a of all three flow ducts 7 to 9 .
The wall plates 10 , 11 and 12 between the flow ducts 7 , 8 and 9 divide the exhaust manifold into different angular sections, hermetically separated from one another, in such a way that the ratio of the respective angular sections corresponds to the ratio of the unrestricted inlet cross sections 7 a , 8 a and 9 a of the relevant flow duct.
The shut-off flaps 16 and 17 are suitably designed to conform to the contour of the inside wall 14 and 15 of the collecting chamber 13 , so that, in their open positions, the shut-off flaps fit precisely against the inside wall 14 and 15 . If necessary, only that wall side of each shut-off valve 16 and 17 facing the inside wall is designed to conform to the contour of the inside wall, whereas the outside may assume a different form and may, in particular, be optimized with regard to the fluid mechanics. In the shutoff position the unexposed face of each shut-off flap 16 and 17 bears against the wall plate 10 and 11 respectively between the adjacent flow ducts 7 and 8 or 8 and 9 .
The design according to FIG. 3 differs from that according to FIG. 2 in the ratio of the inlet cross sections 7 a , 8 a and 9 a of the flow ducts 7 , 8 and 9 to one another. The inlet cross section 7 a of the left-hand, outer flow duct 7 occupies half of the total inlet cross section in the admission flow plane 20 . The inlet cross section 8 a of the middle flow duct 8 is approximately twice as large as the inlet cross section 9 a of the right-hand outer flow duct 8 , which taken together cover the remaining half of the total inlet cross section, so that the inlet cross sections 7 a , 8 a and 9 a of the flow ducts are in a ratio of 3:2:1 to one another. It is therefore possible, through corresponding flap positions, to open the total cross section by one third, by half, by five sixths or completely.
In the open position, the shut-off flaps 16 and 17 are accommodated in recesses in the respective inside walls 14 and 15 of the collecting chamber 13 , so that in the open position there is a smooth, unobstructed inside wall surface without increased flow resistance.
Use of the invention in a radial-flow turbine and/or a mixed-flow turbine may also be considered as an alternative to an axial-flow impulse action turbine.
|
In an exhaust-gas turbocharger having a compressor and an exhaust-gas turbine, which drives the compressor and comprises a multipart exhaust gas supply duct manifold and a turbine rotor, to which pressurized exhaust gas can be delivered by way of the exhaust gas supply duct, the exhaust gas supply duct manifold includes at least three flow passages, which, except for one, are provided with shut-off flaps, which are adjustable independently of one another.
| 5
|
This is a continuation of application Ser. No. 423,812 filed Dec. 11, 1973 and now abandoned.
BACKGROUND AND SUMMARY OF THE INVENTION
The invention relates to such treatment of cellulose fiber material, e.g. chips, suspended fibers, sawdust and similar, which takes place in the cellulose industry with e.g. impregnated, prehydrolized or cooked fiber material before or after defibration, unbleached or bleached fiber suspensions etc., mainly consisting in that the fiber material during a stage of the manufacture through steaming, impregnation, cooking or other treatment reaches a specific weight higher than that of a liquid in which the fiber material is suspended and even higher than a treatment liquid, and by its sinking movement by its own weight, e.g. through a container, is met by an upward flowing treatment liquid and that liquid is separated and discharged from the upper end of the container.
For the method according to the invention the essential characterization consists in the omission of screens or strainers during the separation of fiber material and liquid. Thus, the fiber material is fed continuously through an inverted into the upper part of a treatment container filled with a suspension liquid and after piling up to a level just underneath the invested funnel opening and after a certain retention time in the container, the treated fiber material is continuously discharged from the container lower end. Above the fiber material surface there is a certain liquid volume. Furthermore, treatment liquid is added close to the bottom of the container and this liquid is flowing upwards counter-currently to the fiber material flow in order to displace the suspension liquid. Upflowing liquid is separated from the surface of the fiber material into the liquid volume around the inverted funnel. By choosing proper funnel dimensions the upflow liquid velocity around the funnel can be kept relatively low so that even light fiber material particles will not tend to be carried or floated upwards. Also the liquid outlets from said volume should be located at a relatively high level compared to the inverted funnel outlet in order to stabilize the liquid flow. Thus, fiber material particles will get time to sediment or settle on the surface of the other fiber material and thereafter follow it downwards.
The commonly known problem within the cellulose industry with plugged strainers in connection with separation of fiber material and liquid can therefore by means of such treatment of the fiber material be considered solved. The invention is even directed at an apparatus suitable for the working of the method.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be more closely described below with reference to enclosed drawing wherein
FIG. 1 schematically and in vertical section shows a preferred design of an apparatus for carrying out such counter-current displacement treatment of fiber suspensions and
FIG. 2 is a schematic showing of several vessels connected together in series.
DETAILED DESCRIPTION OF THE INVENTION
The shown treatment container is made as a tower with cylindrical wall 10 and with a conically shaped top part 11 and a conical lower part 12. The top part is equipped with a cover 13, to which is fastened a vertical, straight or downward somewhat expanding inlet inverted funnel 14 with completely open lower end through which fiber material 15 is fed into the container. In the container top part above said inverted funnel opening is arranged one or more liquid outlets indicated by pipe 16 through which displaced liquid 17 can leave the container. The container bottom part is equipped with a lid 18, through which a vertical shaft 19 is arranged. The shaft is rotatable by means of a driving device 20 and is equipped with a sealing device, e.g. a packing box 21. Said shaft 19 is hollow and the inside chamber 22 is at its lower end by means of a suitable coupling 23 of e.g. rotor type, connected to a pipe 24 for admission of treatment liquid 25. At the upper end of chamber 22 is arranged one or more radial arm-like devices 26 equipped with hollow chamber 27 and openings 28 for distribution of liquid.
The treatment liquid 25 is fed in through the inlet 24 and reaches first the hollow chamber 22, thereafter the hollow chamber 27 and is thereafter flowing out through the openings 28. During rotation of the shaft 19, the arm 26 is also rotating and treatment liquid is distributed over the cross-section of the container. To said rotating shaft 19 is also fastened a number of arms 29, 30, 31 with e.g. leaf-like shovels 32, 33, 34 for stirring and feeding out of the fiber material which then leaves the container through the outlet 35.
The fiber material level in the container can be controlled by a level meter 38 which through a connecting line 37 is controlling the valve 36 on the outlet line 35. Any desired dilution liquid 39 can be added through a number of evenly distributed inlets 40 around the periphery of the container.
During operation, the fiber material together with its suspension liquid enter through the inverted funnel 14 into the container which is full of liquid or at least has a liquid level above the outlet 16. Due to its sinking tendency the fiber material will form an angled surface 41 corresponding to the natural angle of repose. Said free surface 41 will then represent the outlet area of the fiber material from which upflowing liquid is separated without strainers.
The entering fiber material can also be distributed by means of e.g. a rotating scraper (not shown). A possible design of such a scraper can consist of an elongation of shaft 19 upwards to the neighborhood of the inverted funnel 14. There the shaft can be equipped with one or more scraper arms which are stretching out towards the container periphery. During the rotation of the shaft the incoming fiber material will be distributed over the cross-section of the container and it will then form a more or less horizontal surface. This can be of positive effect to the separation operation.
During its continuous flow downwards in the container the fiber material is met by an upward, counter-currently flowing treatment liquid 25 entering through inlet 24, chamber 22, and chamber 27. This liquid flows out through the openings 28 and is by means of the rotation of shaft 19 distributed over the cross-section area of the container. The treatment liquid can also be distributed in other ways, such as e.g. known from continuous digesters, by adding treatment liquid through a central pipe in the container and flowing radially outwards to separation strainers in the container wall. The quantity of treatment liquid added is balanced with liquid entering and leaving together with the fiber material and liquid added for dilution as well as liquid extracted in such a quantity that treatment liquid is moving upwards counter-currently to the fiber material at a sufficiently low velocity so controlled that said fiber material will not be carried upwards, and furthermore, the outlet 16 for discharge of liquid is arranged at a level so high above the fiber material level and thereby above the inverted funnel lower end, e.g. at a height not less than one fifth of the container diameter, that the liquid chamber 42 gets sufficient cross-section and volume to permit eventual fine particles of fiber material in the liquid to sink downwards, settle and then follow the other fiber material down through the container, i.e. the upflow liquid velocity must be lower than the sinking velocity of the fiber material. In this respect also the cross-section area of the inverted funnel 14 has to be taken in consideration. Preferably it should not exceed one fifth of the container cross-section area. As a result, particles of the fiber material will not reach up to the wall opening of outlet 16 and accordingly no strainers will be needed for separation of liquid and fiber material at the outlet. To operate without strainers is of very great advantage since, as mentioned, especially in connection with fiber material, strainers often have a tendency to plug and thereby cause great problems and possible operation stops.
In the figure, the container 10 itself is shown open through the inlet funnel, or in other words only exposed to the atmospheric pressure, but it is very possible to make the container part of a system of equipment in which it is desirable to maintain a certain pressure during the treatment time. The fiber material can then by known methods be fed into the container by means of e.g. a rotating feeding apparatus or plug feeder, pump, screw or similar. A system working under pressure will not to any considerable degree influence the discharge from the container, since it is possible, as known from continuous digesters, e.g. to blow the content of the pressurized container out through the outlet 35 and regulate the flow by means of a valve 36 for further blowing to suitable cyclon or any treatment apparatus. Due to compression the pressure will also make the fiber material sink faster, especially if it contains air or gases.
In the figure, the container itself is furthermore shown as a separate unit, but the container can also constitute an intergrated part of an apparatus with or without superatmospheric pressure for certain treatment sequence or series of treatments of the fiber material in such a way that the container is e.g. preceded by a similar container (see 10' in FIG. 2) for certain pretreatment of the fiber material and/or is succeeded by a similr container (see 10" in FIG. 2) for certain after-treatment of the fiber material, or that the container constitutes a part of a greater container in which the fiber material can undergo two or more treatment stages after each other in the greater container.
The above description of the invention concerns a preferred embodiment, but the invention can be varied within the scope of the following patent claims.
|
In counter-current treatment of cellulosic fiber material it is known to have strainers for separation of liquid from the fiber material. In this invention strainers are omitted by introducing pretreated sinking fiber material through an inverted funnel into a liquid filled tank passing treatment liquid counter-currently to the fiber material and extract liquid from a liquid room above the surface of the fiber material and above the open lower end of said funnel. The tank may be operated at atmospheric or at higher pressures to suit the conditions.
| 3
|
Subsets and Splits
No community queries yet
The top public SQL queries from the community will appear here once available.