description stringlengths 2.98k 3.35M | abstract stringlengths 94 10.6k | cpc int64 0 8 |
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TECHNICAL FIELD
[0001] This invention relates generally to an implement of a work machine, and, more particularly, to a landscape tiller of a work machine having a single direct drive motor.
BACKGROUND
[0002] Work machines, such as skid steer loaders, tractors, wheel loaders, or backhoe loaders, or other similar work machines use implements, such as landscape tillers, to cultivate the ground, till the ground, level the ground, or other additional operations. When used to perform these sorts of operations, it is normally helpful to have the landscape tiller balanced. Most landscape tillers use two motors, each being positioned on one end of the tiller to offset the weight of each motor and help balance the tiller. Having two motors increases the cost of the tiller and the potential for malfunction. The use of a single motor large enough to drive the landscape tiller, however, can cause the landscape tiller to be off balance.
[0003] One known tiller assembly design is disclosed in U.S. Pat. No. 6,467,550 B1 that issued to Firdaus on Oct. 22, 2002. It discloses a tiller assembly including a tine assembly that is rotatably connected to a tiller body. The tiller assembly includes a hydraulic system that is operatively connected to a hydraulic motor that drives the tine assembly. This design has only one hydraulic motor to drive the tine assembly, but due to the weight of the hydraulic motor, the tiller may become off balance and may not till level.
[0004] The present disclosure is directed to overcoming one or more of the problems as set forth above.
SUMMARY OF THE INVENTION
[0005] One embodiment disclosed herein is an implement comprising a housing having a first-side portion and a second-side portion, at least one element having a weight and being attached to the second-side portion of the housing, the weight of the element creating a moment arm, a shaft positioned between the first-side portion and second-side portion of the housing and operably coupled to at least one of the element, and a counterweight attached to the first-side portion of the housing to offset the moment arm created by the weight of the element.
[0006] In another embodiment disclosed herein, a method comprises fabricating a housing having a first-side portion and a second-side portion, attaching a motor to the second-side portion of the housing, positioning a shaft between the first-side portion and the second-side portion of the housing and connecting it thereto, operably coupling the motor to the shaft, and attaching a counterweight to the first-side portion of the housing to offset the moment arm created by the weight of the motor.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] For a better understanding of the present disclosure, reference may be made to the accompanying drawings in which:
[0008] FIG. 1 is a diagrammatic front and side view of a landscape tiller operatively mounted to a skid steer loader;
[0009] FIG. 2 is a diagrammatic view of the underside of the landscape tiller;
[0010] FIG. 2 a is a diagrammatic view of a side portion of the landscape tiller; and
[0011] FIG. 3 is a diagrammatic side view of the side portion of the landscape tiller.
DETAILED DESCRIPTION
[0012] Referring to the drawings, depicted in FIG. 1 is an implement, such as a landscape tiller 100 , operatively mounted in the conventional manner to a body portion 107 of a work machine 105 , such as, but not limited to, a skid steer loader, tractor, wheel loader, or backhoe loader. The work machine 105 includes a hydraulic system 110 including a source of pressurized fluid. The hydraulic system 110 includes a pair of hydraulic fittings 115 adapted to attach, in fluid communication, the landscape tiller 100 with the hydraulic system 110 . First and second level indicators 120 , 125 are attached at opposite ends of the landscape tiller 100 so that the operator can visually determine the orientation of the landscape tiller 100 .
[0013] As depicted in FIG. 2 , with reference numbers of previous figures being used to identify similar components therein, the landscape tiller 100 includes a tiller mechanism 205 partially enclosed in a housing 210 having a first-side portion 215 and a second-side portion 220 . As depicted in FIG. 2 a, the housing 210 includes a first aperture 225 in the first-side portion 215 and a second aperture (not shown) in the second-side portion 220 .
[0014] As further depicted in FIG. 2 , the tiller mechanism 205 includes a shaft 245 , having a first end 250 and a second end 255 . The first end 250 is adjustably and rotatably attached to the first-side portion 215 of the housing 210 . The second end 255 is operably attached to a motor 260 (as more specifically described below), which may be a hydraulic motor, a gerotor type motor, an electric motor, a gasoline motor, or other types of motors. The tiller mechanism 205 further includes a plurality of plates 265 attached to the shaft 245 by welding or another suitable process. Removably attached to each plate 265 is a plurality of teeth 270 .
[0015] As depicted in FIG. 2 , the second-side portion 220 of the housing 210 has at least one element attached thereto such that the second-side portion 220 of the housing 210 is heavier than the first-side portion 215 of the housing 210 when nothing is attached thereto, and because of the weight of the at least one element, a moment arm is created. In this embodiment, the element includes the motor 260 , but alternatively, may include an additional motor, at least one pump, at least one controller, etc. The housing 201 , further, has a first skid 275 and second skid 280 attached thereto, by bolting or another suitable process, to the first-side portion 215 and second-side portion 220 , respectively. The first and second skids 275 , 280 contact the ground when the landscape tiller 100 is in an operable condition. Mounted above the second skid 280 on the second-side portion 220 of the housing 210 is a motor mount 282 . The motor mount 282 is attached by bolting it thereto, or another suitable process. The motor 260 is attached to the motor mount 282 in a conventional manner at the second-side portion 220 . The motor 260 includes a splined coupling (not shown) that extends through the second aperture in the second-side portion 220 of the housing 210 and is rotatably attached to the shaft 245 in a conventional manner. A motor-shaft seal (not shown) is attached to the motor 260 so as to protect it against debris entering therein. Additionally, a shaft seal (not shown) located adjacent the motor-shaft seal is attached at the attachment location of the splined coupling of the motor 260 and the shaft 245 . Finally, first-end portions 294 of a pair of hydraulic hoses 292 are connected with the motor 260 and second-end portions 295 of the hydraulic hoses 292 are connected with the hydraulic fittings 115 of the hydraulic system 110 , as depicted in FIG. 1 . When the hydraulic hoses 292 are connected with the motor 260 of the landscape tiller 260 and the hydraulic fittings 115 of the work machine 105 , the motor 260 is in fluid communication with the hydraulic system 110 .
[0016] As depicted in FIGS. 2 and 3 , with reference numbers of previous figures being used to identify similar components therein, a counterweight 297 is located at the first-side portion 215 of the housing 210 to offset the moment arm created by the weight at the second-side portion 220 of the housing 210 , including the weight of the motor 260 . The counterweight 297 , in this embodiment, is attached to the first-side portion 215 of the housing 210 , but may also be formed integrally with the housing 210 . The counterweight 297 , of this embodiment, includes a first plate 302 and a second plate 299 , each plate having an aperture (not shown). The first plate 302 is placed on an outside 301 of the first-side portion 215 of the housing 210 covering the first aperture 225 and the second plate 299 is placed on an inside 298 of the first-side portion 215 of the housing 210 covering the first aperture 225 . The first and second plates 302 , 299 are bolted together in compressive engagement with the first-side portion 215 of the housing 210 ; the compressive forces holding the first and second plates 302 , 299 in place.
[0017] Finally, the shaft 245 is adjustably and rotatably attached to the first and second plates 302 , 299 by extending the first end 250 of the shaft 245 through the apertures in the first and second plates 302 , 299 creating a sealed rotatable attachment thereto. Then a plurality of floating bearings 303 are attached to the first end 250 of the shaft 245 and attached to the first plate 302 , further rotatably attaching the first end 250 of the shaft 245 to the first and second plates 302 , 299 . Adjusting the location of the attachment of the counterweight 297 to the first-side portion 215 of the housing 210 permits the shaft 245 to align with the motor 260 . In particular, the shape of the first aperture 225 in the housing 210 permits the first and second plates 302 , 299 to be adjusted by moving the first and second plates 302 , 299 within the first aperture 225 until the floating bearings 303 align with the shaft 245 and the shaft 245 aligns with the motor 260 .
INDUSTRIAL APPLICABILITY
[0018] Normally, the operator will activate the landscape tiller 100 in a conventional manner so that pressurized fluid is sent from the hydraulic system 110 through the hydraulic hoses 292 to the motor 260 . The pressurized fluid activates the motor 260 and the motor 260 rotates the shaft 245 . The shaft 245 may rotate in either a clockwise or a counter-clockwise direction as selected by the operator.
[0019] The landscape tiller 100 normally needs to be substantially balanced. In the present embodiment, this is accomplished by having the counterweight 297 on the second-side portion 220 of the housing 210 being of substantially the same weight as that of the motor 260 so as to offset the moment arm created by the weight of the motor 260 . Additionally, the housing 210 may be formed with the counterweight 297 integral with the first-side portion 215 thereof so as to offset the moment arm created by the weight of the motor 260 . Finally, the counterweight 297 may also offset the moment arm created by not only the weight of the motor 260 but the weight of any other element that may be attached to the second-side portion 220 of the housing 210 , such as an additional motor, at least one pump, at least one controller, etc., where the weight of the counterweight 297 is substantially similar to the weight of all of the elements attached to the second-side portion 220 of the housing 210 . This will permit the landscape tiller 100 to operate in a relatively balanced position.
[0020] Other aspects, objects and advantages of the invention could be obtained from a study of the drawings, the disclosure and the appended claims. | An implement and method of assembly, wherein the implement comprises a housing having a first-side portion and a second-side portion, at least one element having a weight, the element being attached to the second-side portion of the housing and the weight of the element creating a moment arm, a shaft positioned between the first-side portion and second-side portion of the housing and operably coupled to at least one of the element, and a counterweight attached to the first-side portion of the housing, the counterweight offsetting the moment arm created by the weight of the element. | 4 |
This application is a continuation-in-part of Ser. No. 621,419, filed June 18, 1984 now abandoned.
FIELD OF THE INVENTION
It is an object of the present invention to provide a new class of polymerizable monomers which are polyfunctional, so as to be cured to cross-linked high molecular weight polymer networks, and which are readily cationically polymerizable.
BACKGROUND OF THE INVENTION
In USSR Patents 443874 and 478026 there are described ion exchange polymers prepared by free radical copolymerization of styrene or maleic anhydride, respectively, with p-glycidoxy- α-methyl styrene (I) ##STR2##
In U.S. Pat. No. 3,327,019 there are described diethers which are the reaction product of p-glycidoxy styrenes and polyols. These compounds include aliphatic hydroxyl groups.
In Macromolecules, 16, 510-517(1983), there is described the cationic polymerization of p-methoxy and p-(ethoxymethoxy)- α-methyl styrenes with boron trifluoride etherate as initiator in dichloromethane. These polymers are then subjected to ether cleavage reactions to yield linear polymers containing pendant phenolic groups.
It is known from kinetic studies of the cationic polymerization of p-methoxy styrene that this monomer has a very high rate of polymerization. See, e.g., Macromolecules, 9, 931-936(1976); and Polymer, 16, 819-826(1975).
SUMMARY OF THE INVENTION
The present invention is directed to a new class of cationic polymerizable monomers. In common with the monofunctional monomers discussed above, the inventive monomers contain styryloxy (p-vinylphenol ether) functionality. They are represented by the formulas: ##STR3## where R 1 and R 2 are H and the other is methyl; R 3 and R 4 are H, lower alkyl, or alkoxy if R 2 is not methyl; R 5 is a divalent hydrocarbon radical; G is any multivalent organic or inorganic radical free of amino, aliphatic thiol, aliphatic hydroxyl, or other groups which interfere with cationic polymerization; and n is an integer of two or more.
In addition to high reactivity to cationic polymerizations, the inventive monomers have been shown to develop an intense coloration when they are polymerized by UV irradiation in the presence of acid generating photoinitiators. Under some circumstances this coloration is sufficient to mask a substrate, providing a useful means of generating opacity in photocurable coatings. This coloration is also observed in chemically initiated cationic polymerizations of these materials.
An additional feature of solid polyfunctional styryloxy resins of the invention is an ability of these resins to cure by UV irradiation without added photoinitiator. This cure is believed to involve a radical mechanism.
DETAILED DESCRIPTION OF THE INVENTION
The inventive monomers may readily be prepared from p-vinyl phenols, p-propenyl phenols or p-isopropenyl phenols by a variety of methods such as etherification with an appropriate multifunctional etherifying agent, or reaction with multifunctional epoxies followed by reaction of the resulting aliphatic hydroxyl with a polyisocyanate or other suitable capping agent.
A suitable p-vinyl phenol is the commercially available vinyl guaiacol (2-methoxy-4-vinyl phenol). Synthetic methods for obtaining other suitable phenols include those reported in U.S. Pat. No. 3,327,019, column 3, line 38 - column 4, line 2; Japanese Kokai Tokkyo Koho 79:55,529 (dehydrogenation of ethyl phenol to give vinyl phenol); J. Kahovec, et al., J. Collect. Czech. Chem. Commun., 36, 1986(1971) (various α-methylvinyl phenols); and Macromolecules, 16 510-517 (1983)(p-hydroxy-α-methyl styrene by cleavage of 2,2-bis(p-hydroxyphenyl)-propane), the disclosures of which are incorporated herein by reference.
Yet another synthetic procedure involves the modification of the procedure of Macromolecules, 16, 510-517 (1983), in which p-(ethoxymethoxy)-α-methyl styrene is prepared from p-hydroxyacetophenone by etherifying the hydroxyl group and then using a Wittig reaction on the resulting p-(ethoxymethoxy) acetophenone. One modification required for the synthesis of the inventive monomers is the initial reaction of p-hydroxyacetophenone with an appropriate polyfunctional etherification reagent to form a molecule having multi-acetophenone functionalities. Subjecting such a molecule to a Wittig reaction as in the Macromolecules reference will yield a polyfunctional monomer of the invention.
An alternative modification of the Wittig reaction procedure is to use a monofunctional etherification reagent which is capable of entering into subsequent chain extension reactions with polyfunctional moieties. An example is etherification of p-hydroxyacetophenone with allyl bromide, Wittig reaction to give the corresponding allyloxy styrene and hydrosilation using a silicone resin with poly Si-H functionality.
In the formulas (II) and (III) above, it is generally preferred that R 3 is H, methyl, or methoxy and R 4 is H. However, other lower alkyl or alkoxy (up to about C 4 ) may be included as substituents R 3 and/or R 4 ).
Examples of R 5 groups are methylene, ethylene or cycloaliphatic, aromatic hydrocarbons such as 1,4-dimethylenebenzene or unsaturated linear hydrocarbons such as propenylene or butenylene.
The only limitation on G is that it must not interfere with cationic polymerization of the styryloxy groups. G must not include any strongly electron withdrawing group in conjugation with the styryloxy group oxygen atom as such groups will interfere with vinyl cationic polymerizations. Amines, aliphatic hydroxyls, and aliphatic thiols are known to prevent or slow vinyl cationic polymerizations. "Developments in Polymerization -1," R.N. Howard ed., Applied Science Publishers, 1979, pg. 80. Inclusion of these groups in G should therefore also be avoided.
Polymerization of the inventive monomers may be accomplished by conventional acid and Lewis acid cationic initiators such as methane sulfonic acid, toluene sulfonic acid and boron trifluoride etherate. UV cationic initiators may also be used. Such UV cationic photointiators include salts of a complex halogenide having the formula:
[A].sub.d.sup.+ [MX.sub.3 ].sup.-(e-f),
where A is a cation selected from the group consisting of iodonium, sulfonium, pyrylium thiopyrylium and diazonium cations, M is a metalloid, and X is a halogen radical, b equals e minus f, f equals the valance of M and is an integer equal to from 2 to 7 inclusive, e is greater than f and is an integer having a value up to 8. Examples include di-p-tolyl iodonium hexafluorophosphate, diphenyl iodonium hexafluorophosphate, diphenyl iodonium hexafluoroarsenate and UVE 1014 (trademark of General Electric), a commercially available sulfonium salt of a complex halogenide.
Certain monomers, usually solids, will also undergo UV initiated polymerization in the solid state without initiator, yielding an essentially uncolored product. A radical mechanism is believed to be involved. This UV, initiator free, polymerization has also been obtained with a liquid silicone backbone resin of the invention.
The production of colored reaction mixtures by cationic initiators has been reported before for styryloxy monomers. Permanent coloration in the cured products of the invention is believed to result from particular termination reactions involving stable carbocations. The development of color can thus be controlled by selecting polymerization conditions designed to select for or against termination by stable carbocations. The development of permanent color as a result of polymerization termination reactions is especially advantageous at certain UV cured opaque coating applications where the use of pigments or dyes in the composition blocks UV, resulting in only surface cure of the coating. Since the inventive resins develop their intense coloration only after initiation of polymerization, initation by UV is not interfered with. The invention may be illustrated by reference to the following nonlimiting examples:
EXAMPLE 1
To a mixture of 3.0 grams vinyl guaiacol, 27.0 grams ethanol, 30 grams acetone and 20 grams potassium carbonate stirred in a round-bottom flask was added, dropwise over 30 minutes, a solution of 2.8 grams α, α'-dibromo-p-xylene in 30 grams acetone. The resulting mixture was stirred at room temperature for 24 hours. The potassium carbonate was then filtered off and the solvent removed under reduced pressure. The residue was redissolved in chloroform (250 ml) and extracted with distilled water (3×100 ml). The chloroform layer was then dried over sodium sulfate and filtered. Solvent was removed under reduced pressure and the residue was recrystallized from hot ethanol to yield 2.01 grams slightly yellow crystals. This material was identified from proton NMR (CDCl 3 ; δ =3.87, singlet, methoxy protons; δ5.05,5.22.5.45 and 5.74 quartet, β-vinyl protons; δ=5.12, singlet, benzyl protons; δ=6.44-7.2 multiplet, α-vinyl and guaiacol ring protons; δ=7.45, singlet, xylene ring protons) and IR (3085cm -1 : vinyl C-H; 3010cm -1 : aryl-H; 2860cm -1 methoxy C-H; 1625cm -1 conjugated c=c; 1140cm -1 : aromatic-0; 1030cm -1 : alkyl C-O-aromatic; 995 and 900cm -1 : R-CH=CH 2 : 860cm -1 : 2 adjacent aromatic C-H) spectra as αα'-bis(2-methoxy-4-vinylphenoxy)-p-xylene.
EXAMPLE 2
A mixture of 5.0 grams vinyl guaiacol, 3.47 grams allyl glycidyl ether, 45 grams ethanol, 0.68 grams of a commercially available ion exchange resin (Rohm and Haas Amberlyst A-27) and 0.80 grams benzyl trimethyl ammonium hydroxide was heated for 65 hours at reflux. The mixture was then filtered and solvent was removed under reduced pressure. The residue was chromatographed on a silica gel column using chloroform as the eluent, yielding 6.8 grams of a slightly orange viscous material which was identified by proton NMR and IR spectra as the adduct of vinyl guaiacol and allyl glycidyl ether.
A mixture of this adduct (2.64 grams), a commercially available polyfunctional isocyanate resin (Bayer Desmodur L-75) (2.92 grams), 0.06 grams stannous octoate, and 20 grams chloroform was heated at reflux for 90 minutes under nitrogen. At the end of this time infrared analysis indicated that all of the isocyanate groups had been consumed. After solvent was evaporated, the crude product was washed in a soxhlet extractor and dried in a vacuum desiccator to yield 2.44 grams of product. This product was shown by liquid chromatography, NMR and IR spectroscopy to be a high molecular weight resin containing styryloxy functional groups.
EXAMPLE 3
A solution of 0.120 grams of the αα'-bis (2-methoxy-4-vinylphenoxy)-p-xylene prepared in Example 1 and 0.010 grams of a commercially available cationic sulfonium salt photoinitiator (GE UVE-1014) in 1.000 gram chloroform was coated onto a glass slide and the solvent allowed to evaporate. The coating was then irradiated under a medium-pressure mercury lamp at an intensity of 70 mw/cm 2 for 20 seconds, producing a tack-free brittle film with an intense purple coloration. The irradiated film was effective at obscuring the contrast on a Morest chart #05. The irradiated material was insoluble in common organic solvents.
EXAMPLE 4
A solution of 0.100 grams of the styryloxy resin prepared in Example 2 and 0.006 grams of ditolyliodonium hexafluorophosphate in 0.100 grams of anisole was coated onto a glass slide and irradiated under a medium-pressure mercury lamp at an intensity of 60mw/cm 2 for 5 seconds. The film was tack free after irradiation and insoluble in common organic solvents.
EXAMPLE 5
A dilute solution of the α,α'-bis (2-methoxy-4-vinylphenoxy)-p-xylene synthesized in Example 1 was prepared by dissolving 0.4022 grams of this material in 50 milliliters of dry dichloromethane. To this solution was added, with stirring, 10 milliliters of a solution prepared by dissolving 0.0574 grams of triphenylcarbenium hexachloroantimonate in 100 milliliters of dry dichloromethane. The reaction mixture developed a red color rapidly and was stirred for three hours at room temperature. The mixture was then added to 50 milliliters of methanol to quench the reaction. Solvents were removed under reduced pressure yielding 0.395 grams of a pink solid polymer. The polymer was dissolved in hot dichloromethane and absolute alcholol was added gradually. On cooling a white precipitate formed. Solvents were removed under reduced pressure yielding 0.352 grams of material. This material was dissolved in tetrahydrofuran and analyzed on a Waters Model 244 Liquid Chromatograph fitted with one 1000 angstrom and two 100 angstrom columns. The material was found to be a high polymer with a peak molecular weight corresponding to 6,500 on a polystyrene calibration.
EXAMPLE 6
To a mixture of 20 grams vinyl guaiacol, 180 grams ethanol, 300 grams acetone and 65.6 grams potassium carbonate was added dropwise over 20 minutes 22.27 grams of ethyl bromoacetate. The color of the mixture changed gradually from green to light brown. The mixture was heated at 45° C. for two hours, then cooled to room temperature and left for a further sixteen hours. Thin-layer chromatography on a sample of the reaction mixture showed the presence of vinyl guaiacol after this time. Consequently, the mixture was heated to reflux for 7 hours and left at room temperature for a further 64 hours. The mixture was then filtered and solvents were removed under vacuum. When 350 grams of solvent had been removed, a precipitate formed in the mixture. The precipitate (3.84g.) was removed by filtration. The remaining material was distilled into three fractions and a residue (4.32g, 4.91g, 1.48g, and llg respectively). Gas-liquid chromatographic analysis of the second fraction showed that it consisted principally (85%) of the adduct of ethyl bromoacetate and vinyl guaiacol, 3-methoxy-4-(2-oxo-2-ethoxy)-ethoxy styrene. The adduct was characterized by NMR (CDCl 3 ;δ-1.27, triplet, ester methyl protons; δ=3.91, singlet, methoxy protons; δ=4.3, quartet, ester methylene protons; δ=4.72, singlet, ether methylene protons; δ=5.1,5.3,5.5, and 5.8, quartet, ⊕vinyl protons; δ=6.5-7.1, multiplet, α-vinyl and ring protons). The remainder of the second fraction (15%) consisted of vinyl guaiacol.
Material from the second fraction (4.0 grams), 1,6-hexanediol (1.0 gram) and lithium ethylene glycolate (0.05 gram) were refluxed in dry heptane for 3 hours. The heptane was removed by distillation to yield 4.73 grams of product. The product was analyzed by liquid chromatography and shown to consist of approximately equal portions of unreacted 3-methoxy-4-(2-oxo-2-ethoxy)ethoxy styrene (MOES), the monofunctional product of the transesterification of MOES and 1,6-hexanediol, and the difunctional product of the transesterification of MOES and 1,6-hexanediol.
A concentrated solution of this product mixture was prepared by dissolving 0.45 grams of the material in 0.65 grams dry dichloromethane. When one drop of methanesulfonic acid was added to the solution the material polymerized instantly to give a red, insoluble product.
EXAMPLE 7
To a solution of 136g 4-hydroxyacetophenone in 500 mls acetone was added 276.41g potassium carbonate. This mixture was stirred for 15 minutes. A solution of 133g allyl bromide in 200 mls acetone was then added dropwise over 45 minutes, and the resulting mixture was stirred for a further 4 hours and left standing for a further 16 hours. Thin-layer chromatography showed some starting material to be present at the end of this time. The mixture was then heated to reflux for 4 hours and left standing a further 16 hours. After filtration the solvent was removed by distillation leaving 230g of a brown liquid. This residue was distilled under reduced pressure (B.Pt. 107°-115° C. at 0.6mmHg.) to yield 158g of pale yellow liquid which was identified by infrared and n.m.r. spectroscopy as 4-allyloxyacetophenone.
To a solution of 5.58g potassium metal in tertbutanol was added 51g methyl triphenylphosphonium bromide. The resulting yellow suspension was stirred for 20 minutes. A solution of 18.86g 4-allyloxyacetophenone in 30 mls tert-butanol was then added gradually and stirred for 16 hours at room temperature. After this time, the mixture was filtered and solvent removed under reduced pressure. The resulting mixture was extracted with petroleum ether to yield 28g of brown resin. This resin was distilled under reduced pressure (B.Pt. 88° C. at 1 mm Hg) yielding 15.21g of a clear colorless liquid which was identified by infrared and n.m.r. spectroscopy as 4-allyloxy isopropenyl benzene (Proton NMR: (CDCl 3 ) δ=2.12 singlet, α-methyl protons; δ=4.50, 4.58, doublet, allyloxy methylene protons; δ=5.0-6.5, multiplets, allyl and vinyl group protons; δ=6.80, 6.95, 7.35 and 7.50, quartet, aromatic protons).
A solution of 13.92g 4-allyloxy isopropenyl benzene in 50.0g toluene was stirred for 5 minutes at room temperature. To this solution was added 0.693g of a 2% solution of dihydrogen hexachloroplatinate hexahydrate in n-butyl acetate. The resulting solution was then heated to 80° C. and 40.40g of a difunctional Si-H terminated polydimethylsiloxane resin of molecular weight 1010 was added gradually over 90 minutes. At the end of that time infrared spectroscopy showed that the peak at 2130 cm- -1 had disappeared indicating complete consumption of the Si-H groups. Solvent was then removed under reduced pressure to yield 55.78g of a light brown low viscosity liquid.
Reaction of 1 gram of this product with 0.02 grams methanesulfonic acid led to rapid formation of a rubbery gel insoluble in common organic solvents.
EXAMPLE 8
A mixture of 20.0g 4-hydroxy-3-methoxy styrene, 27.5g potassium carbonate and 180 grams ethanol was heated to 40° C. and 17.7g allyl bromide addded gradually as a 50% solution in ethanol. The mixture was stirred for two hours at 55°-65° C. The solids were then filtered and solvent removed under reduced pressure. The remaining liquid was then distilled under reduced pressure (B.Pt. 96°-108° C. at 0.2mmHg) to yield 13.2g of clear liquid identified by infrared and n.m.r. spectroscopy as 4-allyloxy-3-methoxystyrene (Proton NMR: (CDCl 3 ) δ=3.87, singlet, methoxy protons; δ=4.55, 4.62, doublet, allyloxy methylene protons; δ=5.05-7.1, multiplets, vinyl, allyl and aromatic protons.
To a solution of 9.5g 4-allyloxy-3-methoxy styrene in 34.75g toluene was added 0.459g of a 2% solution of dihydrogen hexachloroplatinate hexahydrate in n-butyl acetate. The resulting solution was then heated to 80° C. and 25.3g of a difunctional Si-H terminated polydimethylsiloxane resin of molecular weight 1010 was added gradually over 30 minutes. At the end of that time infrared spectroscopy showed that the peak at 2130 cm -1 had disappeared indicating complete consumption of the Si-H groups. Solvent was then removed under reduced pressure to yield 32.97g of a clear colorless resin.
Reaction of 0.5 gram of this product with 0.02 gram methane sulfonic acid led to rapid formation of a rubbery purple gel which was insoluble in common organic solvents.
EXAMPLE 9
An aliquot of the difunctional styryloxy silicone resin synthesized in Example 2 was blended with 3% by weight of a commercially available triarylsulfonium salt photoinitiator (UVE-1014, trademark of General Electric). A drop of this formulation was placed on a glass slide and irradiated under a medium-pressure mercury lamp at an intensity of about 100mw/cm 2 at 365nm for 10 seconds. At the end of this time the formulation had completely cured to a rubbery tack-free film. Irradiation for 30 seconds led to formation of a purple rubbery tack-free film.
EXAMPLE 10
To a solution of 122g 4-hydroxybenzaldehyde in 500 mls acetone was added 276g potassium carbonate. This mixture was stirred for 15 minutes. A solution of 133g allyl bromide in 200 mls acetone was then added dropwise over 30 minutes. The resulting mixture was heated at reflux for 1 hour, left standing for a further 16 hours and finally heated at reflux for 2 hours. After filtration, the solvent was removed by distillation leaving 175g of a reddish liquid. This residue was distilled under reduced pressure (B.Pt. 104°-114° C. at 1.5 mmHg) to yield 130g of a pale yellow liquid which was identified by infrared and n.m.r. spectroscopy as 4-allyloxybenzaldehyde.
To a solution of 9.36g potassium metal in 500 mls tert-butanol was added 85.68g methyltriphenylphosphonium bromide. The resulting yellow suspension was stirred for 20 minutes and 32.4g 4-allyloxybenzaldehyde was then added over 10 minutes. This mixture was stirred for 30 minutes and then allowed to stand overnight. After filtration the solvent was removed under reduced pressure leaving 107g of a red semi-solid residue. Petroleum ether (B.Pt. 40°-60° C.) was added to the residue precipitating a solid which was filtered. After removal of the petroleum ether, the remaining resin was distilled under reduced pressure (B.Pt. 68°-82° C. at 0.4 mmHg) yielding 26.7g of a clear colorless liquid which was identified by infrared and n.m.r. spectroscopy as 4-allyloxystyrene (Proton NMR: (CDCl 3 ) δ=4.50, 4.58, doublet, allyloxymethylene protons; δ=5.0-6.5, multiplets, allyl and vinyl group protons; δ=6.80, 6.95, 7.30 and 7.45, quartet, aromatic protons). A solution of 8.0g 4-allyloxystyrene in 33.0g toluene was stirred for 5 minutes at room temperature. To this solution was added 0.414g of a 2% solution of dihydrogen hexachloroplatinate hexahydrate in n-butyl acetate. The resulting solution was then heated to 80° C. and 25.25g of a difunctional Si-H terminated polydimethylsiloxane resin of molecular weight 1010 was added gradually over 4 hours. At the end of that time, infrared spectroscopy showed that the peak at 2130 cm -1 had disappeared indicating complete consumption of the Si-H groups. Solvent was then removed under reduced pressure to yield 33g of a light brown low viscosity liquid. Reaction of 1 gram of this product with 0.02 grams methanesulfonic acid led to rapid formation of a rubbery gel insoluble in common organic solvents.
EXAMPLE 11
Example 3 was repeated except that no photoinitiator is used and the irradiation time was 1 minute. A slightly yellow film insoluble in chloroform and other common organic solvents was obtained.
EXAMPLE 12
A mixture of 8.0g 4-allyloxystyrene in 26.57g toluene was stirred at room temperature for 5 minutes and 0.35g of a 2% solution of dihydrogen hexachloroplatinate hexahydrate in n-butyl acetate was added. The mixture was then heated to 80° C. and 18.57g of a heptafunctional Si-H containing polydimethylsiloxane resin of molecular weight 2600 was added over 40 minutes.
Solvent was then removed under reduced pressure to yield 26.76g of a slightly yellow viscous liquid.
Reaction of 0.5 gram of this product with 0.02 gram methane sulfonic acid led to rapid formation of a reddish brown solid mass.
EXAMPLE 13
An aliquot of the styryloxy silicone resin synthesized in Example 12 was blended with 3% by weight of a commercially available triarylsulfonium salt photoinitiator (UVE-1014, trademark of General Electric). A drop of this formulation was placed on a glass slide and irradiated under a medium-pressure mercury lamp at an intensity of about 100 mw/cm 2 at 365g for 30 seconds. At the end of this time the formulation had completely cured to a tack-free rubbery film. Irradiation for 70 seconds led to formation of a purple rubbery tack-free film. | Polyfunctional cationically polymerizable styryloxy compound of the formula ##STR1## where R 1 and R 2 are H, or one of R 1 and R 2 are H and the other is methyl; R 3 and R 4 are H, lower alkyl, or alkoxy if R 2 is not methyl; R 5 is a divalent hydrocarbon radical; G is any multivalent organic or inorganic radical free of amino, aliphatic hydroxyl, aliphatic thiol or other groups which interfere with cationic polymerization; and n is an integer of two or more. | 2 |
CROSS-REFERENCE TO RELATED APPLICATION
This application contains subject matter in common with prior application Ser. No. 06/508,603, filed June 28, 1983, for WHEELCHAIR HAVING ANTI-ROLLBACK MECHANISM, now U.S. Pat. No. 4,462,605.
BACKGROUND OF THE INVENTION
The anti-rollback mechanism for manual wheelchairs disclosed in the prior patent application, while completely effective in its operation, is constructed with relatively expensive precision machine parts including sprag clutches and stainless steel races. This tends to reduce the overall practicality of the mechanism from a commercial standpoint.
Accordingly, it is the object of the present invention to provide a wheelchair anti-rollback mechanism of considerably greater simplicity, constructed from comparatively inexpensive components, such as bicycle brake pads and simple springs, all without loss of the full operational capability of the mechanism in the prior application. In fact, both mechanisms are operated in exactly the same manner by the occupant of a manual wheelchair. The less expensive mechanism embodied in this invention utilizes a simple over center linkage including component parts which can be stamped from sheet metal or molded from plastics.
An object of the present invention is to provide a wheel-chair anti-rollback mechanism which utilizes instead of an expensive one-way clutch a simple over center friction lock mechanism including a partial or complete brake drum fixed to the frame of the chair and cooperative pivoted over center brake shoes carried by the main wheel of the chair, together with simplified means to release the shoes when backward propulsion of the wheelchair is desired. As in the prior application, the mechanism normally allows only forward motion of the manual wheelchair as when traveling up an incline, thereby greatly reducing the effort expended by the user in powering the chair at this time. Without any anti-rollback mechanism on the chair, the user must exert a force on the propulsion ring with the hands and arms to counter the tendency for the chair to roll backwards on an incline. The extra energy required to prevent backward movement of the chair greatly increases the fatigue factor, especially when traveling up long inclines. The energy required is expended much more beneficially for producing forward motion only according to the invention.
Further objects of the invention are to provide an anti-rollback mechanism of decreased weight compared to previous designs, wherein the mechanism does not contribute to tire wear, and to utilize a self-locking friction mechanism as the heart of the anti-rollback system.
Other features and advantages of the invention will become apparent during the course of the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevation of a manual wheelchair equipped with the anti-rollback mechanism according to one preferred embodiment of the invention.
FIG. 2 is an enlarged fragmentary side elevation showing the mechanism where the chair is in the normal forward movement mode.
FIG. 3 is a similar view of the mechanism in the locked mode to prevent backward rolling of the chair.
FIG. 4 is a similar view of the mechanism released to allow the chair to be propelled rearwardly by the occupant.
FIG. 5 is a fragmentary exploded perpsective view of components of the anti-rollback mechanism.
FIG. 6 is a side elevation of the wheelchair equipped with an anti-rollback mechanism according to a modified embodiment of the invention.
FIG. 7 is an enlarged fragmentary side elevation of the modified embodiment showing the mechanism where the chair is in the normal forward movement mode.
FIG. 8 is a similar view of the modified embodiment of the mechanism released to allow the chair to be propelled rearwardly by the occupant.
DETAILED DESCRIPTION
Referring to the drawings in detail wherein like numerals designate like parts, a conventional manually powered wheelchair 10 includes main wheels 11, each having a manual propulsion ring 12 disposed near the outer side thereof in ready reach of the hands of a chair occupant.
In the present invention, as in the prior referenced patent application, the propulsion ring 12 is not directly and rigidly anchored to the main wheel 11 but instead is connected therewith through a lost motion mechanism, whereby the ring 12 can be rotated in either direction relative to the wheel 11 through short distances only.
The lost motion mechanism comprises preferably three circumferentially spaced spokes 13, adapted to be formed of sheet metal and being connected to form a unitized hub at their inner ends by yoke extensions 14 having fastener-receiving apertures 15. The hub structure of the spokes 13 thus formed can be supported on a suitable low friction bearing carried by the axle of the main wheel 11, substantially in the manner disclosed in the prior referenced application. The arrangement forms a three spoke spider structure which can have limited rotation about the axle of the main wheel 11.
Each spoke 13 carries an outer end crosshead 16 having a slot 17 receiving a radial drive pin 18 fixed to and projecting inwardly from the rim 19 of main wheel 11. It can be seen that a rotational lost motion connection between the wheel 11 and the spider consisting of the spokes 13 is provided.
The manual propulsion ring 12 is equipped on its inner side at circumferentially spaced points with threaded studs 20 engaging through openings 21 of the spokes 13 near their outer ends, the studs receiving nuts 22 thereon to complete the rigid connections between propulsion ring 12 and the spokes 13.
The anti-rollback mechanism proper comprises a circular brake drum sector 23 having a friction facing 24, and being disposed interiorly of the wheel 11 and between such wheel and the adjacent side frame structure 25 of the wheelchair. The drum sector 23 is secured by screws 26 to a sector mounting plate 27 having a center opening 28 receiving a projecting horizontal support pin 29 carried by the frame structure 25 and being coaxial with the axis of rotation of the wheel 11. The arcuate surface of friction facing 24 is concentric with the wheel 11 and propulsion ring 12, as shown.
The attaching screws 26 for brake drum sector 23 after passing through apertures 30 of sector mounting plate 27 are received in threaded openings 31 of clips 32 and 33 which embrace vertical and horizontal components of the chair frame 25 to secure the drum sector to such frame rigidly. In some cases, a complete circular friction brake drum can be utilized in lieu of the drum sector 23, the latter being preferred in the interest of saving weight.
The anti-rollback mechanism further includes preferably three over center friction brake shoe devices spaced equidistantly circumferentially of the wheel 11 and spaced somewhat from corresponding sides of the spokes 13. Each device 34 comprises a shoe element 35 having a friction lining 36 of rubber or the like secured thereto, the lining preferably having an arcuate face 37 for contact with the drum facing 24. Each shoe element 35 is pivoted by a bolt 38 or the like to an arm 39, which in turn is pivoted through another bolt 40 to an anchor plate 41 fixed to the inner face of the main wheel rim 19.
Bifurcated extensions 42 of each arm 39 straddle a web 43 of the shoe element 35 and engage ledge surfaces 44 of the shoe element to restrict pivoting of the shoe element 35 on the arm 39 carrying it.
Basically, the three brake shoe devices 34 are free-swinging on their pivots 40 with the anchor plates 41. The spacing of the devices 34 on the wheel 11 is such that there will always be contact between one of the devices 34 and the drum sector 23.
For releasing the anti-rollback brake shoe devices 34 at proper times so that a chair occupant can propel the chair rearwardly, cables 45 are connected between the spokes 13 of the lost motion mechanism and the devices 34. More particularly, corresponding ends of the cables 45 are secured within cable connectors 46 on the spokes 13 by clamping set screws 47. The connectors 46 are secured to the spokes 13 at 48, somewhat inwardly of the spoke crossheads 16, FIG. 5. The other ends of cables 45 are connected to top extensions 49 of shoe elements 35 by connector elements 50. The cables are thus attached to the elements 35 above their articulation axes 38 with the arms 39.
In the operation of the wheelchair in a forward mode, FIG. 2, the shoe elements 35 merely drag lightly over the friction facing 24 of drum sector 23. In this mode, the brake shoe devices 34 assume angled relationships to the drum sector, FIG. 2, and the two pivot elements 38 and 40 are out of alignment radially of the wheel 11. The devices 34 do not impede normal forward propulsion of the wheelchair by use of the propulsion ring 12 by its occupant.
If the chair is being propelled forwardly up an incline, each time manual pressure on the rings 12 is released, the anti-rollback devices 34, one of which is always passing over the drum sector 23, become activated automatically and assume the positive locking positions relative to the drum sector 23 as shown in FIG. 3, without the requirement for any activity by the chair occupant. The tendency for reverse movement of the chair on the incline forces the friction lining 36 into tight locking engagement with facing 24, FIG. 3, and the two pivot elements 38 and 40 move closer to a radial dead center relationship. The extensions 42 of pivoted arms 39 now bear solidly on the ledges 44 of shoe elements 35. The devices 34 now securely lock the chair wheel 11 against backward rotation on the incline. The slight angularity of the devices 34 from the true radial and the action of the extensions 42 on the pivoted shoe elements 35 prevent the devices 34 from swinging beyond or through their locking positions shown in FIG. 3 under the tendency of the chair to roll rearwardly.
When the chair occupant at any time wishes to propel the chair rearwardly by use of the propulsion rings 12, the lost motion connection between the ring 12 and wheel 11 afforded by the spokes 13 and associated parts including the slots 17 is sufficient to tension cables 45, as shown in FIG. 4. At all other times, these cables are slack, as shown in FIGS. 2 and 3. Under tension, the cables 45 acting on extensions 49 of shoe elements 35, in effect, break the toggle joint between the arms 39 and shoe elements 35 through their pivots 38. This action relieves the pressure of the linings 36 on friction facing 24 and enables the taut cable to elevate the particular device 34 clear of the drum sector 23, FIG. 4, the device 34 turning on its pivot axis 40 under influence of the cable 45. Thus, the particular device 34, which is in frictional locking engagement with the drum sector 23, is released so that the chair can be propelled rearwardly by its occupant. Upon resumption of forward propulsion of the chair or stopping of the chair, the device 34 will automatically assume its inactive or non-locking position of FIG. 2. However, the next time that undesired rearward movement of the chair tends to begin, as on an incline, the anti-rollback mechanism will automatically return to the active position of FIG. 3 to prevent backward rolling of the chair. As in the prior referenced application, the chair occupant need never remove his or her hands from the rings 12, risking momentary loss of control of the wheelchair. The anti-rollback mechanism is simple, comparatively lightweight, reliable in operation, and is composed of inexpensive components which are adaptable to mass production methods.
In FIGS. 6 through 8, a modification of the invention is depicted. In these figures, one piece brake shoe locking elements 51 having arcuate friction linings 52 are pivoted at 53 to anchors 54 fixed to the rim of chair wheel 11. The same three spoke lost motion mechanism between the chair wheel 11 and manual propulsion ring 12 previously described is employed, and essentially the same circularly curved brake drum sector 55 having a friction facing 56 is attached to the wheelchair frame.
In lieu of the previously-described cable release means for the articulated devices 34, each locking element 51 has a rigid arcuate link 57 adjustably secured thereto by a bolt 58 engaging through an adjusting slot 59 of the link to form a pivotal connection. An arcuate lost motion slot 60 provided in the link 57 receives slidably therethrough a bolt 61 or the like on the spoke 13.
FIG. 7 depicts the anti-rollback mechanism according to the modification in a mode whereby the wheelchair can be propelled forwardly by use of the manual rings 12 in a normal manner, with each locking element 51 being dragged lightly across the friction facing 56 of drum sector 55.
A retractile spring 62 is connected between one end of each link 57 and one wire spoke 63 of the chair wheel 11. During forward propulsion of the chair, the springs 62 are not stretched and exert no restraining force on or through the links 57.
However, when the occupant consciously propels the chair in a reverse mode through use of the manual rings 12, the described lost motion connection through the spokes 13 and associated parts will stretch or tension the springs 62 and the bolts 61 of spokes 13 will move to the ends of slots 60, following which the pivoted locking elements 51 are turned on their pivots 53 and swing out of engagement with the fixed drum sector 55, FIG. 8, to enable conscious rearward propulsion of the chair. Upon stopping of the chair or resumption of its forward movement, the springs 62 are relaxed and the parts return automatically to their normal free forward propulsion positions shown in FIG. 7.
The modified anti-rollback mechanism operates automatically on an incline or the like to resist chair rollback in substantially the identical manner previously-described in connection with the prior embodiment of the invention. In each embodiment, a lost motion connection between the wheel 11 and propulsion ring 12 is utilized in conjunction with a simple over center release linkage or mechanism to lift pivoted anti-rollback devices out of contact with the brake drum sector.
It is to be understood that the forms of the invention herewith shown and described are to be taken as preferred examples of the same, and that various changes in the shape, size and arrangement of parts may be resorted to, without departing from the spirit of the invention or scope of the subjoined claims. | The customary side hand propulsion ring adjacent to each main wheel of a manual wheelchair is mounted through a lost motion connection between the propulsion ring and main wheel so that the propulsion ring can have limited rotational movement relative to the main wheel. A friction brake drum or partial drum fixed to the wheelchair frame inside of the main wheel is engaged by at least one of a plurality of circumferentially spaced over center friction locking devices pivotally held on the main wheel. Each over center friction locking device is moved by a release element to a non-locking position relative to the drum or partial drum in response to reverse movement of the propulsion ring by a chair occupant. Economy and ease of operation are provided for. The wheelchair occupant need not remove his or her hand from the propulsion ring when operating the anti-rollback mechanism. | 0 |
TECHNICAL FIELD
[0001] The present invention relates to an electromagnetic valve, in particular for slip-controlled motor vehicle brake systems.
BACKGROUND OF THE INVENTION
[0002] DE 43 39 305 A1 discloses an electromagnetic valve of binary operation for use in a slip-controlled motor vehicle brake system, the valve closure member of which remains either in a closed or a fully opened switch position in relation to the valve seat. To avoid the undesirable switching noise of the electromagnetic valve, a hydraulically operated switching piston is arranged in the electromagnetic valve, switching into a position that throttles the valve passage when a defined pressure difference is reached. The effort in construction entailed for noise reduction by hydraulically throttling the pressure fluid is significant.
[0003] In view of the above, it is an object of the invention to improve an electromagnetic valve of the indicated type to the effect that the above-mentioned shortcoming is avoided.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] FIG. 1 is a total view of an electromagnetic valve of the type concerned for use in a slip-controlled brake system.
[0005] FIG. 2 is a diagram for plotting the brake pressure variation and the current variation for the electromagnetic valve according to FIG. 1 .
[0006] FIG. 3 is another diagram for plotting an alternative brake pressure and current variation for the electromagnetic valve according to FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0007] FIG. 1 shows a total view of an electromagnetic valve normally open in its basic position and designed as a two-way/two-position directional seat valve, comprising a cartridge-type valve housing 8 including a spherical valve closure member 9 at a stepped valve tappet 1 . Valve tappet 1 is in contact with a cylindrical magnet armature 10 at the opposite frontal end of the valve closure member 9 . The valve closure member 9 points to a tubular valve seat member 2 , while the oppositely disposed magnet armature 10 faces the magnet core 11 integrated in the valve housing 8 . Fastened to the magnet core 11 is a preferably deepdrawn sleeve 12 in which the magnet armature 10 can align itself and move in an axial direction. A magnet coil 13 is arranged at the periphery of sleeve 12 and is embedded between a yoke-type metal sheet 16 and a magnetic plate 17 .
[0008] In a per se known fashion, the magnet armature 10 moves in the direction of the magnet core 11 during energization of the magnet coil 13 so that the valve closure member 9 shaped at the valve tappet 1 interrupts the pressure fluid connection between a pressure fluid inlet and a pressure fluid outlet channel 14 , 15 that is normally open in the basic position, in opposition to the effect of a valve spring 4 interposed between the valve tappet 1 and the valve seat member 2 .
[0009] The electromagnetic valve is meant for use in slip-controlled motor vehicle brake systems, and its valve closure member 9 cooperating with the magnet armature 10 is lifted in the basic position from the valve seat member 2 by means of the valve spring 4 that is arranged between the valve tappet 1 and the valve seat member 2 . In the electrically energized valve position, the valve closure member 9 moves in the direction of the valve seat member 2 , and the magnet armature 10 moves in the direction of the magnet core 11 . The special feature is that the magnet coil 13 is energized by means of three different switching current values I 1 , I 2 , I 3 for reducing the valve switching noise. In the electrically non-energized condition of the magnet coil 13 , the first switching current value I 1 =0 so that the valve closure member 9 is completely opened due to the valve spring 4 . In the condition partly energized by means of the second switching current value I 2 which is higher than the first switching current value I 1 but lower than the third switching current value I 3 , the valve closure member 9 opens a throttle cross-section at the valve seat member 2 . To be able to keep this throttle position, it needs a defined geometric design of the valve seat member 2 and the valve tappet 1 . Valve closure member 9 at the valve tappet 1 has a preferably spherical contour with a diameter of 1.8 to 2.2 millimeters for this purpose. This corresponds to a sealing diameter at the valve seat of 0.9 to 1.1 millimeters. The valve seat angle amounts to 120 degrees herein.
[0010] In the fully energized condition, the electromagnetic valve is closed by the effect of the third switching current value I 3 . This permits noise reduction without structural modification of the electromagnetic valve.
[0011] A tandem master cylinder is connected as a brake pressure generator 3 to the pressure fluid inlet channel 14 of the electromagnetic valve illustrated in FIG. 1 . At the level of valve spring 4 , the pressure fluid outlet channel 15 of the electromagnetic valve is connected to a wheel brake 5 . Connected to said pressure fluid connection that leads to wheel brake 5 is a return line provided with an outlet valve 7 and including a low-pressure accumulator 18 and a pump 19 according to the return delivery principle. Said return line is connected to the pressure fluid inlet channel 14 . The illustrated hydraulic circuit is of a principal nature and serves for general explanations. Deviations herefrom are possible.
[0012] Based on the electrically non-energized condition I 1 of the magnetic coil 13 in which the electromagnetic valve is initially completely open, as shown in the drawings, in a brake pressure control operation the electromagnetic valve is principally switched into a fully energized condition I 3 where it is completely closed. Subsequently, it is opened electrically only in part (condition I 2 ) for noise reduction, and it is switched to re-assume the completely closed condition I 3 only subsequently. Details regarding the control sequence are referred to in the description relating to FIG. 2 .
[0013] The valve spring 4 is preferably configured as a helical spring and has a progressive spring characteristic curve, the spring force of which is rated so that the valve closure member 9 remains in the partly opened, noise-reducing switching position when the magnet coil 13 adopts its condition partly energized with the second switching current value I 2 .
[0014] For illustrating the hydraulic pressure difference applied to the valve closure member 9 in the partly opened switching position, a means is provided sensing the hydraulic pressure that prevails upstream and downstream of the valve closure member 9 . It is of great significance to determine the pressure difference as exactly as possible by way of appropriate means because in the partly opened condition of the electromagnetic valve, the electric switching current value I 2 that is necessary for the partial opening of the electromagnetic valve will no longer be sufficient to keep the electromagnetic valve open starting from a defined pressure difference.
[0015] As a means for sensing the hydraulic pressure difference, e.g. pressure sensors 6 are well suited that are connected to the brake circuit upstream and downstream of the valve closure member 9 . The pressure sensor signals representative of the pressure difference at the valve closure member 9 are evaluated in an electronic controller 20 actuating the magnet coil 13 .
[0016] According to the illustrated pattern, the electromagnetic valve is inserted into a brake pressure line of a slip-controlled motor vehicle brake system connecting the brake pressure generator 3 to the wheel brake 5 so that alternatively to the pressure sensing by means of pressure sensors 6 , the pressure difference can be sensed by appropriate software in a characteristic field for a pressure model, for what purpose the electronic controller 20 actuating the magnet coil 13 is appropriate. The pressure model represents the pressure variation in the wheel brake 5 and in the brake pressure generator 3 . Advantageously, it is possible to dispense with the comparatively expensive pressure sensor equipment by using the pressure model.
[0017] The pressure model representative of the pressure variation in the wheel brake 5 is computed based on the vehicle-related and brake-specific parameters. Among these parameters is data relating to the vehicle deceleration, the pilot pressure in the brake pressure generator, and the brake pressure increase and brake pressure decrease characteristics. The calculation of the pressure model for the brake pressure generator 3 takes into account the number of the brake pressure increase pulses and/or the duration of the brake pressure increase pulses necessary to complete the desired brake pressure increase by actuating the magnet coil 13 . Further, the pressure model for the wheel brake 5 is included in the calculation of the pressure model for the brake pressure generator 3 .
[0018] FIG. 2 shows a diagram in which, along the ordinate, the brake pressure variation for a slip-controlled wheel brake 5 (cf. FIG. 1 ) and the three different switching current values I 1 , I 2 , I 3 of the electromagnetic valve known from FIG. 1 are plotted as a function of time t. The pressure variation rising linearly from the zero point of the axes of coordinates initially represents the slip-free brake pressure increase initiated by the brake pressure generator 3 because the electromagnetic valve is non-energized (I 1 =0). When the allowable brake pressure value (points A-B) is reached and maintained, the magnetic coil 13 is energized by means of the switching current value I 3 that is higher than the switching current values I 1 , I 2 , with the result that the valve closure member 9 adopts its closed position. Simultaneously, the outlet valve 7 connected to the wheel brake 5 (cf. FIG. 1 ) is switched into the open position so that a rapid pressure reduction commences in wheel brake 5 until point C. After an initially steep pressure reduction, there will be a short phase where the pressure in wheel brake 5 is maintained constant after the closing of outlet valve 7 due to the closed position of the valve closure member 9 , until the reduction of the switching current value I 3 to the switching current value I 2 (point D) that reduces the valve noise. By energizing the magnet coil 13 with a switching current value I 2 , the valve closure member 9 will adopt a throttled position so that the pressure rise in the wheel brake 5 up to point E takes place with a lower pressure rise gradient. Following is a pressure-maintaining phase, to what end the magnet coil 13 is again energized with the maximum switching current value I 3 , with the result that the valve closure member 9 moves to sit on the valve seat member 2 . For the purpose of further throttled pressure increase in the wheel brake 5 , the switching current value I 3 of the magnet coil 13 is reduced in point F to the noise-reducing switching current value I 2 , what causes a further throttled pressure rise until point G. Until point H, a pressure-maintaining phase will follow due to the increase of the electric current of I 2 to the switching current value I 3 . Due to the new reduction of the energization of the magnet coil 13 to the switching current value I 2 , a continued throttled, low-noise pressure rise takes place until point J, which corresponds to the maximum brake pressure value (cf points A, B). Due to the energization of the magnet coil 13 with the switching current value I 3 , the valve closure member 9 will adopt the closed switch position again so that a pressure-maintaining phase follows until point K. When the maximum brake pressure value causes inadmissible brake slip, the outlet valve 7 allows a quick pressure reduction in the wheel brake 5 until point L is reached, which is again succeeded by a phase where the pressure is maintained constant and a phase of throttled pressure increase.
[0019] The brake pressure control operation described herein is based on a so-called current ramp actuation of the electromagnetic valve, whereby lower pressure increase gradients are achieved due to the throttling in the electromagnetic valve, which gradients permit reducing the valve noise and the pedal pulsation during brake pressure control.
[0020] Instead of the initially proposed electromagnetic valve that acts as an inlet valve for a brake system and adopts three different switch positions for noise reduction and minimizing the pedal pulsations with three different current values I 1 , I 2 , I 3 , an electromagnetic valve is disclosed to solve the object at issue (based on the valve construction shown in FIG. 1 ). The magnet coil 13 of said valve is operated with one single switching current value I 1 in such a fashion that the electromagnetic valve is never closed completely in the electrically energized condition of the magnet coil 13 , but always remains slightly opened so that a pressure fluid connection with a throttle is established between the valve seat 2 and the valve closure member 9 for noise reduction. Consequently, the idea is based on a permanent leakiness at the valve seat member 2 during the energization of the magnet coil 13 with the switching current value I 1 so that the valve closure member 9 will never provide complete sealing at the valve seat member 2 . Consequently, the idea is based on a permanent leakage at the valve seat member 2 during energization of the magnet coil 13 with the switching current value I 1 so that the valve closure member 9 will never fully seal at the valve seat member 2 . This obviates the need for a complicated actuation of the electromagnetic valve and thereby minimizes the valve noise and the pedal pulsations, without detrimental influence on brake pressure control in which the outlet valve 7 is to be included.
[0021] In this respect, FIG. 3 shows a diagram in which the brake pressure variation for a slip-controlled wheel brake 5 (cf FIG. 1 ) and the switching current value I 1 of the electromagnetic valve known from FIG. 1 are plotted along the ordinate as a function of time.
[0022] The pressure variation linearly rising from the zero point initially represents the slip-free brake pressure increase initiated by the brake pressure generator 3 because the electromagnetic valve is non-energized (I=0). When the allowable brake pressure value (point A) is reached, the magnet coil 13 is energized with the switching current value I 1 , with the result that the valve closure member 9 assumes its throttled position. In addition, the outlet valve 7 connected to wheel brake 5 (cf FIG. 1 ) is switched to adopt its open position so that a rapid pressure reduction commences in wheel brake 5 until point B. After an initially steep pressure reduction, there will be a flat pressure rise in the wheel brake 5 after the outlet valve 7 has closed on account of the throttled position of the valve closure member 9 , until the interruption of the partial current value I 1 (point C). Due to the effect of valve spring 4 , the valve closure member 9 moves from its throttled into the fully open valve switching position, with the result that the pressure gradient rises between points C-D. As soon as the magnet coil 13 is again energized with the partial current value I 1 (point D), the valve closure member will again assume its throttled position, with the result that the further pressure rise in the direction of point E occurs with a flat gradient again. When the pressure reduction phase in wheel brake 5 sets in by the outlet valve 7 customary in slip-controlled brake systems opening, the pressure will drop rapidly until the point F of the characteristic curve because the amount of fluid penetrating the outlet valve 7 is of course considerably greater than in the narrowest throttle cross-section of the electromagnetic valve that acts as an inlet valve. When the outlet valve re-adopts its closed position, the pressure in wheel brake 5 will rise slightly corresponding to the throttled position of the valve closure member 9 until point G. When the energization of the magnet coil 13 is interrupted in point G, the electromagnetic valve will switch back into the unthrottled open position, and a rapid pressure increase takes place in wheel brake 5 until point H. When the electromagnetic valve again switches into the throttled position due to the partial current value I 1 , the flat pressure rise in wheel brake 5 will repeat. Thus, moderation of the valve noise and the pedal pulsations is ensured by the low pressure increase gradients. | The present invention relates to an electromagnetic valve, which is electrically switched to adopt a throttled position in brake pressure control for reducing valve switching noises. | 1 |
FIELD OF THE INVENTION
[0001] The invention relates generally to the field of digital image processing and, more particular to a method for using multiple recomposed versions of the input digital image to improve scene classification.
BACKGROUND OF THE INVENTION
[0002] Automatically determining the semantic classification (e.g., sunset, picnic, beach) of an arbitrary image is a difficult problem. Much research has been done recently, and a variety of classifiers and feature sets have been proposed. The most common design for such systems has been to use low-level features (e.g., color, texture) and statistical pattern recognition techniques. Such systems are exemplar-based, relying on learning patterns from a training set (see A. Vailaya, M. Figueiredo, A. Jain, and H. J. Zhang, “Content-based hierarchical classification of vacation images”, Proceedings of IEEE International Conference on Multimedia Computing and Systems, 1999). Such exemplar-based systems are in contrast to model-based systems, in which the characteristics of classes are specified directly using human knowledge, or hybrid systems, in which the model is learned.
[0003] Semantic scene classification can improve the performance of content-based image organization and retrieval (CBIR). Many current CBIR systems allow a user to specify an image and search for images similar to it, where similarity is often defined only by color or texture properties. This so-called “query by example” has often proven to be inadequate. Knowing the category of a scene a priori helps narrow the search space dramatically. For instance, knowing what constitutes a party scene allows us to consider only party scenes in our search to answer the query “Find pictures of Mary's birthday party”. This way, the search time is reduced, the hit rate is higher, and the false alarm rate is expected to be lower.
[0004] Current scene classification systems enjoy limited success on unconstrained image sets. What are the reasons for this? The primary reason appears to be the incredible variety of images found within most semantic classes. Exemplar-based systems must account for such variation in their training sets. Even hundreds of exemplars do not necessarily capture all of the variability inherent in some classes. Take the class of sunset images as an example. Sunset images captured at various stages of the sunset can vary greatly in color, as the colors tend to become more brilliant as the sun approaches the horizon, and then fade as time progresses further. The composition can also vary, due in part to the camera's field of view: does it encompass the horizon or the sky only? Where is the sun relative to the horizon? Is the sun centered or offset to one side?
[0005] A second reason for limited success in exemplar-based classification is that images often contain excessive or distracting foreground regions, which cause the scene to look less prototypical and thus not match any of the training exemplars well. For example, FIG. 1 shows four scenes (a)-(d) with distracting foreground regions. This is especially true in consumer images, where the typical consumer pays less attention to composition and lighting than would a professional photographer. Therefore, consumer images contain greater variability, causing the high performance (on professionally-taken stock photo libraries such as the Corel database) of many existing systems to decline when used in this domain.
[0006] Consequently, a need exists for a method that overcomes the above-described issues in image classification. These issues are addressed by introducing the concept of spatial image recomposition, designed to minimize the impact of undesirable composition (i.e., foreground objects), and of simulated or effective temporal image recomposition, designed to minimize the effects of color changes occurring over time.
[0007] This approach is supported by past success in other domains. In face recognition and detection, researchers used perturbed versions of faces in training (e.g., see H. Rowley, S. Baluja, and T. Kanade, “Rotation invariant neural network-based face detection”, Proceedings of IEEE Conference on Computer Vision and Pattern Recognition, 1998) in order to handle geometric variation. This is related to resampling or bootstrapping. In addition, bagging (bootstrap aggression) uses multiple versions of a training set to train a different component classifier and the final classification decision is based on the vote of each component classifier (see R. O. Duda, P. E. Hart, and D. G. Stork, Pattern Classification . John Wiley & Sons, New York, 2001, pp. 475-476).
SUMMARY OF THE INVENTION
[0008] The present invention is directed to overcoming one or more of the problems set forth above. Briefly summarized, according to one aspect of the present invention, the invention resides in a method for improving image classification of a digital image comprising the steps of: (a) providing an image; (b) systematically recomposing the image to generate an expanded set of images; and (c) using a classifier and the expanded set of images to determine an image classification for the image, whereby the expanded set of images provides at least one of an improved classifier and an improved classification result.
[0009] The present invention provides a method for either (or both) systematically generating recomposed versions of an exemplar image to generate an expanded set of training exemplars to derive a robust classifier, or systematically generating recomposed versions of a testing input digital image to generate an expanded set of testing images with the same salient characteristics to derive a robust image classification result. This has the advantage of increasing the diversity of training exemplars, allowing better match of an image with exemplars, and providing a method of obtaining more robust image classification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIGS. 1 ( a )- 1 ( d ) show four examples of sunset images with distracting foreground regions.
[0011] FIGS. 2 ( a )- 2 ( d ) show a series of images exemplifying how an arbitrary image (a) is transformed into one (d) that better matches a prototypical exemplar.
[0012] FIGS. 3 ( a )- 3 ( c ) show an example of spatial recompositions, where original image (b) can be transformed by a horizontal mirroring (a) or a crop (20% from bottom as shown on (c)).
[0013] FIGS. 4 ( a )- 4 ( f ) show an example of temporal recomposition comprising a series of illuminant shifts.
[0014] FIGS. 5 ( a ) and 5 ( b ) show typical examples of false positives induced by using spatial recomposition.
[0015] FIGS. 6 ( a )- 6 ( f ) show examples of how sunsets and false positives are processed when temporal recompositions are used, where the original (left images) and illuminant-shift (+6 buttons) images (right images) are shown. Note that the bottom image is one of the purposefully confusing images: A winter scene with the sun low in the horizon, but not setting.
[0016] [0016]FIG. 7 shows a table resolving independent recomposition decisions using voting where, e.g., “T10” means 10% cropped from the image top, and so on.
[0017] FIGS. 8 ( a )- 8 ( c ) show examples of sample testing images that gained by using recomposition according to the invention.
[0018] [0018]FIG. 9 is a diagram illustrating elements of a method for practicing the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0019] The present invention will be described as implemented in a programmed digital computer. It will be understood that a person of ordinary skill in the art of digital image processing and software programming will be able to program a computer to practice the invention from the description given below. The present invention may be embodied in a computer program product having a computer readable storage medium such as a magnetic or optical storage medium bearing machine readable computer code. Alternatively, it will be understood that the present invention may be implemented in hardware or firmware.
[0020] A large obstacle to high performance in semantic scene classification is the immense variety, both in terms of color and composition, of images in each class. Obtaining enough training data for an exemplar-based system can be a daunting task, especially when the classes contain many variations. Manually collecting large numbers of high-quality, prototypical images is time-consuming, even with the help of themed stock photo libraries. Therefore, it is critical to make efficient use of all available training data.
[0021] Furthermore, the best match of a testing image with the set of training exemplars occurs when the image matches an exemplar of its class, both in its color and its composition. However, the test image may contain variations not present in the training set. The degree of match is affected by the photographer's choice of what to capture in the image (affecting its composition) and when to capture the image (potentially affecting its color due to changes in the scene illuminant over time). If it were possible to “relive” the scene, one could attempt to obtain an image with more prototypical color and composition for the class. For instance, referring to FIGS. 2 ( a )- 2 ( d ), an original scene (FIG. 2( a )) contains a salient sub-region (FIG. 2( b )) which is cropped and re-sized (FIG. 2( c )). Finally, in FIG. 2( d ), an illuminant shift is applied, simulating a sunset occurring later in time. How can one “relive” the scene? In other words, how can one transform an arbitrary image into one that will match a prototypical exemplar better?
[0022] According to the invention, a concept called effective spatial and temporal recomposition is used to address the above issues. Image recomposition is generally defined as a process that systematically creates altered versions of the same image, including spatial composition and color composition. The different types and uses of spatial recomposition (mirroring and cropping images) and effective (simulated) temporal recomposition (shifting the color of images) are presented in Table 1 and will be elaborated in more detail below. They are categorized as recomposition in training, testing, and both. Some type-use combinations need visual inspection to ensure such recompositions do not destroy the integrity of the training examples (e.g., aggressive crop may result in the loss of the main subject of the picture).
TABLE 1 Types and Uses of Image Recomposition. Type Use Mirror Training Conservative crop Training, testing Aggressive crop Training (need inspection), testing Color shift Training (need inspection), testing
[0023] Recomposition in Training
[0024] Using recomposition on a limited-size set of training data can yield a much richer, more diverse set of exemplars. The goal is to obtain these exemplars without having to inspect each image visually. One technique is to reflect each image about the vertical axis, thereby doubling the number of exemplars. For instance, as shown in FIGS. 3 ( a )- 3 ( c ), the original image ( 3 ( b )) is transformed by a horizontal mirroring ( 3 ( a )) or a crop (20% from the bottom as shown in 3 ( c )). Clearly, the classification of the new image is unchanged; that is, while reflecting a sunset image with the sun on the left side of the image moves the sun to the right side, the image remains a valid sunset image.
[0025] Another technique is to crop the edges of an image. The assumption is that the salient portion of an image is in the center and imperfect composition is caused by distractions in the periphery. Cropping from each side of the image in turn produces four new images of the same classification. Of course, one does not want to lose a salient part of the image (such as the sun or the horizon line in a sunset), but for a conservative crop of a small amount, e.g., 10%, the semantic classification of a scene is highly unlikely to change, although the classification by an algorithm may change.
[0026] Recomposition in Testing
[0027] while recomposing the training set yields more exemplars, recomposing a test image and classifying each new, recomposed image yields multiple classifications of the original image. In terms of spatial recomposition, the edges of the image can be cropped in an attempt to match better the features of a test image against the exemplars. It may be necessary to crop more aggressively (as in FIG. 2) to obtain such a match. However, if the classifier has been trained using mirrored images, there is no need to mirror the test image due to symmetry already built into the classifier. For example, when using a 1-NN classifier, the feature vector, T, of a testing image will lie a certain distance from the nearest exemplar vector E. Call the vectors of the reflected images of E and T, E′ and T′, respectively. Due to symmetry in the features, d(E,T)=d(E′, T′), making T′ redundant.
[0028] Some classes of images contain a large variation in their global color distribution, and shifting the overall color of the test image appropriately can yield a better match with a training exemplar. Using the class of sunset images as an example, an early and a late sunset may have the same spatial distribution of color (bright sky over dark foreground), but the overall appearance of the early sunset is much cooler, due to a color change in the scene illuminant. By artificially changing the color along the illuminant (=red-blue) axis towards the warmer side, we can simulate the appearance of capturing the image later in time; we dub this illuminant shift an effective temporal recomposition. For example, as shown in FIGS. 4 ( a )- 4 ( f ), a temporal recomposition comprises a series of illuminant shifts in 3-button increments, starting from −6 buttons (FIG. 4( a )) and ending at +9 buttons (Figure (f)), where a button equals 0.4 of a photographic stop. Likewise, variation within the amount of illuminant in the scene can be handled using changes along the luminance axis. Color shift along other axes may be applicable in other problem domains.
[0029] Whether using spatial or temporal recomposition, the classifier may or may not label a new, recomposed image with the same class as the original image. How does one adjudicate when the classifications of the recomposed images differ? Duin (see R. P. W. Duin, “The combining classifier: To train or not to train?”, Proceedings of International Conference on Pattern Recognition, 2002) discussed two types of combiners, fixed and trained. Fixed combining rules include voting schemes and using the sum or average of the scores. A trained combiner is a second classifier for mapping the scores to a single score. Two considerations affect the choice of which to use: the availability of training data and the degree to which the base classifiers have been trained. Duin suggests that undertrained classifiers can benefit from a trained combiner, while those that are overtrained (e.g., support vector machines (SVMs)) cannot. In the present study, this was found to be the case (e.g., a second-stage SVM did not help).
[0030] In a two-class problem, one interesting fixed combiner of r recompositions is to use the m-th order statistic, e.g., the maximum (m=1), the second largest (m=2), or the median (m=r/2). Varying the parameter m moves the classifier's position on the operating curve. Small m classifies images positively in an aggressive manner, giving greater recall at the expense of more false positives. The choice of m will clearly depend on the application.
[0031] The scores can also be combined in such a way as to find the most consistent image classification. For instance, a voting scheme can be used for combination. This is desirable: classification based on a number of slightly varied recomposed images with the same salient scene content should be more robust than classification based on the original image alone. If the single classification based on the original image is incorrect due to some statistical anomaly (e.g. foreground distractions or poor spatial registration with the set of exemplars), yet many of the recomposed images are classified correctly, a majority rule will correct the anomaly.
[0032] Recomposition in Both Training and Testing
[0033] For some applications, recomposition may be used on both the training and testing data. Since each serves a different purpose, they may be combined readily. One may question the need for using both types of recompositions; namely, if one had a sufficiently rich set of training exemplars, why would recomposing the test image be necessary? The need to use recomposition in both training and testing is practical. There is no guarantee that the training data is diverse enough to begin with, or that recomposition in training exemplars has exhaustively created all possible variations and completely fills the image space.
[0034] A related question is the choice between recomposing training images and obtaining additional unique exemplars. Aside from the argument presented earlier about the lack of good training data, and the time necessary to gather it, there is also the question of the quality of the data available. Recomposing a small set of prototypical exemplars is likely to be more desirable than using more but lesser quality exemplars.
[0035] In addition, use of recomposition in testing on top of recomposition in training is certainly a way to boost recall if so desired, though potentially at the expense of a higher false alarm rate.
[0036] A last question is whether a more aggressive approach may be used in recomposing the training data so as to minimize the need to recompose the test data. Because aggressive recomposition can cause images to lose their salient content, one must ensure that the integrity of the expanded training set is not compressed; the discussion now turns to a technique for doing exactly this.
[0037] Semi-Supervised Recomposition in Training
[0038] Our goal in using conservative recompositions on the training set is to make the process completely unsupervised. However, if yet more training data is desired and aggressive recompositions, such as larger amounts of cropping or significant color shifts, are used, a training methodology is needed so that one does not need to go to the other extreme, that of inspecting every recomposed image.
[0039] Admittedly, because some aggressive recompositions can remove some scene content characteristic to the class of an image, a more rigorous approach to adding these images to the training data would be to visually inspect each of the recomposed training images. Doing so can be tedious and laborious. Only inspecting a subset of the recomposed images needing attention would be more efficient. In order to screen the recomposed images, one can train a classifier using the original training images and then classify the recomposed versions of the training images using this classifier. Only those recomposed images that fail (or pass with low confidence) the classifier need to be evaluated visually to determine if the recomposition has caused the image to lose salient scene content. Such recomposed images are then eliminated while the remaining recomposed images are added to the expanded training set to improve its richness. This is a preferred tradeoff between generating fewer recomposed images in an unsupervised manner and generating many recomposed images in a completely supervised fashion.
[0040] Next, three preferred embodiments of the present invention are described for sunset detection, outdoor scene classification, and automatic image orientation detection, respectively.
[0041] Sunset Detection
[0042] In the aforementioned hierarchical image classification scheme described by Vailaya et al., sunsets were easily separated from mountain/forest scenes. Color was found to be more salient for the problem than other features, such as edge direction alone, confirming an intuition that sunsets are recognizable by their brilliant, warm colors. Furthermore, spatial information should be incorporated to distinguish sunsets from other scenes containing warm colors, such as those of desert rock formations. Therefore, spatial color moments may be used, dividing the image into 49 regions using a 7×7 grid and computing the mean and variance of each band of a Luv-transformed image. This yields 49×2×3=294 features.
[0043] A Support Vector Machine (SVM) is preferably used as the classifier because SVMs have been shown to give higher performance than other classifiers such as Learning Vector Quantizers (LVQ) on similar problems (See, for example, B. Scholkopf, C. Burges, and A. Smola, Advances in Kernel Methods: Support Vector Learning , MIT Press, Cambridge, Mass., 1999, pp. 263-266, and Y. Wang and H. Zhang, “Content-based image orientation detection with support vector machines,” Proceedings of IEEE Workshop on Content - Based Access of Image and Video Libraries, 2001). In particular, a Gaussian kernel was used, creating an RBF-style classifier (RBF=Radial Basis Function, see Wang and Zhang). SVMs are designed for two-class problems, and output a real number for each testing image. The sign is the classification and the magnitude can be used as a loose measure of the confidence.
[0044] Using recomposition in the training set increased performance significantly, presumably because the set was much richer. This overcomes some of the effects of having a limited training set. Using recompositions in the testing set increased both the number of hits and the number of false positives. Finally, using recompositions in both training and testing gave the best results overall. Note that these results correspond to optimal operating points on different curves.
[0045] Using spatial recomposition on the testing images met the goal of correctly classifying sunset images with large distracting foreground regions: for example, the images presented in FIG. 1 were all classified incorrectly by the baseline system, but correctly when recomposition was used (gained by recomposition). The image (b) on the upper right is a good example of how recomposition by cropping can help. Cropping the large, dark, water region in the foreground from the image increases the SVM score substantially. The other images fared similarly: for example, cropping the bottom 20% from the bottom left image (a) eliminates the confusing reflection in the water.
[0046] However, the number of false positive images also increased, partially offsetting the gain in recall. Typical false positives induced by recomposition are shown in FIGS. 5 a and 5 b . Each of these images contains patterns not typical of sunsets (e.g., the multiple bright regions in the night image, or the sky in the desert image), which when cropped out, make the image appear to be much more sunset-like.
[0047] Some sunset images have prototypical composition, but weak colors, corresponding to early or late sunsets. Shifting the scene illuminant “warms up” these images, causing them to be classified correctly, but also introduces many false positives, both of which are shown in FIG. 6.
[0048] Outdoor Scene Classification
[0049] The above system is extended to distinguish between six types of outdoor scenes: beach, sunset, fall foliage, field, mountain, and urban (defined in Table 2). The images used for training and testing included Corel and consumer images. The same features and classifier are used as for the sunset detector, although the SVM classifier was extended to multiple classes by using a one-vs.-all approach (see B. Scholkopf, C. Burges, and A. Smola. Advances in Kernel Methods: Support Vector Learning . MIT Press, Cambridge, Mass., 1999 , pp 256-258). Spatial recomposition was especially effective when used in training, since the training set was still limited. Recomposition was not used on the testing set.
TABLE 2 Definitions of six outdoor scene classes Class Definition Beach At least 5% each of water, sand, and sky Sunset Illuminant source in front of camera Fall foliage Detectable color in turned leaves on tree Field No aerial view, not cluttered with trees (“open”) Mountain Open, whole mountains, mid-range view, Less than 90% snow or fog-covered Urban At least one building, no extreme perspectives
[0050] Image Orientation Detection
[0051] The goal of automatic image orientation detection (see Y. Wang and H. Zhang, “Content-based image orientation detection with support vector machines”, Proceedings of IEEE Workshop on Content - Based Access of image and Video Libraries, 2001) is to classify an arbitrary image into one of four compass directions (N, S, E, W), depending on which direction the top of the image is facing. Doing so based on image content alone is a difficult problem. For the preferred embodiment, a baseline system uses spatial color moments and a one-vs.-all SVM classifier, which is similar and achieves similar results to that in Wang et al.
[0052] Recomposition in testing can be expected to improve classification in this domain as well, but the rationale for using it is much different: cropping the edges of an image should not affect the perceived orientation of the image. Therefore, the combined classification based on a number of slightly different images should be more robust than that of a single image. Experimenting with both fixed (voting) and trained combiners, the performance of each was found to be comparable; voting was chosen for its simplicity.
[0053] In this application, an image is classified with four scores, each coming from a SVM tuned to recognize images of a given orientation. The one-vs.-all classifier classifies the image with the orientation corresponding to the SVM that yields the maximum score. This process is repeated nine times, once for each cropped version of the image. The process finally votes among the nine classifications, using the scores to break ties (although a tie means no single orientation dominated and that the image is a good candidate for rejection, i.e., no apparent orientation). An example of the voting scheme is given in FIG. 7.
[0054] Sample Corel images that were gained by using the recomposition scheme are shown in FIG. 8. In each of these cases, some region on the border of the image is distracting. The dark shadows (FIG. 8( c )), the dark trees (FIG. 8( b )), and the reflection of the sun (FIG. 8( c )) all confused the classifier; bright or dark regions appear at the side of an image, not at the top or bottom.
[0055] Image recomposition is similar in spirit to bootstrapping or bagging methods, with a major distinction being that only a single classifier is trained and used in classification. The key to successful application of this scheme to an image classification problem is that such image recomposition would only affect the distractive components in the image in such a way that they can be discounted in the final classification and the salient content is invariant to such perturbation to the image. Thus, this is a general approach to boosting classification performance as long as appropriate ways of recomposition are selected according to the domain of problem and the features/classifier used.
[0056] The following guidelines are offered to help decide how to use image recomposition in image classification. First, if the training set is sparse, using conservative spatial recompositions can help greatly. More aggressive recomposition, both spatial and temporal, should be done in a semi-supervised manner. In a two-class problem, recomposing the test image can cause a better match with an exemplar of the same class, giving an operating curve parameter that can be used to customize the performance to the application. In a multi-class problem, voting among the classifications of recomposed images is more robust. Clearly, in the ideal case where classes are well separated in training data and testing images match the exemplars well, recomposition is not expected to help much.
[0057] [0057]FIG. 9 shows a diagram of the method for improving the scene classification of a digital image according to the invention. Initially either an input exemplar image 10 or an input test image 12 is provided in an input stage 14 and then applied to a recomposition stage 16 , where the input image is systematically recomposed according to either a spatial recomposition algorithm 18 or a temporal recomposition algorithm 20 (or both), as described heretofore in the detailed description of the invention. The result of the recomposition is an expanded set of images 22 , which depending on the type of input image (exemplar or test image) will be an expanded set of exemplar images 24 or an expanded set of test images 26 (or both). If the expanded set of images are exemplar images, they are used to train the classifier in a training stage 28 , thereby providing an improved classifier according to the invention. If the expanded set of images are test images, they are used in a classifier stage 30 , thereby providing an improved image classification result according to the invention. As indicated by the broken line 32 connecting the training stage 28 and the classification stage 30 , the improved classifier resulting from the expanded set of exemplar images 24 may be used together with the expanded set of test images 26 to provide an overall improved classification result. However, it is also possible to apply the recomposition stage 16 in only one of the two paths shown in FIG. 10 (i.e., either in training an improved classifier or in providing an improved image classification result, but not both).
[0058] The subject matter of the present invention relates to digital image understanding technology, which is understood to mean technology that digitally process a digital image to recognize and thereby assign useful meaning to human understandable objects, attributes or conditions and then to utilize the results obtained in the further processing of the digital image.
[0059] Scene classification can also find application in image enhancement. Rather than applying generic color balancing and exposure adjustment to all scenes, the adjustment could be customized to the scene, e.g., retaining or boosting brilliant colors in sunset images while removing warm-colored cast from tungsten-illuminated indoor images.
[0060] The recomposition technique described by the present invention is not limited to photographic images. For example, spatial recomposition can also be applied to medical images for medical image classification (although color recomposition does not apply).
[0061] The invention has been described in detail with particular reference to certain preferred embodiments thereof, but it will be understood that variations and modifications can be effected within the spirit and scope of the invention.
Parts List
[0062] [0062] 10 input exemplar image
[0063] [0063] 12 input test image
[0064] [0064] 14 input stage
[0065] [0065] 16 recomposition stage
[0066] [0066] 18 spatial recomposition algorithm
[0067] [0067] 20 temporal recomposition algorithm
[0068] [0068] 22 expanded set of images
[0069] [0069] 24 expanded set of exemplar images
[0070] [0070] 26 expanded set of test images
[0071] [0071] 28 training stage
[0072] [0072] 30 classification stage
[0073] [0073] 32 broken line | A method for improving scene classification of a digital image comprising the steps of: (a) providing an image; (b) systematically recomposing the image to generate an expanded set of images; and (c) using a classifier and the expanded set of images to determine a scene classification for the image, whereby the expanded set of images provides at least one of an improved classifier and an improved classification result. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a rudder propeller with an underwater transmission having a planetary gearing, the planetary gearing including a sun gear, a stationary ring gear, and planet gears mounted between the sun gear and ring gear and supported on planetary axles of a planet carrier.
2. Discussion of Related Art
Rudder propellers of the type mentioned above are known, for example, from German Patent Reference DE 28 43 459 A1. The rudder propeller is used to drive and control a watercraft. The engine torque of a drive motor, which is usually situated inside the watercraft, is transmitted by an above-water transmission via a drive shaft extending vertically downward to an underwater transmission, which usually includes an angle drive and a subsequent planetary gearing, from which the engine torque is finally transmitted to the horizontally extending propeller shaft, which supports the propeller. In order to control the watercraft, the underwater transmission is situated in a housing that can be rotated around the vertical axis.
Inside the planetary gearing, which reduces the speed of the drive motor, such as to a speed suitable for the propeller shaft, the roller bearing mounting of the planet gears that is standard in the prior art is critical because during operation of the rudder propeller, the bearings are subjected to significant loads, in particular alternating loads. The roller elements of the roller bearing mountings used therefore cannot run in optimal fashion and are susceptible to wear. Consequently, there are known proposals to use multilayer roller bearings in lieu of the roller bearing mountings of the planets on the planet axles, but this mounting is very cost-intensive.
SUMMARY OF THE INVENTION
One object of this invention is to avoid disadvantages of the known rudder propeller and to ensure an increased service life and fault tolerance of such a rudder propeller at a relatively low cost and with a relatively simple assembly.
In order to attain the above object and others, according to this invention, the design of a rudder propeller with the features, advantageous embodiments and modifications are described in this specification and in the claims.
This invention proposes supporting the planet gears on the planet axles by hydrodynamic plain bearings so that an overall width of the planet gears and their maximum diameter can be used, resulting in greater rigidity, longer service life, and reduced wear.
The properties of the hydrodynamic bearings, which usually function with a lubricating oil, permit an extremely smooth and wear-free continuous operation of such a planetary gearing, which is easy to manufacture.
Because the coefficient of friction in hydrodynamic plain bearings is a function of the speed, such as the relative speed between the sliding surfaces, it transitions from a static friction at rest through a mixed friction at a low speed, to the desired fluid friction of the lubricating film at a sufficiently high speed. Because marine propulsion systems such as rudder propellers are usually operated at a particular nominal speed or within only a limited speed range, the hydrodynamic plain bearing according to this invention can be calibrated to this speed range.
In order to overcome the mixed friction that is typical for low speeds when starting the rudder propeller and when slowing it to a stop and also when operating at changing speeds, such as when maneuvering, this invention proposes that the planet axles have supply conduits for a lubricant, extending from an infeed opening to the hydrodynamic plain bearing. It is thus possible in these speed ranges, in which static or mixed friction is present, to supply lubricant with a suitable pressure to the hydrodynamic plain bearing in order to facilitate the transition to the desired fluid friction.
According to one embodiment of this invention, this exertion of pressure via the supply conduits can either be implemented by the already provided lubrication system of the rudder propeller or separate lubricant pumps for this purpose. The control can be carried out in a speed-dependent way by a corresponding control unit of the rudder propeller. As soon as the speed range in which fluid friction predominates due to the prevailing relative speed between the sliding surfaces has been reached, the supply of lubricant via the supply conduits can be switched off since it is no longer required at this point in time.
According to one embodiment of this invention, the supply openings are connected to a common feeder conduit for the lubricant provided in the planet carrier so that they communicate with one another. This produces a central lubricant supply inside the planet carrier, which branches into all of the planet axles for the individual planet gears extending from the planet carrier. A planetary gearing includes at least two, preferably three such planet gears together with planet axles.
The pressure of the lubricant that can be exerted in order to facilitate the starting and stopping of the planetary gearing, for example which lies in a relatively low pressure range of a few bar, which can be easily implemented with the existing or already provided lubrication system of the rudder propeller.
On their outer surface oriented toward the planet gear, the hydrodynamic plain bearings are advantageously embodied with a circumferential groove into which the supply conduits feed so that the lubricant film can form directly around the hydrodynamic plain bearing.
In order to achieve the most compact, easy-to-assemble structural unit, the planet axles are inserted, preferably shrink-fitted, into corresponding receiving bores on an end surface of the planet carrier.
According to another embodiment of this invention, the planet gears are supported on the planet axles in cantilevered fashion by the hydrodynamic plain bearings so that it is possible to use the entire tooth width of the planet gears to transmit force.
In another embodiment of this invention, the planet gears are secured to the planet axle on a side oriented away from the planet carrier by a thrust washer to prevent them from shifting axially.
BRIEF DESCRIPTION OF THE DRAWINGS
Other details and embodiments of this invention are explained in greater detail below in view of the drawings, which show one exemplary embodiment, wherein:
FIG. 1 shows a detail view of a planetary gearing according to this invention; and
FIG. 2 shows an underwater transmission of a rudder propeller according to the prior art.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 2 shows a schematically simplified view of the underwater transmission of a rudder propeller according to the prior art.
From a drive motor, which is not shown and is situated above water, a drive shaft 10 that is supported by bearings 100 , 9 extends in a vertical direction and inside the underwater transmission shown, ends at a pinion that engages with a bevel gear 8 and together with the latter, forms an angle drive. The bevel gear 8 is supported on a horizontally extending propeller shaft 1 , which supports a propeller at one end which is not shown in the drawing. A clutch 7 connects the bevel gear 8 to a sun gear 6 of a planetary gearing. The remaining components of the planetary gearing are a planet carrier 2 with a plurality of planet axles 3 protruding from one end face, roller bearings 5 a mounted thereon for supporting planet gears 5 , and a fixed ring gear 4 . The fixed ring gear 4 is mounted in a manner that is not shown, for example to the housing of the underwater transmission. On the other hand, the planet carrier 2 is shrink-fitted onto the propeller shaft 1 so that the speed of the drive shaft 10 , after being redirected by the bevel gear 8 , is reduced in speed by the planetary gearing and the propeller shaft 1 is driven at this reduced speed.
The rolling support on the roller bearings 5 a of the planet gears 5 used in the exemplary embodiment shown in FIG. 2 is very susceptible to wear due to the alternating loads that occur.
In the embodiment according to this invention as shown in FIG. 1 , a hydrodynamic plain bearing 50 is mounted on each planet axle and supports the planet gear 5 on the planet axle 3 .
The planet axle 3 is shrink-fitted into a corresponding receiving bore 21 of the planet carrier 2 and supply conduit 30 for a lubricant initially extending axially from an infeed opening 300 , which then branches off at right angles and leads to a groove 500 embodied on the outer surface of the hydrodynamic plain bearing 50 .
The infeed opening 300 of the supply conduit 30 communicates with a feeder conduit 20 provided in the planet carrier 2 so that it is possible for a lubricant pump, not shown in detail, for example the usual lubricant pump that is provided inside the underwater transmission, to supply a flow of lubricant via the feeder conduit 20 into the individual supply conduits 30 , which is explained in greater detail below.
On the side oriented away from the planet carrier 2 , the hydrodynamic plain bearing 50 and the planet gear 5 supported on it are secured by a thrust washer 51 to prevent them from shifting axially on the planet axle 3 .
The drawing also shows a part of the housing 12 of the underwater transmission and an accompanying housing cover 120 , which jointly fix the ring gear 4 of the planetary gearing.
During operation of a thusly designed underwater transmission for a rudder propeller, when at a standstill, there is a static friction between the plain bearing 50 and the planet gear 5 supported on it. If the rudder propeller is then to be set into operation, for example, the drive shaft 10 and the subsequent parts of the underwater transmission are to be set into rotation, then first, a corresponding control command of the rudder propeller control unit pushes a flow of lubricant with a pressure of a few bar, for example, up to 3 bar, via the feeder conduit 20 to the adjoining supply conduits 30 into the circumferential groove 500 of the hydrodynamic plain bearing 50 in order to rapidly overcome the mixed friction that occurs inside hydrodynamic plain bearings 50 at low speeds. As soon as the mixed friction, which decreases with increasing speed, transitions into the fluid friction that is typical for the hydrodynamic plain bearing, the flow of lubricant and the exertion of pressure with the lubricant via the feeder conduit 20 and the supply conduit 30 are switched off, so that the pumping action achieves the lubricant film required for the bearing on the surfaces of the hydrodynamic plain bearing 50 and planet gear 5 and for this reason, the planet gear rotates in a virtually wear-free fashion and using the entire tooth width between the fixed ring gear 4 and the sun gear 6 .
In addition to the above-explained lubricating oil support during the startup of the planetary gearing, such a lubricating oil support can also be activated by the corresponding control unit when bringing the system to a stop, for example, when reducing the speed from the range in which fluid friction predominates. | A rudder propeller with an underwater mechanism including a planetary gearing, the planetary gearing including a sun gear, a fixed internal gear and planetary gears, mounted between the sun gear and the internal gear and running on planetary axles of a planet carrier, wherein the planetary gears are mounted on the planetary axles by hydrodynamic slide bearings. | 5 |
TECHNICAL FIELD
[0001] The technical field generally relates to hood assemblies for vehicles, and more particularly to a hood assembly capable of rapidly elevating the hood of the vehicle for the protection of pedestrians.
BACKGROUND
[0002] Legal requirements with respect to pedestrian protection in the event of an accident with a motor vehicle are evolving. In order to decrease the consequences of injuries in the event of an impact of the pedestrian's head on the hood of a vehicle, it is desirable that the pedestrian (or his/her head) be slowed down as gradually as possible, for instance, by allowing a deformation of the hood. There must, however, be a sufficiently large space below the hood for such deformation. However, providing a large space between the hood and the underhood components can bring negative consequences into the design and performance of the vehicle (e.g., reduced aerodynamic efficiency, reduced visual appeal, reduced fuel efficiency or reduced outward visibility). To avoid the large space under the hood of the vehicle, devices are needed for automatically raising the hood in the event of an impact (or detected impending impact) to increase the distance between the hood and the engine allowing more hood deformation to occur.
[0003] Accordingly, it is desirable to provide a hood elevation feature for a vehicle. Also, it is desirable to provide a rapid hood elevation feature that facilitates the hood being re-latched so that the vehicle may be driven after an impact. Additionally, other desirable features and characteristics of the present disclosure will become apparent from the subsequent description taken in conjunction with the accompanying drawings and the foregoing technical field and background.
BRIEF SUMMARY
[0004] In accordance with exemplary embodiments, a hood elevation system is provided for a vehicle. The system comprises a first member configured to be coupled to a body member within an engine compartment of a vehicle. Also included is a second member configured to be coupled to a hood latch of the vehicle, and is also coupled to the first member in a first position. The second member is releasably slideable away from the first member to a second position upon activation of an actuator. In this way, the hood latch is elevated by the actuator moving the second member (and the hood latch) to the second position to elevate the hood of the vehicle.
[0005] In accordance with exemplary embodiments, a hood elevation method is provided for a vehicle. The method comprises activating (via a controller) an actuator coupled to a first member, which causes the actuator to release and slide a second member relative to the first member, the second member is coupled to a hood latch engaging a hood of a vehicle to elevate the hood responsive to the controller detecting a condition.
DESCRIPTION OF THE DRAWINGS
[0006] The subject matter will hereinafter be described in conjunction with the following drawing figures, wherein like numerals denote like elements, and:
[0007] FIG. 1 is an illustration of a vehicle suitable for using exemplary embodiments of the present disclosure;
[0008] FIG. 2 is an illustration of one embodiment of a hood latch elevation mechanism suitable for use with the hood latch assembly of FIG. 1 ;
[0009] FIG. 3 is a rear illustration of FIG. 2 ;
[0010] FIG. 4 is an illustration of the hood latch elevation mechanism of FIG. 2 including a hood latch member;
[0011] FIG. 5 is a magnified partial view of FIG. 3 illustrating the re-latch feature of the hood latch elevation mechanism according to one embodiment;
[0012] FIG. 6 is a illustration of another embodiment of a hood latch elevation mechanism suitable for use with the hood latch assembly of FIG. 1 ;
[0013] FIG. 7 a magnified partial view illustrating the latch release and re-latch feature of the hood latch elevation mechanism of FIG. 6 ; and
[0014] FIG. 8 is an illustration of the hood latch elevation mechanism of FIG. 6 in the separated (hood elevated) position.
DETAILED DESCRIPTION
[0015] The following detailed description is merely exemplary in nature and is not intended to limit the subject matter of the disclosure or its uses. Furthermore, there is no intention to be bound by any expressed or implied theory presented in the preceding technical field, background, brief summary or the following detailed description.
[0016] In this document, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Numerical ordinals such as “first,” “second,” “third,” etc. simply denote different singles of a plurality and do not imply any order or sequence unless specifically defined by the claim language.
[0017] Additionally, the following description refers to elements or features being “connected” or “coupled” together. As used herein, “connected” may refer to one element/feature being directly joined to (or directly communicating with) another element/feature, and not necessarily mechanically. Likewise, “coupled” may refer to one element/feature being directly or indirectly joined to (or directly or indirectly communicating with) another element/feature, and not necessarily mechanically. However, it should be understood that, although two elements may be described below, in one embodiment, as being “connected,” in alternative embodiments similar elements may be “coupled,” and vice versa. Thus, although the schematic diagrams shown herein depict example arrangements of elements, additional intervening elements, devices, features, or components may be present in an actual embodiment.
[0018] Finally, for the sake of brevity, conventional techniques and components related to vehicle electrical and mechanical parts and other functional aspects of the system (and the individual operating components of the system) may not be described in detail herein. Furthermore, the connecting lines shown in the various figures contained herein are intended to represent example functional relationships and/or physical couplings between the various elements. It should be noted that many alternative or additional functional relationships or physical connections may be present in an embodiment of the invention. It should also be understood that FIGS. 1-7 are merely illustrative and may not be drawn to scale.
[0019] Referring to the drawings, wherein like reference numbers refer to like components, FIG. 1 shows a vehicle 10 suitable for use with the exemplary mechanical embodiments of the present disclosure. The vehicle 10 may be any one of a number of different types of vehicle, such as, for example, a sedan, a wagon, a truck, or a sport utility vehicle (SUV), and may be two-wheel drive (2WD), four-wheel drive (4WD), or all-wheel drive (AWD). The vehicle 10 may also incorporate any one of, or combination of, a number of different types of engines, such as, for example, a gasoline or diesel fueled combustion engine, a flex fuel vehicle (FFV) engine (i.e., using a mixture of gasoline and alcohol), a gaseous compound (e.g., hydrogen and/or natural gas) fueled engine, a combustion/electric motor hybrid engine, and an electric motor.
[0020] The vehicle 10 includes a hood 12 that provides closure to a front compartment. In some embodiments, the vehicle engine, powertrain and other components reside in the front compartment. In embodiments having a mid or rear mounted engine, the front compartment may house other components such as spare tires, batteries, etc. Typically, the hood 12 is attached to the vehicle body with at least one, preferably a pair of, laterally spaced hinges 14 . The hood 12 is held in a closed position (shown in solid lines) by a striker (not shown) coupled to the hood engaging a hood latch assembly 16 . In some embodiments the hood 12 has hinges 14 mounted to its rearward portion (as illustrated) with a latch mounted in the forward portion. Alternately, the hood 12 can be configured having the hinges 14 mounted in the forward portion of the hood and latch(es) mounted in the rearward portion. According to exemplary embodiments, a sensor 18 is positioned to detect an impending or actual impact (such as with a pedestrian) and a controller 20 then activates (via conductor 22 ) a hood latch elevation mechanism (not shown in FIG. 1 ) of the hood latch assembly 16 to rapidly elevate or raise the hood to a partly open position 24 (shown in dashed lines). The controller 20 may be any one of a variety of controllers typically found on modern vehicles, such as an engine controller or may be a separate controller dedicated to the hood latch assembly 16 . The controller 20 is programmed to analyze the sensor 18 data and determine if one or more conditions indicative of an impending risk of vehicle impact under the predetermined conditions exists. Elevation of the hood 12 creates more space between the hood and the underhood components (not shown) of the vehicle 10 , which facilitates a more gradual deceleration of the pedestrian (or other obstacle) by allowing the hood to deform and absorb energy. According to exemplary embodiments discussed in more detail below, the hood 12 may be released by operation of an actuator that comprises a pyrotechnic or gas actuator that can rapidly elevate the hood 12 to the partly open position 24 .
[0021] Referring now to FIG. 2 , there is shown an illustration of one embodiment of a hood latch elevation mechanism 30 that in various embodiments of the present disclosure forms a supporting part of the hood latch assembly ( 16 in FIG. 1 ). The hood latch elevation mechanism 30 includes a first member 32 that is attached to a vehicle body member (e.g., tie bar) via fasteners 34 . A second member 36 is coupled to the first member 32 by destructible fasteners 38 (e.g., aluminum rivets). The second member 36 includes attachment points 40 where a hood latch may be attached to the hood latch elevation mechanism 30 as part of the hood latch assembly ( 16 in FIG.1 ). The first member 32 also includes guide pins 42 that are configured in slots 44 in the second member 36 . In normal operation, the first member 32 and the second member 36 are held in a coupled arrangement via destructible fasteners 38 , facilitating the hood ( 12 in FIG. 1 ) to be latched or unlatched as desired by an operator of the vehicle 10 .
[0022] However, as illustrated in FIG. 3 , in the event of an impending or detected collision, an actuator 46 is activated by the controller ( 20 in FIG. 1 ) via conductor 22 causing a rapid release and separation of the second member 36 from the first member 32 . The force of the actuator 46 is sufficient to sufficiently deform destructible fasteners 38 and driving the second member 36 slideably away from the first member 32 to become separated as permitted by the guide pins 42 and slots 44 .
[0023] Accordingly to exemplary embodiments, the actuator 46 can be configured to activate upon a determination by the controller ( 20 in FIG. 1 ) that a set of predetermined conditions has been met. The actuators 46 may activate upon the sensor ( 18 in FIG. 1 ) sensing an impact with the vehicle body or determining that the possibility of impact with the vehicle is greater than a predetermined amount (e.g., such as upon sensing an object in the vicinity of the vehicle 10 or upon rapid deceleration of the vehicle). In the latter arrangement, the sensor 18 monitors the environment near the front of the vehicle 10 and provides data representing the vehicle's environmental conditions the controller 20 .
[0024] FIG. 4 is an illustration of the hood latch elevation mechanism 30 , wherein like reference numbers refer to like components in previous figures, and includes an attached hood latch 50 of convention construction with an integrated secondary release apparatus 54 and secondary release lever 52 . As will be appreciated, since the hood latch 50 is coupled to the second member 36 at the attachment points 40 , the hood latch is elevated with the second member 36 and the hood ( 12 in FIG. 1 ). Given that the destructible fasteners 38 have been destroyed, the hood cannot be returned to a closed position and remains in the partly open position with a re-latch apparatus.
[0025] Referring now to FIG. 5 , a magnified partial view of FIG. 3 illustrates a re-latch apparatus useful with exemplary embodiments of the hood latch elevation mechanism 30 . In operation, the re-latch apparatus includes of a spring member 56 that pivots about a post 58 , a pintle latch 60 coupled to the second member 36 via a post 62 , and two guide pins 64 and 66 . Prior to elevation, the spring member 56 is held out of the locking position by guide pin 64 . During elevation (that is, activation of the actuator 46 ), the pintle latch 60 and guide post 64 are also elevated since they are attached to the second member 36 . The post-elevation absence of guidepost 94 releases the spring 56 such that it rotates about post 58 until one end 64 of the spring member 56 contacts a positioning member 70 . With this arrangement, the hood ( 12 in FIG. 1 ) may be re-latched via the vehicle operator pushing down on the hood surface over the latch. This action moves the hood, the hood striker, hood latch, the second member 36 and pintle 60 in a downward direction toward the first member 32 . As the ramped surface pintle 60 contacts the end 68 of the spring member 56 , the end 68 rotates away from positioning member 70 . When the pintle 60 is moved below the end 68 of the spring member 56 , the end 68 rotates back toward the positioning member 70 engaging the post 62 , which retains the hood in a closed (or near closed) position. This allows the vehicle to be driven (if not too damaged) to a service center for repairs and replacement of this embodiment of the hood latch assembly ( 16 in FIG. 1 ).
[0026] FIG. 6 illustrates an alternate embodiment of the hood latch elevation mechanism 30 , wherein like reference numbers refer to like components in previous figures. In this embodiment the first member 32 and the second member 36 are coupled by releasable latches 80 that also comprise the re-latch member in this embodiment.
[0027] FIG. 7 is a magnified partial illustration of the hood latch elevation mechanism 30 , wherein like reference numbers refer to like components in previous figures. When the actuator 46 is activated by the controller ( 20 in FIG. 1 ), a tab 82 coupled to the actuator 46 engages pins 84 of the latches 80 pushing them back to release the second member 36 from the first member 32 just as the actuator begins activation. As the actuator continues to activate, the force of the actuator (e.g., explosive force from a pyrotechnic cartridge), separates the second member 36 from the first member 32 causing the second member 36 to slide linearly away from the first member 32 via the guide pins 42 and arrangement of the slots 44 (see, FIG. 5 ). The resulting separation 90 is illustrated in FIG. 8 , which in some embodiments may be approximately thirty to forty millimeters, although other separation distances are possible. In the embodiment of FIGS. 6-8 , since the latches 80 are opened and not destroyed, the hood ( 12 in FIG. 1 ) may be closed merely by pushing the hood down to the closed position, where the latches 80 will re-couple the first member 32 to the second member 36 (see FIG. 5 ). Once the hood is re-latched, the vehicle may be driven (if not too damaged) to a service center for repairs and replacement of this embodiment of the hood latch assembly ( 16 in FIG. 1 ).
[0028] Accordingly, a hood elevation feature is provided for a vehicle. The exemplary embodiments of the disclosed hood elevation feature also facilitate the hood being re-latched so that the vehicle may be driven after an impact. Moreover, exemplary embodiments of the hood elevation feature may also be applied to other hood elements, such as, for example, the hinges ( 14 in FIG. 1 ) so that they may also elevate by attaching the hood hinges to the attachment points 40 of the various disclosed embodiments.
[0029] While at least one exemplary embodiment has been presented in the foregoing summary and detailed description, it should be appreciated that a vast number of variations exist. It should also be appreciated that the exemplary embodiment or exemplary embodiments are only examples, and are not intended to limit the scope, applicability, or configuration of the disclosure in any way. Rather, the foregoing summary and detailed description will provide those skilled in the art with a convenient road map for implementing the exemplary embodiment or exemplary embodiments. It should be understood that various changes can be made in the function and arrangement of elements without departing from the scope of the disclosure as set forth in the appended claims and the legal equivalents thereof. | A hood elevation system and method are provided for a vehicle. The system includes a first member configured to couple with a body member within an engine compartment of a vehicle and a second member configured to couple with a hood latch of the vehicle and the first member. The second member is releasably slideable away from the first member upon activation of an actuator. In this way, the hood latch is elevated by the actuator moving the second member to elevate the hood of the vehicle. The method includes activating (via a controller) an actuator coupled to a first member, causing the actuator to release and slide a second member relative to the first member, the second member coupled to a hood latch engaging a hood of a vehicle to elevate the hood responsive to the controller detecting a condition. | 1 |
BACKGROUND OF THE INVENTION
In a fixed vane or rolling piston rotary compressor, the discharge port is in the motor end bearing. The discharge port is located such that about half of it overlies the piston bore and the remainder overlies the cylinder. The portion of the cylinder overlain by the discharge port is recessed to provide a fluid path from the cylinder bore to the discharge port. Accordingly, the discharge port faces the piston bore and recess. To provide a smooth flow path, the entrance to the discharge port is normally chamfered.
The discharge port is exposed to the compression chamber during the entire compression and discharge cycles. However, flow, other than that associated with the reduction in volume during the compression cycle, does not take place until the pressure in the compression chamber is sufficient to open the discharge valve against any bias and system pressure acting on the discharge valve and tending to keep it closed. It follows that there is normally a significant registration between the compression chamber and the discharge port at the time of opening of the discharge valve.
SUMMARY OF THE INVENTION
Although there is a significant registration between the compression chamber and the discharge port of a rolling piston rotary compressor, it has been determined that providing a streamlined port geometry influences the turbulent energy generated in the gas pulse through the valve port. There is evidence that this energy excites the valve stop at its resonance frequency. A notch is provided in the motor end bearing at the entrance to the discharge port. The notch is aligned with the direction of the discharge valve centerline and is located on the side of the discharge port corresponding to the pivoted end of the discharge valve. Accordingly, the notch provides a smooth transition for flow from the compression chamber to the discharge port. Additionally, the notch tends to direct the flow towards the free end of the valve, thereby providing a less circuitous path. Since the notch is localized, it does not unnecessarily add to the clearance volume.
It is an object of this invention to reduce the pressure drop across the discharge valve.
It is an additional object of this invention to reduce flow noise associated with gas pulsation through a valve port.
It is another object of this invention to minimize the additional clearance volume.
It is a further object of this invention to provide a smooth transition for the discharge flow. These objects, and others as will become apparent hereinafter, are accomplished by the present invention.
Basically, a notch is provided in a portion of the motor end bearing at the entrance to the discharge port such that flow is directed through the discharge port in a streamlined manner and towards the free end of the discharge valve.
BRIEF DESCRIPTION OF THE DRAWINGS
For a fuller understanding of the present invention, reference should now be made to the following detailed description thereof taken in conjunction with the accompanying drawings wherein:
FIG. 1 is a vertical sectional view of a rolling piston compressor taken through the suction structure;
FIG. 2 is a sectional view taken along line 2--2 in FIG. 1;
FIG. 3 is a partial, vertical sectional view corresponding to that of FIG. 1 but taken through the discharge structure which is the subject matter of this invention;
FIG. 4 is a pump end view of the motor bearing;
FIG. 4A is an enlarged view of a portion of FIG. 4;
FIG. 5 is a view corresponding to that of FIG. 4 but with the shaft, piston and vane added;
FIG. 6 is a sectional view taken along line 6--6 of FIG. 4;
FIG. 7 is a view corresponding to FIG. 6 showing a first modified embodiment; and
FIG. 8 is a view corresponding to FIG. 6 showing a second modified embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIGS. 1-3, the numeral 10 generally designates a vertical, high side rolling piston compressor. The numeral 12 generally designates the shell or casing. Suction tube 16 is sealed to shell 12 and provides fluid communication between suction accumulator 14, which is connected to the evaporator (not illustrated), and suction chamber S. Suction chamber S is defined by bore 20-1 in cylinder 20, piston 22, pump end bearing 24 and motor end bearing 28.
Eccentric shaft 40 includes a portion 40-1 supportingly received in bore 24-1 of pump end bearing 24, eccentric 40-2 which is received in bore 22-1 of piston 22, and portion 40-3 supportingly received in bore 28-1 of motor end bearing 28. Oil pick up tube 34 extends into sump 36 from a bore in portion 40-1. Stator 42 is secured to shell 12 by shrink fit, welding or any other suitable means. Rotor 44 is suitably secured to shaft 40, as by a shrink fit, and is located within bore 42-1 of stator 42 and coacts therewith to define an electric motor. Vane 30 is biased into contact with piston 22 by spring 31.
Referring to FIG. 3, discharge port 28-2 is formed in motor end bearing 28 and partially overlies bore 20-1 and overlies discharge recess 20-3 which is best shown in FIG. 2 and which provides a flow path from compression chamber C to discharge port 28-2. Discharge port 28-2 is serially overlain by discharge valve 38 and spaced valve stop 39, as is conventional. As described so far, compressor 10 is generally conventional. The present invention adds notch 28-3A which is best shown in FIGS. 3-6. In FIG. 3 the view of notch 28-3A is that seen when looking in the direction of the axis of valve 28 towards the fixed end of valve 28. Notch 28-3A is a more extensively recessed portion of chamfer 28-3, as best shown in FIG. 4A, and has a projected profile that has a curved shape that intersects with the discharge port 28-2 or, preferably, with the discharge port chamfer 28-3. Notch 28-3A is symmetrical with the axis of the discharge valve 38. Notch 28-3 can be 10° to 180° in circumferential extent, but is preferably 90° or less, and corresponds, in part, to a portion of discharge port 28-2 overlying bore 20-1, or, more specifically, compression chamber C. As best shown in FIG. 5, where the piston 22 and vane 30 are 180° in the cycle from the FIG. 2 position and where the discharge cycle has ended and the suction cycle is ending, the notch 28-3A mostly overlies cylinder 20 but because of its limited circumferential extent it does not significantly add to the clearance volume. Notch 28-3A is located, however, where at least some of the flow from compression chamber C to discharge port 28-2 would otherwise be over a 90° edge with attendant losses. As best shown in FIG. 6, the valve 38 is flexed on opening and has its greatest distance from valve seat 28-4 and hence the least resistance to flow on the side of discharge port 28-2 opposite to notch 28-3A. Accordingly, flow passing through notch 28-3A tends to be diverted to a limited degree such that the flow tends to go diagonally across port 28-2 with only a glancing impingement on valve 38 and passing past the tip of valve 38. This should be contrasted with a flow straight through port 28-2 such that it directly impinges upon valve 38 and is directed, in part, to the sides of valve 38 and requiring a subsequent 90° change in flow direction.
In operation, rotor 44 and eccentric shaft 40 rotate as a unit and eccentric 40-2 causes movement of piston 22. Oil from sump 36 is drawn through oil pick up tube 34 into bore 40-4 which acts as a centrifugal pump. The pumping action will be dependent upon the rotational speed of shaft 40. Oil delivered to bore 40-4 is able to flow into a series of radially extending passages, in portion 40-1, eccentric 40-2 and portion 40-3 to lubricate bearing 24, piston 22, and bearing 28, respectively. Piston 22 coacts with vane 30 in a conventional manner such that gas is drawn through suction tube 16 and passageway 20-2 to suction chamber S. The gas in suction chamber S is trapped, compressed and discharged from compression chamber C via a flow path defined by notch 28-3A and recess 20-3 into discharge port 28-2. The high pressure gas unseats the valve 38 and passes into the interior of muffler 32. The compressed gas passes through muffler 32 into the interior of shell 12 and passes via the annular gap between rotating rotor 44 and stator 42 and through discharge line 60 to the condenser 70 of a refrigeration circuit (not illustrated).
At the completion of the compression process, the direction of motion of piston 22 will be tangent to the bore 20-1, in the region of recess 20-3 or, nominally, as shown in FIG. 5. The clearance volume will be the volume of recess 20-3, the volume of discharge port 28-2, the volume of chamfer 28-3, and the volume of the material removed to form notch 28-3A. Accordingly, the increase in the clearance volume is minimized due to the reduced circumferential extent of notch 28-3A.
Referring now to FIG. 7, a modified discharge port 128-2 is disclosed. Port 128-2 differs from port 28-2 by the addition of a second flow guiding surface 128-3B located across port 128-2 from notch 128-3A. Notch 128-3A and guiding surface 128-3B coact to provide a streamlined flow and to guide the flow in a direction along the axis of valve 138 such that the flow tends to glance off valve 138 and flow past the tip of valve 138.
Referring now to FIG. 8, a second modified discharge port 228-2 is disclosed. Discharge port 228-2 is circular but formed at an angle in motor end bearing 228 such that flow through port 228-2 is directed towards the free end of valve 238. The angle of port 228-2 effectively forms an inlet notch and a discharge notch when port 228-2 is viewed straight on.
Although the present invention has been illustrated and described in terms of a vertical, variable speed compressor, other modifications will occur to those skilled in the art. For example, the invention is applicable to both horizontal and vertical compressors using discharge valves. Similarly the motor may be a variable speed motor. It is therefore intended that the present invention is to be limited only by the scope of the appended claims. | A notch is provided in the motor end bearing of a rotary compressor in the region of the discharge port. The notch enhances the flow by smoothing the flow path and guiding the flow so as to impinge upon the discharge valve in a glancing manner and reduces the noise from the valve and valve stop and from the turbulent flow through the discharge port. The notch is located along the axis of the discharge valve and on the side of the valve port on which the valve is pivoted. | 5 |
PRIORITY CLAIM
[0001] The present application claims benefit of the filing date of the U.S. provisional patent application Ser. No. 60/461,102 filed Apr. 8, 2003.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to an apparatus for handling carpet. More specifically, this invention relates to an apparatus for unloading a carpet roll or rolled other materials from a transport vehicle at a job site where heavy unloading equipment and lifts are generally unavailable. The carpet unloading apparatus enables one or more individuals to handle rolls of carpet without the excessive lifting and straining generally associated with such work.
[0004] 2. Description of the Prior Art
[0005] Rolls of carpeting are commonly very large, bulky and heavy. Therefore, to manually handle these rolls is very strenuous, tiring and undesirable, as well as a potential cause of back injuries or muscle strain. Unfortunately, the type of heavy equipment usually associated with handling carpet rolls is generally unavailable at a job site where carpet in being installed. Thus, leaving a burdensome task to the individuals involved that has not been overcome by the numerous methodologies implemented to address carpet roll handling. In particular, none of the prior attempts satisfactorily provide for carpet roll handling at remote work sites.
[0006] U.S. Pat. No. 3,750,811 issued to Anderson discloses a carpet unloading and transporting assembly that comprises an elongate rectangular frame equipped with electric winches and cables. A support leg extending downward at each of the four corners supports this large frame. Each of these legs has a caster attached for mobility. The Anderson apparatus is placed at the rear of a transport vehicle where a cable is placed around a roll of carpet from outside the vehicle. Then, with another set of cables and a winch, the roll is lifted off the floor. The apparatus can then be rolled to another location in a warehouse carrying the carpet with it. While beneficial for its intended use, this equipment is specifically designed for a store or warehouse setting and is not suitable for relocation and use at a jobsite.
[0007] In another example, U.S. Pat. No. 2,702,139 issued to Faustine illustrates a similar apparatus to Anderson above that too is unsuitable for relocation. In yet another example, U.S. Pat. No. 4,396,166 issued to Kollman, provides an apparatus inside a closed-in cargo type trailer. This device consists of a closed-in trailer large enough to carry several rolls of carpet with a rear door through which the rolls can be pulled via an electric power winch mounted inside the trailer. Once the carpet is inside the trailer it can be suspended off the floor by a lifting mechanism mounted inside the trailer, then the end of the roll can be fed as it is unrolled through an opening in the side of the trailer long enough to allow the width of the carpet to pass through. This design allow for the carpet to be cut in lengths as needed while the remainder of the roll is suspended inside the vehicle. While this is a very impressive design, the cost factor would be so great as to render it unaffordable or impractical for many would be users.
[0008] Accordingly, a need exists for a carpet-unloading apparatus that remains with a transport vehicle so that it will be available when needed to unload a carpet roll or the like at a work site. It is also necessary that it be user-friendly, quick and easy to operate. It should also be relatively inexpensive and affordable enough for those who need it. This present invention will meet all these necessities.
BRIEF SUMMARY OF THE INVENTION
[0009] The present invention provides for a novel and unique user-friendly carpet unloading device, part of which will be removably attached and remain inside the vehicle to which it is assigned. The other parts are set up on the outside of the vehicle for use, after which they are folded together and stored in some small area until further needed.
[0010] The apparatus of the invention is small, lightweight and can be assembled into a folding arrangement or stored in very little space in the vehicle while being transported. It is light enough to enable one person to operate. It is relatively inexpensive to manufacture which makes it very affordable. It is very safe and requires very little physical strength to unload a roll of carpet.
[0011] With the use of this present invention, an operator is able to mechanically lift a roll of carpet, remove it from the vehicle and have it resting on an elongated tube, which extends lengthwise through the center of the roll. This tube is then supported on each end by a ridged pedestal or jack stand or combination thereof. This stand will hold the roll of carpet off the floor where it can be unrolled and cut into the desired lengths.
[0012] The present invention is comprised of a framework to be securely attached to the inside of the vehicle. This framework consists of, among other things, a series of columns, or posts that extend upward from the floor to near the top of the vehicle. These columns, or posts are designed to be adjustable in length and can be adjusted to the height of the vehicle in which they are installed. The size and number of these columns are determined by the length of the overhead rail and the weight they are to support. These columns are spaced apart one from another along the side and relative to the wall of the transport vehicle. Each column has a corresponding column of like configuration directly across the vehicle and relative to the opposite wall. Each of these columns has a corresponding cross-member that attaches at the top of teach column and extends in a cross direction toward the center of the vehicle. The cross-members are also adjustable in length and may be adjusted to the width of the vehicle in which it is installed. Each of these corresponding cross-members is then attached to an upper mounting bracket at the top center of the vehicle. Thus, when all these components are connected they make up a set of supports and form a structural arch across the vehicle. This is repeated as often as necessary to support the weight that is to be moved along the top rail.
[0013] The top rail is a long rail or track suspended from the bottom center of each upper mounting bracket via a tie rod or hanger. These tie rods or hangers should be constructed in a manner that will provide for the top rail to be made ridged to the supporting framework.
[0014] A trolley is placed on the rail. This trolley should be suitable for use on this rail and sufficient to move the load suspended beneath it with a relatively minimal amount of force. A hoist sufficient to lift, hold and lower the expected load is attached to the trolley and an attaching devise is lowered down to the load.
[0015] The device of the present invention provides for an adjustable length tube with a telescoping mechanism at one end and a shaft or portion of the tube extending outward from the other while holding a roll of carpet. This tube can be coupled together or separated at approximately center ways. In the outermost section of this tube is stored a slightly smaller and shorter length of similar tube. This inside tube can be extended out in various lengths and locked in place then inserted into the other section of the outer tube and locked in place on that end. This feature allows for the tube to be adjusted to proper length corresponding to the carpet being moved. This tube, when adjusted to the proper length and locked in place can be passed lengthwise through a roll of carpet. The telescoping mechanism of the tube can then be attached to the lower end of the hoist that is attached at the top to the trolley. In one embodiment, a shaft at the outermost end of this tube may be designed to pass through a collar mounted pilot bearing located near the top of a jack. This jack is easily affixed on a stand that is also equipped with large swivel casters that provides for the stand to be easily rolled in any direction while bearing the load of a roll of carpet. These casters are also provided with a locking brake that may be applied when movement is unsuitable. A second stand is also provided that is very similar to the first. The second stand may be provided with a removable jack and include large swivel casters like the first stand. In an alternative embodiment, the second stand may have a ridged pedestal that can be raised or lowered as desired, in lieu of a jack. The carpet roll will generally roll freely about the tube. As an enhancement, the pedestal may include rollers at the top for the tube to rest on once it has been removed from the vehicle. Thus, the tube is passed length ways through a roll of carpet then attached at the innermost end to the hoist and at the outer end to the jack that is affixed to a stand equipped with casters.
[0016] Now when the hoist is raised at one end, the jack at the other end of the roll will be lifted from the surface where it lay. After the roll has been lifted it can be easily pulled in an outwardly direction. At this time the jack stand that is on casters and the overhead trolley will begin to roll, thus removing the carpet from the vehicle. When the trolley reaches the outer limit of the rail, the trolley will stop. At this time the telescoping mechanism can be released. This will allow the roll to be pulled further out until the carpet is clear of the vehicle, then by lowering the hoist the tube can be lowered onto the second stand or jack. After carpet is lowered onto the second jack, the hoist can be disconnected from the telescoping mechanism. The telescoping mechanism can now be pushed back into the tube and the vehicle removed, or, because of the casters at each end of the carpet roll, the carpet roll may be removed to a more suitable location. Because this tube is resting on rollers at one end and a bearing at the other, or alternatively, lateral supports extending from the jack stands, carpet roll or tube may be easily rotated as the carpet is pulled off the roll. The casters can also be locked in position in order to hold the stands while the carpet is unrolled.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] [0017]FIG. 1 is a perspective view illustrating the present carpet unloading apparatus.
[0018] [0018]FIGS. 2 a , 2 b and 2 c are side plan views illustrating the operation of the present carpet unloading apparatus.
[0019] [0019]FIGS. 3 a , 3 b and 3 c are front plan assembly views illustrating the assembly of the support frame of the present invention.
[0020] [0020]FIG. 4 a is a perspective view illustrating the assembly of the overhead support rail of the invention and trolley system.
[0021] [0021]FIG. 4 b is a front side sectional view illustrating the assembly of trolley system of the present invention.
[0022] [0022]FIG. 5 is a side plan view illustrating the assembly of the carpet roll supporting tube, overhead rail, and hoist of the present invention.
[0023] [0023]FIGS. 6 a , 6 b and 6 c are side plan assembly views illustrating the assembly of the supporting tube of the invention, including telescoping members.
[0024] [0024]FIG. 7 is a side plan view illustrating an alternative embodiment of the present carpet unloading apparatus in an operative condition in which a carpet roll has been unloaded onto a pair of jack stands.
DETAILED DESCRIPTION OF THE INVENTION
[0025] Referring now to the drawings, FIG. 1 illustrates a preferred embodiment of the present invention. A carpet unloading apparatus for unloading a roll of material such as a carpet roll 10 from a transport vehicle 12 is provided comprising a support frame structure 14 , a carpet roll support tube structure 42 , and external means 50 and 58 for supporting a carpet roll via the carpet roll support tube structure once the carpet roll is removed from a vehicle. The support frame structure stands within a rear cargo bay 13 of the transport vehicle 12 and supports a trolley system 34 and hoist systems 36 that traverses along an overhead rail 26 to remove a carpet roll from the transport vehicle and place the carpet roll securely on the external support means.
[0026] More particularly, a removable and independent support frame structure 14 is provided having vertically oriented columns 16 for supporting the trolley system 34 and hoist systems 36 above a carpet roll 10 situated within the rear cargo bay 13 of the transport vehicle 12 . Several columns 16 L are located along the left sidewall of the vehicle, and several columns 16 R are located opposite left side columns along the right side wall of the vehicle. The columns 16 rest on the floor 18 of the vehicle 12 and are supported thereby, but not necessarily affixed to the vehicle. Ties or braces 17 attached from the floor, ceiling or sidewalls of the vehicle cargo bay 13 may further support the columns 16 . Sufficient columns 16 are provided to ensure adequate support of the very heavy carpet rolls 10 or the like to be handled by the apparatus. The columns 16 are placed very near to the sidewalls 22 , 24 of the vehicle in order to maximize the workspace provided about the carpet roll 10 stored within the rear cargo bay 13 .
[0027] The column members 16 as shown in FIGS. 1, 3 a and 3 c , are adjustable for height to fit into vehicle cargo bays 13 of varying heights. In particular, the columns 16 may comprise first column members 16 a R and 16 a L and second column members 16 b R and 16 b L. First column members 16 a R, 16 a L may have a smaller circumference that the second column members 16 b R, 16 b L for insertion of first column members into the second column members. Alternatively, a lower portion of the first column members 16 a R, 16 a L may be swedged or have reduced diameter for insertion into second column members 16 b R, 16 b L. Means for fixing the position of the first column members within the second column members is provided to fix the height of the column members 16 . As shown in FIG. 3 c , a bolt 19 may be inserted into an aperture in each second column member 16 b R, 16 b L and tightened to bear against the respective first column member 16 a R, 16 a L contained within the second column member such that the first column member will not slide and will remain in a fixed position.
[0028] The support frame structure 14 includes cross-members 28 that span from the left column members 16 L to the right column members 16 R to provide support above the carpet roll 10 . The columns 16 may have angled upper portions 21 to intersect and connect to the cross-members 28 . In one embodiment as illustrated in FIGS. 3 a and 3 b , the cross-members 28 comprise the angled portion 21 of the columns 16 , a pair of intermediate adjusting members 28 a , 28 b and a center connecting member 28 c , which may be slightly arched to fit the contour of a vehicle cargo bay 13 , increase vertical space available, and align each intermediate member 28 a , 28 b with the center connecting member 28 c and angled portions 21 of the columns 16 . Each intermediate adjusting member 28 a , 28 b connects the angled portion 21 of each respective column 16 to the center connecting member 28 c such that a single horizontal span across the cargo bay 13 of the vehicle 12 is created. The connection of the intermediate members 28 a , 28 b may be accomplished by providing a tubular receptacle on each end of the intermediate members that receives the respective ends of the columns 16 or center connecting member 28 c. Changing the amount of the column 16 or center connecting member 28 c that is inserted into the intermediate member receptacle may adjust the length of the span. Bolts 29 or affixing devices are provided for securing the intermediate members, and, thereby, defining the length of the cross-members 28 .
[0029] The cross-members 28 support a rail 26 , which runs lengthwise along the ceiling of the rear cargo bay 13 of the transport vehicle 12 . The depicted rail 26 comprises a long narrow angle iron situated with the ends 27 of the angle iron pointing downwards. The rail 26 is attached to the cross-members 28 by a tie rod 32 that hangs from the center of the cross-members, and a nut or other method is used to attach the rail to tie rod. The tie rod 32 provides for adequate spacing between the cross-members 28 and rail 26 for the provision of a trolley system 34 .
[0030] As shown in FIG. 5, the trolley system 34 may run along the lengthwise rail 26 via bearing wheels 34 a. An attaching device 34 b such as a bolt and nut combination attaches each bearing wheel 34 a above the ends 27 of the angle iron of the rail 26 and the bolt may provide a shaft for the bearing wheels to rotate about. The trolley system 34 further includes a short angle iron member 34 d with the ends pointing upwards for attachment of the bearing wheels 34 a above the rail 26 . The short angle iron member 34 d is suspended below the rail 26 by the bearing wheels 34 a and provides a support for a hoist and pulley system 36 a that may be attached to the short angle iron by an eye bolt 34 c attached thereto. The bearing wheels 34 a roll along the upper edge of the rail 26 and traverse the rail for movement of a supported carpet roll 10 or the like. Thus, the trolley system 34 may be attached to the end of the carpet roll 10 via a suitable device such as a cable 38 with hoist and pulley 36 a. The trolley 34 would support the carpet roll 10 at the end closest to the inward portion of the vehicle's rear cargo bay 13 . When the carpet roll 10 is removed from the vehicle's rear cargo bay 13 , the trolley system 34 allows the carpet roll to exit the rear of the vehicle 12 while the trolley moves toward the rear of the vehicle along the rail 26 . A hook or attaching device 40 connects the cable 38 to the end of tube that supports the carpet roll.
[0031] The elongate tube 42 shown in FIGS. 5 and 6 a , 6 b and 6 c may comprise a first square tube member 42 a and second square tube member 42 b having a connecting tube member 48 between them, a telescoping tube member 44 , and a shaft 46 . The connecting member 48 may be received by the respective open ends of the first and second square tube members 42 a , 42 b and secured between the tube members by set screws 45 or other securing mechanism such as spring loaded lock buttons. By loosening the setscrews 45 , the length of the elongate tube 42 may be varied according to the length of carpet roll 10 being transported and handled, such as 12 ft or 15 ft.
[0032] At the end of the elongate tube 42 that is positioned toward the inward portion of the vehicle's rear cargo bay 13 , the elongate tube is provided a telescoping tube member 44 . The telescoping tube member 44 may be housed partially within the walls of the second square tube member 42 b and extend from the end of the second square tube member to increase the overall length of the tube 42 . A first bearing member 47 at the inward end of the telescoping tube member 44 promotes the efficient telescoping of the telescoping tube member. The first bearing member 47 as shown includes a bearing wheel 49 rotationally attached to the inward end of the telescoping tube member 44 and contained within the square tube member 42 b. The bearing wheel 49 is situated between the inside corners of the square tube member 42 b , which creates a track for longitudinal movement of the wheel during the telescoping function of the telescoping tube member 44 , while limiting the latitudinal movement of the wheel. A second bearing member 51 at the end of the tube 42 and situated about the telescoping tube member 44 further supports and promotes efficient telescoping of the telescoping tube member. The second bearing member 51 is shown at the end of the tube 42 and is attached thereto. The telescoping tube member 44 rolls along the second bearing member when extended to telescope from the end of the tube.
[0033] The carpet roll 10 is removed from the vehicle's rear cargo bay 13 using the trolley system 34 . Before removal of the carpet roll 10 , a jack 50 supports the outward end of the tube 42 . One preferred jack 50 as shown in FIG. 2 includes a collar with pilot bearing 52 . The shaft 46 extending from the outward end of the tube 42 is inserted into the collar 52 . The shaft 46 may rotate as a result of the supporting pilot bearing 52 .
[0034] [0034]FIG. 7 shows an alternative arrangement of a first jack 68 and second jack 70 in which the jacks include supports 76 A and 76 B extending laterally to a side of the jacks for supporting the tube 42 that the carpet roll is on. In this arrangement, the jacks 68 and 70 support the tube to the side and offset from the center of the jacks.
[0035] Once the jack 50 or 68 supports the outward end of the tube 42 , the jack 50 is moved away from the rear of the vehicle 12 , thus moving the carpet roll 10 out of the vehicle. The carpet roll 10 , which is supported at the inward end of the tube 42 by the moving trolley system 34 , does not completely exit the vehicle 12 because the trolley may only traverse to the end of the rail 26 . Once at the end of the rail 26 , a provided release mechanism, such as a latch pin, is released to permit telescoping of the telescoping tube member 44 to extend the tube and further remove the carpet roll 10 from the rear of the vehicle 12 . The hook or attaching device 40 , which connects the cable to the end of tube 42 to support the carpet roll 10 , attaches to the telescoping tube member 44 . Thus, the carpet roll 10 may be separated from the vehicle 12 via the telescoping tube member 44 , and, the tube 42 then disconnected from hoist cable 38 .
[0036] After disconnecting the tube 42 from the hoist cable 38 , the user may rest the end of the carpet roll 10 opposite the end supported by the jack 50 on an external pedestal 58 . The carpet roll 10 supported by the jack 50 and pedestal 58 may be positioned for using the roll of carpet. Rolling stands 54 A and 54 B (or 72 A and 72 B) along with several casters 56 a and 56 b that are situated beneath the jack and pedestal (or combination of jacks as in FIG. 7) permit movement of the supported carpet roll to a suitable work location. Once situated, stabilizers 74 A and 74 B may be provided to extend from each side of the stands 72 A and 72 B. These stabilizers may be arranged to telescope from the center beam of the stands and turned up to retract into the center beam when not in use. A locking mechanism may be arranged between the stabilizers and stand to affix the stabilizers into the telescoped or retracted positions. The pedestal 58 may have rollers 60 that support the end of the tube 42 . The combination of the pilot bearing 52 supporting the shaft 46 at one end of the tube 42 and the rollers 60 supporting the telescoping tube member 44 at the other end of the tube permit the unrolling of the carpet roll 10 after it has been removed completely from the vehicle 12 . Alternatively, the inward end of the tube 42 could remain attached to the vehicle 12 . A bearing member may be provided on the telescoping tube member 44 to permit the tube 42 to rotate while attached to the vehicle 12 via cable 38 or other means, thus permitting unrolling of the carpet. In another embodiment shown in FIG. 7, each end of the tube 42 may be supported by the brackets 76 A and 76 B. Thereby, the roll of carpet may roll freely about the tube 42 .
[0037] It should be apparent to those skilled in the art that modifications and variations can be made to the embodiments of the invention described herein without departing from the scope and spirit of the invention as set forth in the claims and their equivalents. | An unloading apparatus for unloading a roll of material such as carpet from a transport vehicle comprising a support frame having a rail running lengthwise above a roll of material within the cargo bay. A trolley system is movably attached to one end of the rail for traversing along the rail toward the rear of the vehicle. A lifting device, such as a hoist cable, attaches the trolley system to a first end a mandrel tube that passes through the roll material being supported. The tube may be adjustable in length and includes a telescoping member, which is at the end attached to the lifting device. A mobile support jack is situated outside of the cargo bay for lifting and supporting the second end of the tube when removing the roll material from the vehicle. The support jack may be moved away from the vehicle while supporting the roll of material at its second end. Additionally, a mobile support pedestal or additional jack member may be provided to support the first end of the tube when detached from the trolley system. Both the support jack and support pedestal may be provided bearing members to permit the rolled material to rotate for unrolling. | 1 |
FIELD OF INVENTION
[0001] The present invention relates to the improved process for the preparation of highly pure form of S-[1,2-(dicarbethoxy)-ethyl]O,O-dimethyl phosphorodithioate having formula (I).
[0000]
[0002] The compound of formula (I) has adopted name “Malathion”. The present invention also relates to the novel process of preparing intermediate O,O-dimethyldithiophosphoric acid of formula (II), which is useful in the preparation of Malathion.
[0000]
[0003] The Malathion prepared by the process of this invention is highly storage stable and toxic impurities are much lower than any other commercial preparation available for the pharmaceutical purpose.
BACKGROUND OF THE INVENTION
[0004] Various processes for the preparation and/or purification of Malathion are disclosed in the literature. Malathion {CAS Number: 121-75-5} is an organophosphate insecticide that inhibits cholinesterase activity in vivo. The U.S. Food and Drug Administration (FDA) supports the pharmaceutical use of malathion for the treatment for head lice in children. Due to its low toxicity to humans. Malathion may be prepared by reacting O,O-dimethyldithiophosphoric acid (OODMDTPA) with diethyl maleate (U.S. Pat. Nos. 2,578,652, 2,879,284, 3,403,201, 3,463,841, 3,470,272, 4,367180, 2007/0010496 and 4,681,964).
[0000]
[0005] But, still numerous impurities are found in Malathion preparation. Some of these impurities are formed during storage and some are generated during the manufacturing process. Many of these Malathion impurities have been found to be toxic. O,O,S-trimethyl phosphorodithioate (MeOOSPS) and O,S,S-trimethyl phosphorothioate (MeOSSPO) can cause liver damage (Keadtisuke et al, Toxicology letters 52:35-46 (1990) or immune suppression (Rodgers et al, immunopharmacology 17: 131-140 (1989). The toxicity of Iso Malathion is due to its ability to inhibit acetylcholinesterase, in fact Iso Malathion is ˜1,000 times as active against acetylcholinesterase as compared with Malathion (Tetrahedron letters 33(11). 1415-18 (1992). Malathion physical properties make it difficult to remove impurities by conventional means for example, because Malathion is liquid at ambient temperature (melting point: 2.9° C.), and crystallization is difficult.
[0006] Therefore, we have developed an improved process for the preparation of Malathion for pharmaceutical use. Malathion produced by this method has significantly lower levels of toxic impurities and storage stable, when compared to the any other commercial method available in literature for the pharmaceutical use.
SUMMARY OF THE INVENTION
[0007] The present invention relates to the improved process of preparation of Malathion of formula (I),
[0000]
[0000] which comprises:
i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for the period of 1.5-2 hours; ii) stirring the above suspension for the period of 5-6 hours at 50-55° C.; iii) expelling the H 2 S gas with nitrogen, after cooling the above suspension to 25-28° C.; iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA; v) the crude O,O-DMDTPA is subjected to dissolution in suitable solvent and ammonia gas is purged to precipitate the pure O,O-DMDTPA.NH 3 salt; vi) the above obtain O,O-DMDTPA.NH 3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA; vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure O,O-DMDTPA; viii) adding the above obtain pure O,O-DMDTPA to diethyl maleate at low temperature of −30 to −25° C. in four lots, each at regular interval of 20 minutes; ix) maintain the above reaction mass at temperature of −30 to −25° C. for the period of 4 hours; x) water wash the above mass to remove O,O-DMDTPA; xi) treating the above obtain crude Malathion with sulfur reagent at 5 to 10° C. for the period of 13 hours; xii) crystallizing the above obtained Malathion from methanol at low temperature and xiii) drying the above obtain mass with anhydrous sodium sulphate in isopropanol to obtain Malathion of formula (I).
[0021] The present invention also relates to novel process for the preparation of intermediate O,O-DMDTPA having formula (II), which is used in step (viii) of process of preparation of Malathion of formula (I),
[0000]
[0000] which comprises:
i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for the period of 1.5-2 hours; ii) stirring the above suspension for the period of 5-6 hours at 50-55° C.; iii) expelling the H 2 S gas with nitrogen, after cooling the above suspension to 25-28° C.; iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA; v) the crude O,O-DMDTPA is subjected to dissolution in ethyl acetate and ammonia gas is purged to precipitate the pure O,O-DMDTPA.NH 3 salt; vi) the above obtain O,O-DMDTPA.NH 3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA and vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure product.
[0029] In one aspect, the Malathion prepared by the process of present invention having a reduced level of toxic impurities.
[0030] In another aspect, the Malathion prepared by the process of present invention is storage stable.
[0031] In yet another aspect, the Malathion prepared by this process may be used for pharmaceutical purpose.
[0032] In still another aspect, the Malathion prepared by the process of the present invention comprises:
[0000] i) greater than 99.5% w/w Malathion and less than 0.09% of Isomalathion, less than 0.03 of O,O,S-trimethyl phosphorodithioate, less than 0.002% of diethyl fumarate, less than 0.1% of unknown impurities and less than 0.21 of total impurities.
ii) water content is less than 0.02%.
DETAILED DESCRIPTION OF THE INVENTION
[0033] Accordingly, the present invention relates to the improved process for the preparation of Malathion of formula (I),
[0000]
[0000] which comprises:
i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for the period of 1.5-2 hours; ii) stirring the above suspension for the period of 5-6 hours at 50-55° C.; iii) expelling the H 2 S gas with nitrogen, after cooling the above suspension to 25-28° C.; iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA; v) the crude O,O-DMDTPA is subjected to dissolution in suitable solvent and ammonia gas is purged to precipitate the pure O,O-DMDTPA.NH 3 salt; vi) the above obtain O,O-DMDTPA.NH 3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA; vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure O,O-DMDTPA; viii) adding the above obtain pure O,O-DMDTPA to diethyl maleate at low temperature of −30 to −25° C. in four lots, each at regular interval of 20 minutes; ix) maintain the above reaction mass at temperature of −30 to −25° C. for the period of 4 hours; x) water wash the above mass to remove O,O-DMDTPA; xi) treating the above obtain crude Malathion with sulfur reagent at 5 to 10° C. for the period of 13 hours; xii) crystallizing the above obtained Malathion from methanol at low temperature and xiii) drying the above obtain mass with anhydrous sodium sulphate in isopropanol to obtain Malathion of formula (I).
[0047] Accordingly, there is provided an improved process for the preparation of intermediate O,O-DMDTPA having formula (II), which is used in step (viii) of process of preparation of Malathion of formula (I),
[0000]
[0000] which comprises:
i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for the period of 1.5-2 hours; ii) stirring the above suspension for the period of 5-6 hours at 50-55° C.; iii) expelling the H 2 S gas with nitrogen, after cooling the above suspension to 25-28° C.; iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA; v) the crude O,O-DMDTPA is subjected to dissolution in suitable solvent and ammonia gas is purged to precipitate the pure O,O-DMDTPA.NH 3 salt; vi) the above obtain O,O-DMDTPA.NH 3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA and vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure O,O-DMDTPA.
[0055] In the step (i) of the above preparation, phosphorous sulfide used in the reaction can be selected from phosphorus pentasulfide, tetraphosphorus heptasulfide and tetraphosphorus decasulfide and preferably using phosphorus pentasulfide. Solvent used in the reaction can be selected from group consisting of hexane, benzene, toluene, diethyl ether, chloroform, ethyl acetate and dichloromethane and preferably using toluene.
[0056] In the step (iii) of the above preparation, expel the H 2 S gas with nitrogen, after cooling the above suspension to 25-28° C. If H 2 S is present, it will react with diethyl maleate to afford diethyl-2-mercaptosuccinate and dimerize to form tetraethyl dithiodisuccinate.
[0057] In the step (iv) of the above preparation, the insoluble impurities may be any unreacted solids. Example: Phosphorus sulfide.
[0058] In the step (v) of the above preparation, the solvent used in reaction can be selected from hexane, benzene, toluene, diethyl ether, chloroform, ethyl acetate and dichloromethane and preferably using ethyl acetate. In this step, ammonia gas is purged in the reaction vessel at temperature of −10 to 5° C. till p H of 9.5-9.8 is reached and preferably at a temperature in the range from −5 to 0° C. The duration of the reaction may range from 1 to 4 hours, preferably for the period of 2 hours.
[0059] In the step (vi) of the above preparation, the reaction temperature may range from −30 to −15° C. and preferably at a temperature of −20° C. The duration of the reaction may range from 10 to 30 minutes, preferably for the period of 20 minutes.
[0060] In the step (viii) of the above preparation, the molar ratio of diethyl maleate to O,O-DMDTPA in reaction is 1:2.5 and preferably using the molar ratio of diethyl maleate to O,O-DMDTPA is 1:2.0
[0061] In the step (x) of the above preparation, water washing is carried out to remove water soluble impurities, at 10 to 15° C. until the p H of last water wash is found to be 6.5 to 7.0.
[0062] In the step (xi) of the above preparation, the sulfide reagent used in reaction can be selected from sodium sulfide, potassium sulfide, phosphorus pentasulfide, calcium sulfide, ammonium sulfide and ammonium bisulfide and preferably using phosphorus pentasulfide. An aqueous solution of sulfide reagent used in this step of reaction is usually 3%.
[0063] In the step (xii) of the above preparation, crystallization of above obtain Malathion from methanol at temperature of −45 to −25° C. and preferably at a temperature in the range from −40 to −30° C.
[0064] In the step (xiii) of the above preparation, the reaction temperature may range from 15 to 40° C. and preferably at a temperature in the range from 25 to 27° C. The duration of the reaction may range from 5 to 9 hours, preferably for the period of 7 hours. The water content of isopropanol used in the reaction must below 0.05%.
[0065] The Malathion prepared by the process of this invention is storage stable. Specially, after storage at 8-15° C. for the period of 6 months, the Malathion has following purity/impurity profile
[0066] i. greater than about 99.5% (w/w) Malathion.
[0067] ii. less than 0.09% of Isomalathion
[0068] iii. less than 0.03 of O,O,S-trimethyl phosphorodithioate
[0069] iv. less than 0.002% of diethyl fumarate
[0070] v. less than 0.1% of unknown impurities
[0071] vi. less than 0.21 of total impurities and
[0072] vii. water content is less than 0.02%.
[0073] The details of the invention are given in the examples provided below, which are given to illustrate the invention only and therefore should not be construed to limit the scope of the invention
Example 1
Preparation of Crude O,O-Dimethyl Dithio Phosphoric Acid
Step (i): Preparation of Crude O,O-Dimethyl Dithio Phosphoric Acid
[0074] To 4-necked flask (1 L) equipped with mechanical stirrer, thermometer pocket, pressure equalizing funnel and nitrogen atmosphere, was charged toluene (150 mL, Kf<0.1%) and phosphoruspentasulfide (222 grams) at room temperature. An alkali scrubber was used to trap hydrogen sulfide gas released during the reaction. Methanol (150 grams, Kf<0.1%) was added to the above reaction mass at 25-35° C. for the period of 1.5-2 hours. After the addition of methanol, temperature of the above reaction mass was raised to 50° C. and maintained the temperature at 50-55° C. for a period of 5 hours. The evolution of hydrogen sulfide gas was confirmed by checking with lead acetate paper and the reaction mass was cooled to 25-28° C. and nitrogen gas was purged for 20-30 minutes to expel traces of hydrogen sulfide gas presented. The reaction mass was then filtered through hy-flow bed to remove any unreacted phosphorus pentasulfide and washed with toluene (150 mL). Layer separation was done to remove a small amount of lower layer, and upper toluene layer was taken for concentration under vacuum at 45-50° C. and concentrated till toluene content was found to be below 5%, which is monitored by HPLC.
[0075] Yield: 260-270 grams.
[0076] HPLC purity: 87.21%.
Step (ii): Preparation of 1 st Ammonium Salt of O,O-DMDTPA
[0077] To 4-necked flask (5 L) equipped with mechanical stirrer, thermometer pocket and gas sparger, was charged ethyl acetate (2.7 L) and crude O,O-DMDTPA (270 grams) (obtained from Step (i)). Cooled the above reaction mass to −5° C. and purged the ammonia gas in the reaction vessel at a temperature of −5-0° C. till pH was reached to 9.5-9.8. After the desired pH was achieved, reaction mass was maintained at −5 to 0° C. for a period of 2 hours. The reaction mass was then filtered and washed with ethyl acetate (270 mL). Suck dried and unloaded. The wet weight of obtained ammonium salt was 240-255 grams. Dried at 25-28° C. under vacuum for the period of 5 hours or till constant weight was achieved.
[0000] The dry weight of ammonium salt was 233-240 grams.
[0078] HPLC purity: 99.33%.
Step (iii): Regeneration of Ammonium Salt of O,O-DMDTPA
[0079] To 4-necked flask (3 L) equipped with mechanical stirrer, thermometer pocket and pressure-equalizing funnel, was charged dichloromethane (1.68 L). Cooled the above reaction mass to −25 to −20° C. and concentrated sulphuric acid (65 grams) was charged in the pressure equalizing funnel and added to the above reaction mass drop wise at temperature of −25 to −20° C. Maintained the above reaction mass at −20° C. for 20 minutes and pH of dichloromethane layer was checked as per above pH checking process to obtain pH below 2.0. The temperature of the reaction mass was raised to 25° C. in 30-35 minutes and stirred for the period of 2 hours. The above reaction mass was filtered and washed with dichloromethane (233 mL). The filtered ammonium sulphate containing compound was once again stirred with dichloromethane (1.165 L) for a period of 2 hours and the ammonium sulphate was filtered and washed with dichloromethane (233 mL). The dichloromethane layers were combined and concentrated at 30-35° C. under vacuum till constant weight was achieved. The weight of regenerated O,O-DMDTPA was 184-188 grams and ammonium sulphate was 105-112 grams. If weight of ammonium sulphate is more than theoretical weight, stirred once with dichloromethane.
[0080] HPLC purity: 98.09%.
Step (iv): Preparation of 2 nd Ammonium Salt of O,O-DMDTPA
[0081] To 4-necked flask (3 L) equipped with mechanical stirrer, thermometer pocket and gas sparge, was charged ethyl acetate (1.84 L) and regenerated 0, O-DMDTPA (184 grams) (obtained from step (iii)). Cooled the above reaction mass to −5° C. and purged the ammonia gas in the reaction vessel at a temperature of −5 to 0° C. till pH of 9.5-9.8 was reached. After the desired pH was achieved, reaction mass was maintained at −5 to 0° C. for the period of 2 hours. The above reaction mass was then filtered and washed with ethyl acetate (184 mL). Suck dried and unloaded. The wet weight of obtained ammonium salt was 172-175 grams. Dried at 25-28° C. under vacuum for the period of 5 hours or till constant weight was achieved. The dry weight of ammonium salt was 162-166 grams.
[0082] HPLC purity: 99.68%
Step (v): Regeneration of 2 nd Ammonium Salt of 0, O-DMDTPA
[0083] To 4-necked flask (3 L) equipped with mechanical stirrer, thermometer pocket and pressure-equalizing funnel, was charged dichloromethane (1.204 L). Cooled the above reaction mass to −25 to −20° C. Concentrated sulphuric acid (46 grams) was charged in the pressure equalizing funnel and added to the above reaction mass drop wise at −25 to −20° C. and maintain the above reaction mass at −20° C. for a period of 20 minutes. p H of dichloromethane layer was checked as per above pH checking process to obtain the pH below 2.0. The temperature of the reaction mass was raised to 25° C. in 30-35 minutes and stirred for a period of 2 hours. The above reaction mass was filtered and washed with dichloromethane (163 mL). The filtered ammonium sulphate containing compound was once again stirred with dichloromethane (860 mL) for a period of 2 hours and ammonium sulphate was filtered and washed with dichloromethane (163 mL). The dichloromethane layers were combined and concentrated at 30-35° C. under vacuum till constant weight was achieved. The weight of regenerated O,O-DMDTPA was 123-126 grams and ammonium sulphate was 74-80 grams. If weight of ammonium sulphate is more than theoretical weight, stirred once with dichloromethane.
[0084] HPCL purity: 97.84%.
[0085] IR spectra (cm −1 ): 1016.23;
[0086] 1 H NMR (400 MHz, CD 3 OD): δ 3.0343 (singlet, 1H), 3.83-3.87 (2 singlets, 6H).
Example 2
Preparation of Malathion
Step (i): Preparation of Crude Malathion
[0087] To 4-necked flask (0.5 L) equipped with mechanical stirrer, thermometer pocket and nitrogen atmosphere, was charged O,O-DMDTPA (126 grams, 0.797 M) (obtained from Example 1). Cooled the above reaction mass to −30 to −25° C. and add diethyl maleate (55 grams, 0.319 M, GC purity: 97%) in 4 lots (each 13.8 grams) at regular interval of 20 minutes at −30 to −25° C., and maintained the above reaction mass temperature at −30 to −25° C. for the period of 4 hours. The sample was analyzed after 4 hours to check the diethyl maleate content below 1% by HPLC before proceeding for workup. If the diethyl maleate was found to be more than 1% the above reaction mass was maintained for another one hour at the same temperature and again analyzed by HPLC. After the diethyl maleate content was found to be less than 1% by HPLC, the above reaction mass temperature was raised to 5-10° C. and washed with demineralized water (181 mL) for 6 times. pH of last water wash was checked and found to be 6.5-7.5. In case the pH is not in range, one more water wash needs to be done. The sample was analyzed to check the O,O-DMDTPA content below 0.05% by HPLC.
[0088] Yield: 110-112 grams.
Step (ii): Removal of Diethyl Fumarate from Crude Malathion
[0089] Crude Malathion (111 grams) (obtained from step (i)) was stirred with 3% sodium sulphide solution (111 mL) at 10-15° C. for the period of 13 hours. HPLC analysis of the sample after 13 hours showed diethyl fumarate not more than 0.1%. Both layers were separated and organic layer was washed with demineralised water (111 mL) for 6 times by maintaining temperature at 10-15° C. till pH of 6.5-7.5. was achieved.
[0090] Yield: 80 grams.
Step (iii): Purification of Malathion
[0091] To a 4-necked flask (0.5 L) equipped with mechanical stirrer, thermometer pocket and calcium chloride guard tube, was charged methanol (160 mL) and Malathion (80 grams). The reaction mass was cooled to −40 to −35° C. slowly when formation of white solid was observed. Methanol (160 mL) was once again added and reaction mass temperature is raised to −10° C. The above reaction mass was cooled once again to −30 to −25° C. and maintained for period of 30 minutes. Methanol (240 mL) was siphoned out from the above reaction mass and temperature thereafter raised from 8 to 10° C. To the above reaction, add dichloromethane (160 mL) and demineralized water and stirred at 10° C. for the period of 10 minutes. The layers were separated, aqueous layer volume was measured and found to be 240 mL. To the dichloromethane layer, add demineralized water (160 mL) and stirred at temperature of 5-10° C. for the period of 10 minutes. The layers were separated, aqueous layer volume was measured and found to be 160 mL. The dichloromethane layer was dried over anhydrous dried sodium sulphate (8.0 gram), filtered washed with dichloromethane (40 mL). This dichloromethane layer was filtered through 0.5□ filter paper, concentrated at 25-30° C. under vacuum to obtain pure Malathion.
[0092] Yield: 57 grams.
Step (iv): Drying of Malathion
[0093] The pure Malathion (57 grams) (obtained from step (iii)) was filtered through 0.5 filter paper under nitrogen atmosphere and charged to a 4-necked flask (0.5 L) equipped with mechanical stirrer, thermometer pocket and nitrogen atmosphere. Add isopropanol (275 mL, Kf<0.05%) and anhydrous dried sodium sulphate (27 grams) at 25-27° C. and stirred for the period of 7 hours at 25-27° C. The water content after 7 hours of stirring was checked and found to be 0.16%. The mass was filtered through filter paper no. 1 under nitrogen atmosphere and washed with isopropanol (30 mL). This mass was again filtered through 0.5 filter paper under nitrogen and washed with isopropanol (25 mL). The filtrate was concentrated under 5-10 mm Hg vacuum and maintain temperature at 25-27° C. for a period of 9 hours. The dried Malathion was carefully unloaded under nitrogen atmosphere and water content was checked and found to be less than 0.1%.
[0094] IR spectra (cm −1 ): 1737.28, 1016.23;
[0095] 1 H NMR (400 MHz, CD 3 OD): δ 1.22-1.32 (2 triplets, 6H), 2.90-3.76 (2 quartets, 4H), 3.80-3.81 (2 doublets, 6H), 4.11-4.21 (multiplet, 3H).
Example 3
Analysis of Sample Batches of Malathion Prepared by this Process
[0096] In Table II set forth below, three different batches of Malathion are prepared by the process of present invention (noted as A, B, C) were analyzed by HPLC for the identification of purity and impurities. After storage at 8-15° C. for the period of 6 months:
[0000]
TABLE II
Batch No.
Analysis
A
B
C
HPLC assay
99.8%
99.8%
99.5%
Iso S-[1,2-
0.06%
0.07%
0.09%
(dicarbethoxy)-
ethyl]O,O-dimethyl
phosphorodithioate
Malaoxon
Nil
Nil
Nil
S-imp
0.03%
0.03%
0.01%
O,O,S-trimethyl
phosphorodithioate
Diethyl maleate
Nil
Nil
Nil
Diethyl fumarate
0.002%
0.001%
0.002%
O,O-DMDTPA
Nil
Nil
Nil
Unknown impurities
0.12%
0.20%
0.11%
Total impurities
0.21%
0.3%
0.21%
Water content
0.04%
0.02%
0.04% | The present invention relates to the improved process for the preparation of highly pure form of S-[1,2-(dicarbethoxy)-ethyl]O,O-dimethyl phosphorodithioate having formula (I). The compound of formula (I) has adopted name “Malathion”. The present invention also relates to the novel process of preparing intermediate O,O-dimethyldithiophosphoric acid of formula (II), which is useful in the preparation of Malathion. The Malathion prepared by the process of this invention is highly storage stable and toxic impurities are much lower than any other commercial preparation available for the pharmaceutical purpose. | 2 |
FIELD OF THE INVENTION
The present invention relates to printing systems, and in particular to a printing system that includes a printer wherein the feed rate of the media is self adjusted so as to reduce and/or eliminate throttling in the printing system and therefore increase throughput.
BACKGROUND OF THE INVENTION
Addressing printer systems for printing information such as address information (e.g., destination and/or return address information) and other images, such as one or more logos, on a number pieces of print media, such as envelopes or paper, are known (for convenience, the term “image data” shall be used herein to refer to the entirety of the information that is printed on a piece of print media). In a typical addressing printer system, a host computer is operatively coupled to an addressing printer that includes a fixed print head, a transport mechanism, such as a number of belts forming a belt assembly, which transports the print media while being printed upon by the print head, and a feeding mechanism, such a number of rollers, which feeds the individual pieces of print media from a source of print media to the transport mechanism. The host computer electronically transmits the image data that is to be printed on each piece of print media to the addressing printer, which in turn prints the image data as the print media is being transported by the transport mechanism.
Preferably, during normal operation, the feeder motor which controls the feeding mechanism is continuously in an on condition. This continuous operation provides the maximum throughput that the feeding mechanism is capable of delivering. However, due to the speed of the transport mechanism and the length of the print media, there is a fixed amount of time available for the printer software to prepare the received (from the host computer) image data that is to be printed on each piece of print media. Furthermore, a piece of print media cannot be fed until the image data to be printed is ready to print. Thus, if the preparation time for a piece of image data is longer than it takes to feed a piece of print media, due to the complexity of the image data and/or a delay associated with the communications channel between the host computer and the printer, the feeding mechanism must be stopped while the image data preparation is completed. Only after the image data preparation is completed can the feeding mechanism be restarted. The delay caused by such stopping and restarting of the feeding mechanism (known in the art as “throttling”) results in a lower throughput rate (i.e., lower than if the feeding mechanism was running continuously, even if such continuous operation was at a lower speed than the maximum). There is thus a need for systems and/or methods which reduce and/or eliminate throttling in printing systems.
SUMMARY OF THE INVENTION
In one embodiment, a method of controlling a feed rate of a printer, such as, without limitation, an addressing printer coupled to a host computer, is provided wherein the printer includes a feeder motor driving a feeder mechanism and a transport motor driving a transport mechanism. The method includes receiving image data for a first item of print media in a print job, processing the image data to create printable image data, and determining an image preparation time that is a time difference between the time when the printable image data is completed and the time when the start of the image data is first received. The method then further includes determining a current feeder speed based on at least the image preparation time. Following that that determination, the method includes: (i) turning the transport motor on, and (ii) setting a speed of the feeder motor equal to the current feeder speed and thereafter turning the feeder motor on. Preferably, the method further includes receiving job data relating to the print job that specifies a transport motor speed, wherein the step of turning the transport motor on includes setting the speed of the transport motor to be equal to the transport motor speed specified in the job data and thereafter turning the transport motor on.
In one particular embodiment, the method further includes receiving job data relating to the print job that includes at least a transport motor speed. In this embodiment, the step of determining the current feeder speed includes determining the current feeder speed based on at least the image preparation time and the transport motor speed. In another particular embodiment, the step of determining the current feeder speed includes ensuring that the current feeder speed is no more than a predetermined maximum feeder speed and no less than a predetermined minimum feeder speed.
In yet another particular embodiment, the method further includes printing the first item of print media after the transport motor and the feeder motor are turned, and sometime thereafter: receiving current image data for a subsequent item of print media in the print job, processing the current image data to create printable current image data, determining a subsequent image preparation time that is the time difference between the time when the printable current image data is completed and the time when a start of the current image data is received, determining a subsequent current feeder speed based on at least the subsequent image preparation time, and after the subsequent current feeder speed is determined, setting the speed of the feeder motor to be equal to the subsequent current feeder speed.
In another embodiment, a printer is provided that includes a print head, a transport mechanism for moving print media relative to the print head, a transport motor for driving the transport mechanism, a feeder mechanism for feeding the print media to the transport mechanism, a feeder motor for driving the feeder mechanism, and a processing unit operatively coupled to the transport motor and the feeder motor. The processing unit in this embodiment is adapted to perform one or more of the embodiments of the method just described.
Therefore, it should now be apparent that the invention substantially achieves all the above aspects and advantages. Additional aspects and advantages of the invention will be set forth in the description that follows, and in part will be obvious from the description, or may be learned by practice of the invention. Moreover, the aspects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings illustrate presently preferred embodiments of the invention, and together with the general description given above and the detailed description given below, serve to explain the principles of the invention. As shown throughout the drawings, like reference numerals designate like or corresponding parts.
FIG. 1 is a schematic diagram of a printing system according to one particular, non-limiting embodiment of the invention;
FIG. 2 is a flowchart showing one embodiment of a method of adjusting the speed of the feeder motor of FIG. 1 prior to initiating the printing of any print media in a given print job according to an aspect of the present invention; and
FIG. 3 is a flowchart showing one embodiment of a method of adjusting the speed of the feeder motor of FIG. 1 following the printing of the first print media in a given print job according to a further aspect of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As employed herein, the statement that two or more parts or components are “coupled” together shall mean that the parts are joined or operate together either directly or through one or more intermediate parts or components. As employed herein, the term “number” shall mean one or an integer greater than one (i.e., a plurality).
FIG. 1 is a schematic diagram of a printing system 5 according to one particular, non-limiting embodiment of the invention. The printing system 5 includes a host computer 10 , which may be, for example and without limitation, a PC, which is in electronic communication with a printer 15 through a communications channel 20 . The communications channel 20 may be a wired connection, such as, without limitation, a USB connection, or a wireless connection implemented according to a suitable wireless protocol, such as, without limitation, a wireless protocol established according to the IEEE 802.11 set of standards.
As seen in FIG. 1 , the printer 15 includes a processing unit 25 , which may include a microprocessor, a microcontroller, or any other suitable processor, which is operatively coupled to a suitable memory for storing routines to be executed by the processing unit 25 . Specifically, the memory, which may be separate from and/or internal to the microprocessor, microcontroller or other suitable processor, stores printer software 30 for implementing the methods of operation described in greater detail elsewhere herein.
In addition, the printer 15 includes a fixed print head 35 which is operatively coupled to and under the control of the processing unit 25 . In the preferred embodiment, the fixed print head 35 is an ink jet print head, but it should be understood that other types of suitable print heads, such as, without limitation, thermal print heads, may also be used. The printer 15 also includes a transport motor 40 (such as, without limitation, a DC motor) which is operatively coupled to and under the control of the processing unit 25 and which drives a transport mechanism 45 , such as a belt assembly including a number of belts, for transporting print media relative to the print head 35 so that information can be printed thereon by the print head 35 . The printer 15 further includes a feeder motor 50 (such as, without limitation, a DC motor) which is operatively coupled to and under the control of the processing unit 25 and which drives a feeder mechanism 55 , such as a number of rollers, for feeding individual pieces of print media from a source of print media (not shown) to the transport mechanism 45 . Finally, the printer 15 includes a real time clock 60 which is operatively coupled to the processing unit 25 for providing time information to the processing unit 25 (alternatively, the real time clock 60 can be provided as part of the processing unit 25 ).
FIG. 2 is a flowchart showing one embodiment of a method of adjusting the speed of the feeder motor 50 , and thus the rate of the feeder mechanism 55 , prior to initiating the printing of any print media in a given print job according to an aspect of the present invention. FIG. 3 is a flowchart showing one embodiment of a method of adjusting the speed of the feeder motor 50 , and thus the rate of the feeder mechanism 55 , following the printing of the first print media in a given print job according to a further aspect of the present invention.
Referring to FIG. 2 , the method begins at step 100 , wherein the printer software 30 receives print job data relating to the current print job from the host computer 10 over the communications channel 20 . As will be appreciated, the print job will specify that a plurality of pieces of print media are to be printed, each with specified image data. In the preferred embodiment, the print job data includes at least the speed at which the transport motor 40 is to operate during the print job. Next, at step 105 , the printer software sets (i) the speed of the transport motor 40 , and thus the speed of the transport mechanism 45 , to be equal to the speed specified in the job data, and (ii) the speed of the feeder motor 50 , and thus the speed of the feeder mechanism 55 , to a maximum value based on the speed of the transport motor 40 . Preferably, that maximum value is just below (e.g., a predetermined percentage of or some predetermined value between 75-97% of the speed of the transport motor 40 (referred to as the slowdown factor) in order to provide a tension to the print media being fed and prevent jams. Note, however, that at this point, the neither the transport motor 40 nor the feeder motor 50 have been turned on (i.e., they are idle).
Next, at step 110 , the printer software 30 receives the start of the image data for the first item of print media included in the print job from the host computer 10 over the communications channel 20 and records the time of such receipt based on the input received from the clock 60 . At step 115 , the printer software 30 receives the end of the image data for the first item of print media included in the print job from the host computer 10 over the communications channel 20 . Then, at step 120 , the printer software 30 processes the whole of the received image data for the first item of print media included in the print job to create printable image data (i.e., data that allows the image data to actually be printed by the print head 35 ) and records the time of completion of the printable image data based on the input received from the clock 60 . The processing that is performed at step 120 to create the printable image data may include, for example and without limitation, parsing the received image data and rendering the parsed data.
Next, at step 125 , the printer software 30 determines the image preparation time based on the time difference between the time of receipt of the start of the image data for the first item of print media included in the print job recorded in step 110 and the time of completion of the printable image data recorded in step 120 . At step 130 , the printer software 30 then determines a current feeder speed based on (i.e., as a function of) the image preparation time determined in step 125 . In a preferred, non-limiting embodiment, the current feeder speed is determined based on the image preparation time as follows. First, a first calculated feeder speed is calculated as a function of (i) the image preparation time, and (ii) the transport speed specified in the job data as described above. Next, a second calculated feeder speed is determined as the minimum of (i) the first calculated feeder speed, and (ii) the maximum feeder speed described above (which is based on the transport speed in the job data). In other words, at this point in the determination, the feeder speed is not allowed to exceed the maximum feeder speed. Finally, the current feeder speed is determined as the maximum of (i) the second calculated feeder speed, and (ii) a predetermined minimum feeder speed value chosen so as to avoid stalling. In other words, at this point in the determination, the feeder speed is not allowed to fall below the predetermined minimum feeder speed value. Following step 130 , i.e., once the current feeder speed is determined, the method proceeds to step 135 , wherein the printer software 30 sets the speed of the feeder motor 50 , and thus the speed of the feeder mechanism 55 , to the current feeder speed determined in step 130 , and then turns on both the transport motor 40 and the feeder motor 50 so that feeding and printing can begin.
As noted above, FIG. 3 is a flowchart showing one embodiment of a method of adjusting the speed of the feeder motor 50 following the steps of FIG. 2 , i.e., following the printing of the first item of print media in a given print job. In other words, the method of FIG. 3 is employed to adjust the feeder motor 50 while printing subsequent items of print media included in the print job (i.e., subsequent to the first item described in connection with FIG. 2 ). For illustrative purposes, the method of FIG. 3 will be described in connection with one such subsequent item of print media that is to be printed with particular image data sent from the host computer 10 (referred to as “current image data” in FIG. 3 ). As will be appreciated, the steps of FIG. 3 are repeated for each subsequent item of print media included in the print job. As a result, the speed of the feeder motor is continuously updated and adjusted with each print operation.
The method begins at step 150 , wherein the printer software 30 receives the start of the current image data and records the time of such receipt based on the input received from the clock 60 . At step 155 , the printer software 30 receives the end of the current image data. Then, at step 160 , the printer software 30 processes the received current image data to create printable current image data (i.e., data that allows the current image data to actually be printed by the print head 35 ) and records the time of completion of the printable current image data based on the input received from the clock 60 . As noted elsewhere herein, the processing that is performed at step 160 to create the printable current image data may include, for example and without limitation, parsing the received current image data and rendering the parsed data.
Next, at step 165 , the printer software 30 determines the image preparation time based on the time difference between the time of receipt of the start of the current image data recorded in step 150 and the time of completion of the printable current image data recorded in step 160 . At step 170 , the printer software 30 then determines a current feeder speed based on (i.e., as a function of) the image preparation time, preferably as described elsewhere herein. Finally, at step 175 , the printer software 30 sets (adjusts) the speed of the feeder motor 50 to be equal to the current feeder speed determined in step 170 .
Thus, the method(s) as shown in FIGS. 2 and 3 have been developed to recognize when images are too complex to render at the current feeder speed and adjust the feeder speed to slow it down to prevent starting and stopping of the feeder motor 50 . The method(s) employ a forward feedback loop algorithm wherein the time to prepare (e.g., render) the current image is assumed to be similar to the time of the next image. This is a safe assumption in, for example, the mailing industry where each image of a print run is typically only different by the address being printed. Logos and other pictures are typically constant. Nonetheless, there may still be instances where an image may still be too complex or the host communication too slow such that slowing down the feeder motor 50 to its minimum speed will still not allow enough time to prevent the feeder mechanism 55 from stopping to wait for the image to be prepared. In such as case, the feeder motor 50 will be stopped and will wait until the image is ready to be printed before the feeder motor 50 is started again to feed the print media. In addition, as is apparent from the above description, as each new job is started, the feeder motor 50 is reset to its maximum speed. Thereafter, the time for each image is measured and the speed of the feeder mechanism 55 is adjusted image by image.
While preferred embodiments of the invention have been described and illustrated above, it should be understood that these are exemplary of the invention and are not to be considered as limiting. Additions, deletions, substitutions, and other modifications can be made without departing from the spirit or scope of the present invention. Accordingly, the invention is not to be considered as limited by the foregoing description but is only limited by the scope of the appended claims. | A method of controlling a feed rate of a printer, and a printer employing same, wherein the printer includes a feeder motor driving a feeder mechanism and a transport motor driving a transport mechanism. The method includes receiving image data for a first item of print media in a print job, processing the image data to create printable image data, and determining an image preparation time that is a time difference between the time when the printable image data is completed and the time when the start of the image data is first received. The method then further includes determining a current feeder speed based on at least the image preparation time. Following that that determination, the method includes: (i) turning the transport motor on, and (ii) setting a speed of the feeder motor equal to the current feeder speed and thereafter turning the feeder motor on. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is based on provisional application 60/433,892 filed Dec. 16, 2002 and entitled “Agent-Based Active Diagnostics System for Complex Distribution Networks”, hereby incorporated by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] --
BACKGROUND OF THE INVENTION
[0003] The present invention relates to computerized control systems and in particular to a control system for controlling fluid distribution in a dynamic distribution network.
[0004] Systems for distributing fluids such as fuel, liquid feedstocks, refrigerants, compressed air, fluidized solids, gases, and fluid-like quantities like electricity (subject to pressure and flow through a conduit), are an important component of manufacturing operations, chemical plants, office buildings, and large equipment. Often these distribution systems have complex networks of conduit whose configurations can change with demand or to accommodate failure of portions of the distribution system.
[0005] An example distribution system is chilled-water distribution in a modern warship. Chilled-water provides cooling for critical electronic components and machines as well as cooling for crew quarters and work areas.
[0006] Chilled-water must be provided to high priority users even in the face of damage to the distribution network, such as may occur in wartime. Accordingly, the chilled-water is distributed through a network of redundant pipeways connected by a valve system that allows chilled-water to be routed around damaged pipe sections if necessary. Additional reliability is obtained by providing multiple chilled-water producers that may be flexibly connected to any given chilled-water consumer through the redundant pipeways.
[0007] Controlling such a chilled-water system is extremely difficult. The multiple chilled-water producers, valves, and pipeways provide a large number of configurations, each of which must be considered when programming the control system. The control system must be programmed to accommodate varying and competing demands for chilled-water as chilled-water consumers switch in and out over time. Finally, the control system must respond to highly unpredictable damage to the distribution system such as may occur in battle.
[0008] Conventional programmed control systems can effectively provide only a limited range of responses covering easily anticipated problems and may require additional human supervision and/or manual intervention undercutting the benefits that could be obtained from completely automated control.
BRIEF SUMMARY OF THE INVENTION
[0009] The present invention provides an automatic control system for complex distribution systems that does not attempt to anticipate all possible combinations of demand and network failure and map them to a particular network configuration. Instead, critical components of the distribution system are associated with autonomous control units (ACU's) that are invested with a general decision-making framework that allows them to negotiate among themselves to reconfigure the network in response to unanticipated damage or changes in demand. In the preferred embodiment, the ACU use a “market-model” in which they bid for resources and evaluate solutions based on costs and available money. The result is a highly efficient automatic control of a complex network that yields efficient solutions for unexpected situations far faster than could be obtained by manual supervision.
[0010] Specifically, the present invention provides a control system for a distribution network having a set of distribution endpoints including at least one producer and consumer interconnected by a set of distribution resources including: a plurality of distribution lines joining the producers and consumers and switchable gates interconnecting the distribution lines, producers, and consumers. The control system is made up of: (a) a set of autonomous control units associated with at least some of the distribution endpoints, and (b) a set of autonomous control units associated with at least some of the distribution resources. The autonomous control units execute a stored program and communicate with each other to: (a) implement a set of money rules to allocate money resources to the consumers and a set of pricing rules for distribution resources, (b) bid for distribution resources on behalf of consumers based on the money rules and pricing rules, and (c) select distribution paths between producer and consumer endpoints using distribution resources based on bid responses.
[0011] It is thus one object of the invention to provide an improved method for controlling complex networks that can respond to unexpected situations. The bidding model allows the ACU's to work out specific solutions (e.g., how to route chilled-water) with only general guidance (e.g. knowledge of the consumer needing water and global knowledge as communicated by other ACU's). The market-model provides a familiar set of rules for distributed decision making.
[0012] It is another object of the invention to provide a control system for complex distribution networks that requires less programming for a given application. Once the ACU's are programmed for a particular distribution resource, new applications using that resource may reuse virtually all of that programming. For the same reason, the control system is highly scalable.
[0013] The pricing rules may assign higher prices to distribution between distribution endpoints requiring a greater number of distribution resources. Alternatively or in addition, the pricing rules may assign higher prices to valves that serve to segregate distributions related to separate producers.
[0014] It is thus another object of the invention to provide simple but flexible pricing rules. Tallying the number of resources used causes the system to tend toward simple distribution solutions. A simple price differential can cause the system to avoid certain valves such as those used to separate redundant chilled-water producer sources.
[0015] The money rules may provide greater money resources to a bidder if no successful bids are obtained and/or may provide initial money resources to a bidder based on the price of a previously accepted bid.
[0016] It is another object of the invention to provide a simple money rule that tends toward stable and efficient solutions. By starting at the last successful price, previous bid activity is leveraged to provide faster solutions. Allowing the money to increase if there are no successful bids ensures bid success if possible. The money rules also limit the depth of the search to improve the efficiency of the discovery algorithm by pruning uninteresting combination from the search.
[0017] The autonomous control units may be implemented in spatially separated hardware intercommunicating on a network and/or the stored program may be divided among the autonomous control units. The autonomous control units may be located proximate to the distribution resources or distribution endpoints with which they are associated.
[0018] It is thus another object of the invention to provide a control system that may be decentralized enhancing the ability of the system to resist spatially localized damage.
[0019] The autonomous control units may participate in multiple bids related to different consumers so long as the bids require consistent use of the distribution resource.
[0020] Thus, it is another object of the invention to provide a self-organizing control system that supports the ability of a pipeway to feed multiple consumers.
[0021] The autonomous control units associated with valves may receive an instruction causing them to close and remove themselves from future bidding.
[0022] It is thus another object of the invention to allow pipeway failures to be isolated.
[0023] The consumers may be assigned priorities and when bids associated with competing consumers cannot be satisfied, the stored program executed by the autonomous control units may select among competing consumers by priority.
[0024] It is therefore another object of the invention to allow the control system to simply differentiate between critical and non-critical consumers.
[0025] The autonomous control units associated with consumers may receive an instruction causing them to remove themselves from the bidding process and to release their distribution resources.
[0026] It is therefore another object of the invention to allow the system to quickly move between different modes, such as emergency and non-emergency modes, where different consumers are accepted in the bidding process.
[0027] The bidding may be propagated only between distribution resources directly connected by pipes.
[0028] It is another object of the invention to reduce the network load and time required to collect bids by using the physical topology of the pipes to truncate the bidding domain.
[0029] The network may provide redundant distribution producers and redundant pipes.
[0030] Thus, it is another object of the invention to provide control for a highly reliable distribution system having increased complexity because of the redundant components.
[0031] These particular objects and advantages may apply to only some embodiments of the invention covered by only some of the claims and thus do not define the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] [0032]FIG. 1 is a phantom view of a warship showing a simplified chilled-water distribution system having multiple chilled-water producers, chilled-water consumers and valves;
[0033] [0033]FIG. 2 is a schematic diagram the distribution system of FIG. 1 showing redundant chilled-water supply and return pipes leading to chilled-water consumers and chilled-water producers;
[0034] [0034]FIG. 3 is a block diagram of one chilled-water producer showing its components and sensors, including a heat exchanger, pump, accumulator tank, and flow and pressure sensors, which may be used to detect system failures and showing a connected control module implementing one or more autonomous control units associated with the chilled-water producer;
[0035] [0035]FIG. 4 is a detailed block diagram of one valve and optional sensor connected to a control module implementing an associated autonomous control unit and showing information held by the autonomous control unit during operation;
[0036] [0036]FIG. 5 is a flowchart depicting overall operation of the control system as implemented in a distributed fashion by many autonomous control units;
[0037] [0037]FIG. 6 is a figure similar to that of FIG. 2 showing operation of valve pricing to provide segregation of the chilled-water producers;
[0038] [0038]FIG. 7 shows an example configuration of the network of FIG. 2 such as may be developed by bidding autonomous control units which develop distribution paths;
[0039] [0039]FIG. 8 is a flowchart depicting operation of an individual autonomous control unit associated with a valve such as automatically develops the paths of FIG. 7;
[0040] [0040]FIG. 9 is a fragmentary view of additional steps in the flowchart of FIG. 8, such steps as prevent mixing of water between chilled-water producers;
[0041] [0041]FIG. 10 is a graph showing water level in the accumulator tank of FIG. 3 such as may be used to deduce slow failures of the system;
[0042] [0042]FIG. 11 is a graphical representation of a signature database that may detect more rapid failures of the system of FIG. 1; and
[0043] [0043]FIG. 12 is a depiction of a simplified network similar to that of FIG. 7 showing zones defined by the autonomous control units for isolation of a failure of the distribution network.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0044] Referring now to FIG. 1, a naval vessel 10 may include a chilled-water distribution system 12 having redundant and spatially separate chilled-water producers 14 a and 14 b providing chilled-water to multiple distributed chilled-water consumers 16 a through 16 c . The distribution is through a network of pipes 18 and control valves 20 such as to provide for multiple different paths of connection between any chilled-water producer 14 and chilled-water consumer 16 .
[0045] At times, particular chilled-water producers 14 , pipes 18 , or valves 20 may be destroyed or rendered inoperative. During operation, chilled-water consumers 16 may come on and go off-line at different times depending on their needs.
[0046] Referring now to FIG. 2, the two chilled-water producers 14 a and 14 b may each be connected to a supply pipe 18 a and a return pipe 18 b to provide a closed loop operation. Chilled-water producer 14 a is connected through valve 20 a to supply pipe 18 a and through valve 20 b to return pipe 18 b while chilled-water producer 14 b is connected through valve 20 c to supply pipe 18 a and through valve 20 d to return pipe 18 b . For the purpose of descriptive clarity, only the supply pipes 18 a and its valves 20 will be described henceforth with it being understood that corresponding return pipes 18 b and return pipe valves 20 will be present.
[0047] Directly connected to supply pipe 18 a , to receive constant water flow therefrom, are chilled-water consumers 16 a , 16 b and 16 g . Chilled-water consumers 16 a and 16 b are not subject to individual control but may be shut off by operation of valves 20 elsewhere in the system.
[0048] More importantly, other chilled-water consumers 16 c through 16 g may connect to the supply pipe 18 a through valves 20 allowing them to be individually connected and disconnected from chilled-water. Specifically, chilled-water consumer 16 c connected to supply pipe 18 a via valve 20 d , chilled-water consumer 16 d connects via valve 20 e , chilled-water consumer 16 e connects via valve 20 f , and chilled-water consumer 16 f connects via valve 20 g.
[0049] Generally, the chilled-water distribution system 12 is divided into redundant halves corresponding to the two chilled-water producers 14 a and 14 b . These halves are normally separated by segregation valves 20 h and 20 i , each associated with a pipeway branch 21 a and 21 b connecting the two halves, and 20 j and 20 k which connect in series across an additional branch 21 c between the two halves. Chilled-water consumer 16 g is connected at the junction of segregation valves 20 j and 20 k so as to freely receive chilled-water from either half. During normal operation, the segregation valves 20 h , 20 i , and 20 j and 20 k prevent mixing of chilled-water from chilled-water producer 14 a with chilled-water from chilled-water producer 14 b . This segregation provides an additional reliability against catastrophic failure of a pipe that, where the two halves join, might cause water loss to the entire system.
[0050] The topology of the network shown in FIG. 2 is generally arbitrary except that it allows different chilled-water producers 14 to be flexibly connected through valves 20 to a given chilled-water consumer 16 through at least two different pipeway paths. Thus, for example, chilled-water producer 14 a may provide chilled-water to chilled-water consumers 16 f by passing the water through valve 20 a , 20 h and valve 20 g , or alternatively, through valve 20 a , valve 20 j , 20 k , and 20 g . In this case, a third possible path is provided through valve 20 a , valve 20 i , and 20 g . Thus, damage to pipes in the system can be overcome. Higher degrees of redundancy and additional numbers of sources are also possible.
[0051] Referring now to FIG. 3, a given chilled-water producer 14 includes a heat exchanger/chiller 30 receiving heated water from a return pipe 18 b through a valve 20 ( 20 b or 20 d in the example of FIG. 2) and providing chilled-water to a pump 32 which in turn provides it to a valve 20 ′ ( 20 a or 20 c in the example of FIG. 2) to the supply pipe 18 a . The output of the pump 32 communicates with an accumulator tank 34 of a type well known in the art for closed loop water systems having a water level 36 that may be sensed by water level sensor 38 . The flow of water out of pump 32 may be detected by flow sensor 40 and the pressure of this water may be sensed by pressure sensor 42 .
[0052] Signals from water level sensor 38 , flow sensor 40 , and pressure sensor 42 may be received by input circuits of a control module 50 such as a ControlLogix programmable control module commercially available from Rockwell Automation, Inc., the beneficial assignee of the present invention. The control module 50 incorporates a computer processor and memory for implementing one or more autonomous control units (ACU's) as will be described. The control module 50 may also provide output circuits to provide signals controlling the pump 32 and operation of the chiller 30 using a control program “stub” being a part of each ACU implemented by the control module 50 , as will be described. The control module 50 may communicate by a single or multiple redundant networks 52 such as Control Net or Ethernet having separate network media to resist failure.
[0053] Autonomous Control of the Distribution Network
[0054] Referring now to FIG. 4, each valve 20 may also be connected to a control module 50 connected to network 52 so the control module 50 may operate the opening or closing the valve 20 using an associated ACU implemented by the control module 50 . In the simplest embodiment, the control module exchanges signals with the valve 20 only providing for operation of the valve and confirmation of that operation. In an alternative embodiment, however, as shown, the valve 20 may have an upstream pressure gauge 40 a and a downstream gauge 40 b which may provide signals to the control module 50 which may use these signals to deduce a pressure drop across the valve 20 indicating water flow. Knowing flow plus pressure can be used to deduce network conductance for detecting errors as will be described below.
[0055] Each chilled-water consumer 16 (shown in FIG. 3) may also be associated with an ACU implemented in a control module 50 . By means of the ACU, each chilled-water consumer 16 may initiate a request for chilled-water based on internal considerations, for example, a temperature rise in the associated equipment or an activation signal being received by the associated equipment.
[0056] Referring again to FIG. 4, the amount of application specific information that must be programmed into the ACU is limited allowing rapid configurations of distribution control systems. As mentioned, each ACU may include a control logic stub 54 , for example, implemented in relay logic or other common control program languages, that provides low level control of the valve 20 or chilled-water producer 14 or chilled-water consumer 16 and may include, in the case of a valve, logic for preventing both simultaneous opening and closing signals, for detecting valve jamming or other failure, monitoring safety, and allowing manual operation. The control logic stub may be pre-written as part of a library for a particular device such as a valve 20 or chilled-water producer 14 or chilled-water consumer 16 . The control logic stub 54 may also provide variable data holding certain status information about the associated device (e.g., valve open, valve closed, valve failure) that may be read by the ACU.
[0057] The ACU also includes limited application specific information about the pipeway topology in an ACU data area 55 . In the preferred embodiment, this topology information can be simply the identity of the ACU(s) associated with any upstream resources and the ACU(s) associated with any downstream resources. The cooperative operation of the ACU's allows this fragmentary information to be effectively assembled into knowledge about distribution paths. This limited need for information by the ACU's makes the system highly scalable and simple to implement in a variety of distribution systems. When the ACU data area is in an ACU associated with a chilled-water consumer 16 , it may also include a priority of the chilled-water consumer as will be described below which provides a stable resolution of conflicts between chilled-water consumers 16 as will be described below.
[0058] Each ACU also includes programs (not shown) that control the behavior of the ACU as an ACU in bidding responding to bids and communicating with other ACU's. Generally these programs are not application specific and thus do not require modification for each application. Communication between ACU's may be provided using standard protocols such as described by The Foundation for Intelligent Physical Agents (FIPA) (at www.fipa.org) communicating bidding and other messages as taught in U.S. Pat. No. 6,647,300 entitled: Bidding Partner Cache For Autonomous Cooperative Control System; U.S. Pat. No. 6,459,944 entitled: Self-Organizing Industrial Control System Using A Specific Process To Evaluate Bids; U.S. Pat. No. 6,430,454 entitled: Self-Organizing Industrial Control System Using Iterative Reverse Modeling To Evaluate Bids; U.S. Pat. No. 6,272,391 entitled: Self Organizing Industrial Control System Importing Neighbor Constraint Ranges, and U.S. patent application Ser. No. 2003/78678A1 entitled: Language Structure For Autonomous Cooperative Control System, each beneficially assigned to the present assignee and hereby incorporated by reference.
[0059] Referring now to FIG. 5, once each ACU is provided with its applications specific data, they may intercommunicate to organize themselves to distribute chilled-water in a bidding process. As indicated by start block 60 , bidding may be initiated upon start-up of the system, a chilled-water consumer 16 (or other new resource) coming on-line, or by loss of a resource by failure or damage. The most common example will be that of a chilled-water consumer 16 requesting chilled-water as it reaches a threshold temperature at which cooling is required. At this time, chilled-water consumer 16 creates a bid request as indicated by process block 62 which is forwarded to other resources that might satisfy the bid request. The requirements of the bid request are expressed in a job description language of a type described in the above-referenced patents and in this case simply describing the need for a chilled-water source, a distribution path to a particular destination, at under a particular money limit. The other resources to which bid requests are sent are found by consulting a directory providing addresses of other ACU's having the capabilities required in the bid request.
[0060] In the present invention the bid request is initially forwarded only to chilled-water producers 14 a and 14 b . Chilled-water producers 14 keep track of their current loads in the form of executing bids from other chilled-water consumers 16 and will only accept a bid request if they have uncommitted capacity, or if the bid request comes from a chilled-water consumer 16 having a priority higher than a priority of existing chilled-water consumers 16 serviced by the chilled-water producer 14 . In this latter case, the lowest priority chilled-water consumer is notified to disconnect itself.
[0061] At process block 64 each of the chilled-water producer 14 a and 14 b , having possibly satisfied the bid request requirements of providing a source of chilled-water (depending on their status and current loads), send sub-bid requests to valves 20 that might satisfy the bid request requirement of a path to the destination. The valves 20 stand as proxies for the pipes to which they are connected. Each valve 20 examines the bid request requirements, the available money, and makes a determination whether it can respond.
[0062] When a given ACU completes a bid request, typically a valve connected to the chilled-water consumer 16 making the request, the bid response and path (listing each of the resources in order from source to destination) describing a “job response” are collected and returned to the chilled-water producer 14 . Bid requests that cannot complete in a given time or other limit, or for reasons of excess cost, are abandoned.
[0063] At process block 66 , a determination is made by each chilled-water producer 14 a and 14 b as to the best job response meeting the price and capability requirements. Under a commonly implemented money rule for each bidder (e.g. a chilled-water consumer 16 ), the bid request may be associated with a money limit which is either an arbitrarily chosen initial amount (e.g. 700) or a number slightly above the last successful job response for this chilled-water consumer 16 . This latter rule encourages efficient bidding (by quickly truncating expensive paths), and system stability (by encouraging repeated use of previous solutions as characterized by price).
[0064] If no job responses have been provided (e.g. no bid requests have successfully completed) at the given money limit, then at process block 68 , the money limit is increased under a commonly implemented money rule and the process repeated until a success is obtained at decision block 66 and the winning bid response is implemented at the execute block 70 .
[0065] Referring to FIG. 6 in the present invention, the cost of a job response in the preferred embodiment is determined by a pricing rule that considers simply the sum of the cost of each valve 20 needed to connect the chilled-water producer 14 to the chilled-water consumer 16 . Alternative cost mechanisms which consider the flow characteristics of the paths, for example, their hydrodynamic resistance, or other characteristics can also be used. In the preferred embodiment of the invention, the segregation valves 20 are given a higher price (e.g. 1,000) than the price (e.g. 100) of other valves 20 that do not serve in the capacity of segregation. As a result, successful job responses will tend to use valves 20 other than the segregation valves 20 thus preserving segregation between the two halves of the chilled-water distribution system 12 to the extent possible. As mentioned above, however, if a successful job response cannot be found without using segregation valves, for example because of extensive damage to the chilled-water distribution system 12 , then the raising of the price at process block 68 of FIG. 5 raises the amount that can be bid to a much higher amount, e.g., 7,000, to ensure that chilled-water can be obtained in these circumstances.
[0066] Referring to FIG. 7, in order to reduce the number of bid requests processed, bid requests are only sent to valves connected by pipeways to the chilled-water producers 14 a and 14 b , that is, the bid requests follow the physical pathways of the distribution network. This pathway is collectively known by valves 20 which, as has been described, each know their upstream and downstream connection. Thus chilled-water producer 14 S 1 may be connected by pipes 18 to valve V 1 and valve V 2 and accordingly forwards the job description language bid request only to valve V 1 and valve V 2 and not from valves 20 to which it is not connected by pipes 18 . Likewise, valve V 1 may be connected to valve V 3 and therefore forwards a bid request only to that valve, while valve V 2 may be connected to valve V 4 and valve V 5 and therefore forwards bid requests only to those valves 20 .
[0067] Referring now to FIG. 8, a given ACU receiving a bid request, as indicated by process block 72 , after it determined that it has the necessary capability, evaluates whether the total price of the bid responses as so far accumulated exceeds the income limit as determined by decision block 74 . If the total price is too high at this point, the bid is truncated as indicated by process block 76 .
[0068] On the other hand, if the total price is acceptable, then at decision block 78 the ACU checks to see if the bid request is complete (e.g. the path is complete) as described in the job description of the bid request. If so, a success message is returned as indicated by process block 80 indicating the completed path, its cost, and the fact that it is a complete bid response. The ACU returns the successful bid response including the path and the total price. ACU's may contribute to a bid response even if they are already committed to another executing bid so long as the response does not require a change of state of the valve 20 .
[0069] If the bid is not complete, then the ACU proceeds to decision block 82 . Decision block 82 determines that the bids are only sent to valves that are not already on the bid path so as to prevent the possibility of loops. If the sub-bid will not create a loop, a sub-bid request is forwarded to these other ACU's that have the necessary capabilities and might complete the bid as indicated by process block 84 . These sub-bids requests follow the topology of the actual distribution network as indicated and described above with respect to FIG. 7.
[0070] Referring now to FIG. 9, an additional decision block 86 may be placed in the program of FIG. 8 in the event that it is desired to preserve segregation of the chilled-water producers 14 . As will be recalled with respect to FIG. 6, some segregation is preserved by increasing the relative price of the segregation valves 20 with respect to other valves 20 . In the preferred embodiment, in the event the segregation valves 20 must be used, mixing of the water from chilled-water producers 14 is prevented by a polling between valves before they contribute to a bid. At decision block 86 , before an ACU can join in a bid response, it must seek approval from directly connected valves 20 as indicated by decision block 88 . Other valves must grant approval if they are closed, or if they are open and receiving water from the same chilled-water producers 14 .
[0071] If at decision block 88 there are objections from any other valve 20 , the bid is truncated as described above.
[0072] Referring now again to FIG. 2, as mentioned, the bid process may be initiated per process block 60 whenever chilled-water consumers 16 come on-line. Conversely, when a chilled-water consumer 16 goes off line, its valve may simply be opened and the commitment to the bid dissolved freeing up resources. Bids may also be initiated when new chilled-water sources 14 are added (for example during an upgrading process) eliminating the need for additional programming. Similarly, when a new valve 20 is added, it may automatically be incorporated into the system (after its connections have been programmed) during the next bid.
[0073] Active Diagnostics
[0074] The bidding process may also be initiated when a failure has been detected and the configuration of the chilled-water distribution system 12 must be changed. This detection may be the result of a chilled-water consumer 16 losing water and renewing a bid. Failed chilled-water producers 14 or valves 20 have self-diagnostics which may remove them from the bidding process. Alternatively, certain valves 20 may be manually removed from the system or placed in a lock mode (for example, to cordon off a leaking pipe) which also will remove them from participating in bids. The bidding process will automatically proceed to reconfigure the chilled-water distribution system 12 appropriately using the rules described above in light of such lost resources of valves or producers.
[0075] The present invention also contemplates anticipatory responses that may be taken by detecting failure before the loss of cooling water is noticed at the chilled-water consumers 16 . In this regard, the present invention considers two methods of determining failure.
[0076] Referring to FIGS. 3 and 10, in the first method, the tank water level 36 is tracked over time and if a predetermined decrease occurs within a predetermined time, it is assumed that there is a slow leak because the chilled-water system is closed. Normal tank level fluctuations are thus distinguished from significant but slow leaks that would be anticipated to produce a problem in the future.
[0077] Referring to FIGS. 11 and 3, the present invention also contemplates a detection system with faster response that may detect rapid drop in water pressure as indicating a failure. Generally, it must be understood that the water pressure fluctuates significantly depending on how many and which chilled-water consumers 16 are on line and depending on the particular connection of pipes 18 . Thus, for example, three given chilled-water consumers 14 will provide a different pressure drop than three different chilled-water consumers 14 or the same three chilled-water consumers 14 connected via a different valve configuration. Further, water hammer effects cause pressure surges when valves open and close. Thus, no fixed threshold of pressure detection will suffice to detect rapid pressure drops caused by pipe failure.
[0078] Accordingly, the present invention provides a learning algorithm that may be implemented at any ACU that has pressure and flow monitoring capability. In this technique, a signature flow/pressure range 63 (indicating a conductance of the pipes of the system) is developed on a continuous learning basis for each combination of chilled-water consumer and each configuration of the pipes. These signatures may be collected in a table or functional surface that is updated when that combination occurs during normal operations (as validated by no failures occurring within a subsequent predetermined time) or during a training period when the resources are cycled through combinations. This learning is facilitated by the fact that the present system tends toward repeating configurations as a result of the money rules described above.
[0079] Once some number of signatures is developed, the conductance of the system is monitored with respect to the range for the signature associated with that particular load combination at a time after settling of any water hammer effects. Pressure deviation outside of that range triggers a failure signal.
[0080] The failure may be isolated manually once brought to the attention of human operators and segregated by locking closed some valves 20 . Preferably, however, the isolation of the failure is done automatically making use of the ACU architecture. Referring now to FIG. 12, a chilled-water producer S 1 may detect a pressure drop either through monitoring the tank per FIG. 10 or monitoring of the pressure zones per FIG. 11 indicating a leak. Alternatively, this process may be initiated by any ACU having tank or flow/pressure sensors.
[0081] Each ACU including S 1 has a copy of the paths associated with all executing bids and from these paths. S 1 may perform a simple tree based search for the source of leakage by selectively opening and closing valves 20 on those paths. For example, S 1 may instruct valve V 1 to close momentarily to see if the problem is remedied as manifested by the detection methods of FIG. 10 or 11 . If so, the problem is below valve V 1 , if not, the problem exists between S 1 and V 1 , and V 1 may be locked or closed (removed from the bidding) and a rebidding process undertaken to reallocate the other chilled-water consumers 14 .
[0082] If the closing of valve V 1 does correct the problem, valve V 2 may be closed to see if the problem has been remedied. If it has been remedied, the problem exists below valve V 2 , in this case between valve V 2 and V 4 . Valve V 2 may then be closed to try to isolate the problem. If this doesn't work, the problem exists between valve V 1 and valve V 2 or valve V 1 and valve V 3 . In this case, valves V 1 , V 2 , and V 3 would need to be closed to accommodate the problem and a report indicating this problem can be forwarded to a monitoring system.
[0083] Referring momentarily to FIG. 4, if each valve 20 is instrumented to provide for pressure sensing and thus flow detection, the initiation of this isolation and detection may occur at any valve 20 as well. Desirably multiple ACU's will be equipped to provide this capability to prevent loss of centralized hardware.
[0084] A similar approach may be used to detect blockage of pipes in the event that the pressure has increased and these analogous processes may be affected on the return pipes 18 b as will be understood from this description by one of ordinary skill in the art.
[0085] It is specifically intended that the present invention not be limited to the embodiments and illustrations contained herein, but include modified forms of those embodiments including portions of the embodiments and combinations of elements of different embodiments as come within the scope of the following claims. In particular, the present invention should be applicable to other types of distribution networks including those which distribute other materials such as fuel or air and those which distribute electrical power in the form of current under a voltage analogous to the pressure driving material fluids through a pipe. | A control system for a complex distribution network uses autonomous control units that may bid among themselves to reconfigure the distribution network in light of fluctuation demand or failures. The autonomous control units may also be enlisted to detect and isolate as well as reconfigure the network to correct for the damage. | 1 |
CROSS-REFERENCE TO RELATED APPLICATION(S)
This patent application claims priority to Provisional U.S. Patent Application Ser. No. 61/781,196, filed Mar. 14, 2013, which is herein incorporated by reference in its entirety.
FIELD OF THE INVENTION
The invention generally relates to surgical staplers and stapling devices.
BACKGROUND
An endocutter is a surgical tool that staples and cuts tissue to transect that tissue while leaving the cut ends hemostatic. An endocutter is small enough in diameter for use in minimally invasive surgery, where access to a surgical site is obtained through a trocar, port, or small incision in the body. A linear cutter is a larger version of an endocutter, and is used to transect portions of the gastrointestinal tract. A typical endocutter receives at its distal end a disposable single-use staple cartridge with several rows of staples, and includes an anvil to oppose and deform the deployed staples in the staple cartridge. The staples may be held in individual pockets, with staple drivers underneath each staple. As a wedge advances into the cartridge, that wedge sequentially pushes a number of staple drivers upward, and the staple drivers in turn both linearly push each corresponding staple upward out of its pocket, deforming it against an anvil.
During actuation of an endocutter, the cartridge fires all of the staples that it holds. In order to deploy more staples, the endocutter must be moved away from the surgical site and removed from the patient, after which the old cartridge is exchanged for a new cartridge. The endocutter is then reinserted into the patient.
SUMMARY OF THE INVENTION
A surgical stapling device is configured for use in open and/or laparoscopic surgical procedures. The device includes a staple holder with a first support element and a second support element for supporting a continuous staple chain. Each staple of the staple chain is configured to be frangibly separated from the staple chain to pierce and secure a target tissue when each staple is deployed. The device also includes a plurality of standoff members wherein each of the plurality of standoff members is configured to support one of each staple of the staple chain when the one of each staple is being deployed. The surgical stapling device may be a cartridge-based or a cartridge-less staple device.
As mentioned, a staple holder of the surgical stapling device may include a first support element and a second support element for supporting a continuous staple chain that is belt-less or without a feeder belt. The first support element may provide lateral support to the staple chain, while the second support element provides vertical support to the staple chain. In addition, each of the plurality of standoff members may be respectively coupled to the first support element along various locations or positions along a length or surface of the first support element. The arrangement is such that each staple of the staple chain is being held in place by a respective or corresponding standoff member while one of each staple of the staple chain is being deployed. The arrangement of the staple chain is that each staple of the staple chain is frangibly coupled to at least one other staple of the staple chain. The staple chain is comprised of an end portion of one of each staple of the staple chain being frangibly coupled to a head portion of another one of each staple of the staple chain. One of each staple of the staple chain is frangibly separated from another one of each staple of the staple chain at a frangibly connection region, location, or point when the one of each staple of the staple chain is being deployed. The frangibly connection region, location, or point is where an end portion of one of each staple of the staple chain meets, connects, couples, or joins to a head portion of another one of each staple of the staple chain. A wedge element, being deployed within the staple holder, configured to directly act on or push each staple of the staple chain to deploy each staple.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a perspective view of an exemplary cartridge and exemplary wedge assembly.
FIG. 2 illustrates a top cutaway view of the exemplary cartridge of FIG. 1 .
FIG. 3 illustrates a perspective cutaway view of the exemplary cartridge of FIG. 1 .
FIG. 4 illustrates a side cross-section view of the exemplary cartridge of FIG. 1 , with staples omitted for clarity.
FIG. 5 illustrates a schematic view of an endocutter utilizing a feeder belt connected at each end to a different rigid rack.
FIG. 6 illustrates a schematic view of an endocutter utilizing a feeder belt connected at each end to a single flexible rack.
FIG. 7 illustrates a schematic view of an endocutter utilizing a feeder belt connected at each end to a single flexible rack, where staples extend from the flexible rack.
FIG. 8 illustrates a top view of an exemplary feeder belt configured to engage a gear.
FIG. 9 illustrates a side view of an exemplary continuous feeder belt.
FIG. 10 illustrates a side view of an exemplary belt-less staple chain.
FIG. 11 illustrates a close-up side view of the exemplary belt-less staple chain.
FIG. 12 illustrates a perspective view of an exemplary belt-less staple chain.
FIG. 13 illustrates a close-up perspective view of the exemplary belt-less staple chain.
FIG. 14 illustrates one example of mounting an exemplary belt-less staple chain on a staple cartridge or mounting provisions in a cartridge-less stapling device.
FIG. 15 illustrates a close-up view of one example of mounting the exemplary belt-less staple chain.
FIG. 16 illustrates a perspective view of mounting an exemplary belt-less staple chain on a staple cartridge or mounting provisions in a cartridge-less staple device.
FIG. 17 illustrates a close-up perspective view of mounting the exemplary belt-less staple chain on a staple cartridge or mounting provisions in a cartridge-less staple device.
FIG. 18 illustrates a further close-up view of the belt-less staple chain and mounting provisions.
FIG. 19A and FIG. 19B illustrate one example of belt-less staple chains mounted in a staple cartridge.
FIG. 20A through FIG. 20E illustrate staple deployment of staples on an exemplary belt-less staple chain by a wedge element.
FIG. 21A and FIG. 21B illustrate one example of an end effector or distal portion of a stapling device using a belt-less staple chain.
FIG. 22A and FIG. 22B illustrate another example of an end effector or distal portion of a stapling device using a belt-less staple chain.
FIG. 23 illustrates one example of a stapling device using a belt-less staple chain.
The use of the same reference symbols in different figures indicates similar or identical items.
DETAILED DESCRIPTION
U.S. patent application Ser. No. 12/400,790, entitled “True Multi-Fire Surgical Stapler Configured to Fire Staples of Different Sizes”, filed on Mar. 9, 2009 (the “Feeder Belt Document”), is hereby incorporated by reference herein in its entirety. The Feeder Belt Document describes exemplary feeder belts used in a surgical stapler, to which plurality of staples are frangibly connected. Because new staples are fed to an end effector of a surgical stapler by the feeder belts for sequential deployment, the surgical stapler of the Feeder Belt Document does not need or utilize plurality of single-use cartridges in order to deploy multiple sets of staples.
As is commonly used in the medical device industry, particularly in the surgical stapler business, the term “cartridge” means, and is expressly defined in this document to mean, a portion of a surgical stapler that holds at least one staple, and that is insertable within and releasably connected to a remainder of the surgical stapler. Referring to FIG. 1 , an exemplary cartridge 2 is shown, along with an exemplary wedge assembly 4 and knife 6 . The cartridge 2 may be utilized in conjunction with any surgical stapler that is capable of receiving it, and that includes at least a wedge assembly 4 capable of moving into the cartridge 2 to deploy staples (as described in greater detail below) and then moving out of the cartridge 2 to allow the spent cartridge 2 to be removed from the surgical stapler. The cartridge 2 may be received in a remainder of a surgical stapler in any suitable manner, such as by a pressure fit or interference fit; passively or affirmatively; or in any other suitable manner. The cartridge 2 may be received at the distal end of a remainder of the surgical stapler, and/or along the side of a remainder of the surgical stapler. The cartridge 2 may be useful in conjunction with an articulated surgical stapler having an articulation proximal to the location at which the cartridge is attached to the stapler. Such an articulation may be, for example, as described in U.S. patent application Ser. No. 12/400,760, entitled “Articulated Surgical Instrument”, filed on Mar. 9, 2009, or in U.S. patent application Ser. No. 12/612,614, entitled “Surgical Stapler with Variable Clamp Gap”, filed on Nov. 4, 2009, both of which are hereby incorporated by reference in their entirety.
The cartridge 2 may be shaped in any suitable manner. As one example, the cartridge 2 may include an upper surface 8 . The upper surface 8 may be generally flat, and generally rectangular. However, the upper surface 8 need not be generally flat along all or part of its area, and may be shaped in a manner other than rectangular. Further, the upper surface 8 need not be a discrete part of the cartridge 2 , and instead simply may be a portion of a larger surface or area of the cartridge 2 . The upper surface 8 of the cartridge 2 may include a plurality of openings 10 defined completely therethrough. As described in greater detail below, each opening 10 may be aligned with a corresponding staple, such that a staple may be deployed through each opening 10 . Each opening 10 may be generally longitudinally-oriented, and generally rectangular in shape. Alternately, the orientation and/or shape of at least one opening 10 may be different from the other openings 10 . The openings 10 may be organized into one or more generally-longitudinally-oriented rows, corresponding to the locations of staples in the cartridge 2 . As another example, the openings 10 may be interconnected to form one or more larger openings, such that more than one staple may be deployed through a single opening 10 . Alternately, the upper surface 8 may be omitted altogether, thereby rendering openings 10 superfluous.
Referring also to FIGS. 2-4 , the cartridge 2 also may include one or more rails 12 . The rails 12 may be oriented generally longitudinally, and may be shaped generally as rectangular solids. At least one rail 12 may be dimensioned greater in lateral width than in vertical height, as seen most clearly in FIG. 3 . As another example, at least one rail 12 may be oriented and/or shaped in any other suitable manner. The rails 12 may be spaced laterally apart from one another. The rails 12 may be fabricated from any suitable material, and in any suitable manner. At least one rail 12 may be vertically spaced apart from the upper surface 8 of the cartridge 2 by a gap 14 . One or more pins 17 may extend from at least one rail 12 across the gap 14 to the upper surface 8 . The pins 17 may be fabricated integrally with the corresponding rail 12 and/or upper surface 8 , or may be fabricated separately and later connected thereto. At least one pin 17 may be generally cylindrical in shape. However, at least one pin 17 may be shaped differently. The pins 17 advantageously are shaped the same as one another, but at least one pin 17 may be shaped differently than at least one other pin 17 .
A plurality of staples 16 may be affixed to and frangibly separable from the cartridge 2 . The staples 16 may be shaped substantially in the same manner as the staples described in the Feeder Belt Document, or may be shaped in any other suitable manner. Each staple 16 may have a free end 18 , and an opposite end 20 that is connected to a stem 22 . The portion of the staple 16 between the free end 18 and the opposite end 20 may be referred to as the tine 24 . The stem 22 of at least one staple 16 may be substantially perpendicular to the tine 24 of that staple 16 . As another example, the stem 22 and tine 24 of a staple 16 may be oriented at a different angle to one another. The stem 22 may be substantially planar and rectangular, but may be shaped differently if desired. Each tine 24 may be fixed to the corresponding stem 22 . Advantageously, the tine 24 and corresponding stem 22 are integral, and may be fabricated by stamping a piece of flat sheet metal, then bending the tine 24 and the stem 22 to the desired angle relative to one another. Advantageously, each staple 16 is positioned on a corresponding rail 12 , such that the stem 22 is positioned on top of that rail 12 . The thickness of the stem 22 may be substantially the same as the height of the gap 14 between each rail 12 and the upper surface 8 . Alternately, the thickness of at least one stem 22 may be less than the height of the gap 14 between each rail 12 and the upper surface 8 . Each staple 16 may be fixed to the upper surface 8 of the cartridge and/or to a rail 12 , in any suitable manner. As one example, at least one stem 22 may include at least one aperture 26 defined therethrough. That aperture 26 may receive a corresponding pin 17 that extends from the upper surface 8 to a rail 12 . As another example, at least one stem 22 may be welded to the top of a corresponding rail 12 and/or to the bottom of the upper surface 8 . As another example, at least one stem may be affixed to the top of a corresponding rail 12 and/or to the bottom of the upper surface 8 by adhesive. As another example, at least one stem 22 may be pressure-fit between the upper surface 8 and the corresponding rail 12 . As another example, at least one stem 22 may be fixed to a corresponding rail 12 and/or the upper surface 8 in two or more ways, such as, for example, by welding and by receiving a pin 17 through an aperture 26 in the stem 22 . At least one staple 16 may be fabricated separately from a remainder of the cartridge 2 , then affixed to the cartridge 2 as set forth above. Alternately, at least one staple 16 may be integral with a remainder of the cartridge 2 .
The staples 16 may be arranged in the cartridge 2 in any suitable manner. As one example, one or more staples 16 may be arranged against a corresponding rail 12 , with each stem 22 fixed to the corresponding rail 12 . The staples 16 may be arranged relative to the rail 12 and to one another such that the tine 24 extending from a particular staple 16 is positioned on one lateral side of the rail 12 , and the tine 24 extending from each longitudinally-adjacent staple 16 is positioned on the other lateral side of the rail 12 . In this way, the tines 24 alternate sides relative to the rail 12 longitudinally along the rail 12 , as seen most clearly in FIGS. 2-3 . As another example, each staple 16 may include a single stem 22 , with two tines 24 extending from it. Each tine 24 may extend from a lateral side opposed to the other. The stem 22 may be positioned on top of a rail 12 , with each stem 22 fixed to the corresponding rail 12 , and with each tine 24 positioned on a different lateral side of the corresponding rail 12 . One tine 24 may be positioned longitudinally distal to the other tine 24 extending from the same stem 22 . Such staples 16 may be arranged relative to the rail 12 such that the tines 24 alternate sides relative to the rail 12 longitudinally along the rail 12 . As another example, at least one staple 16 is integral with the upper surface 8 , and is affixed to a remainder of the upper surface 8 at the end 20 of the tine 24 . In such a configuration, the staple 16 may be fabricated by punching, stamping, or otherwise dislodging it from the upper surface 8 , such that the staple 16 extends from one end of a corresponding opening 10 in the upper surface 8 , and the opening 10 results from the fabrication of the staple 16 associated with it. Further, in such a configuration, the stem 22 may be omitted from the staple 16 . Regardless of the particular configuration of the staples 16 , each tine 24 may be positioned adjacent to a corresponding opening 10 in the upper surface 8 , and/or may be affixed to the upper surface 8 in proximity to the corresponding opening 10 .
At least part of each staple 16 may be frangibly affixed to a remainder of the cartridge 2 . “Frangibly affixed” is defined to mean that at least part of each staple 16 is fixed to a remainder of the cartridge 2 in such a manner that it must be sheared or otherwise broken off from a remainder of the cartridge 2 to be removed therefrom. As one example, at least one staple 16 may be frangible at the junction between the stem 22 and the tine 24 . Such a junction may have a weakened area to facilitate frangibility. As another example, at least one staple 16 may remain intact during deployment, and the stem 22 of the staple 16 is frangible from the corresponding rail 12 and/or the upper surface 8 . As another example, where the tine 24 is integral with the upper surface 8 , the tine 24 may be frangible at the junction between the tine 24 and the upper surface 8 .
The cartridge 2 may be actuated, and the staples 16 deployed, substantially as set forth in the Feeder Belt Document, with the following general differences. The wedge assembly 4 includes one or more wedges 30 configured generally as set forth in the Feeder Belt Document. Initially, the wedge or wedges 30 may be positioned proximal to the cartridge 2 . In this way, the wedge or wedges 30 do not interfere with the insertion of the cartridge 2 into a remainder of the surgical stapler. The cartridge 2 may be inserted into the stapler, or may already be present in the stapler, prior to actuation of the stapler. The wedge assembly 4 is moved distally, advantageously by sliding. As the wedge assembly 4 moves distally, it slides the wedge or wedges 30 distally as well. Advantageously, one wedge 30 slides along a corresponding row of staples 16 to sequentially deform staples 16 outward through the corresponding openings 10 in the upper surface 8 , and then break staples 16 from the cartridge 2 . Such deformation and later breakage of the staple may be as set forth generally in the Feeder Belt Document. As one example, the stem 22 of one or more staples 16 is held substantially in place by its affixation to a corresponding rail 12 and/or to the upper surface 8 , as set forth above. As a wedge 30 slides distally relative to the staple 16 , the wedge 30 first engages the tine 24 of that staple 16 , causing the tine 24 to move upward and to rotate about the junction between the tine 24 and the stem 22 . Rotation of the tine 24 upward causes the tine 24 to move up through a corresponding opening 10 in the upper surface 8 , through tissue, and then move into contact with an anvil (not shown), such as set forth in the Feeder Belt Document. Contact between the tine 24 and the anvil deforms the tine 24 to its closed configuration. As the wedge 30 continues to move distally relative to the staple 16 , both the wedge 30 and the tine 24 may be shaped such that the wedge 30 may continue to contact and exert force on the tine 24 after the tine 24 has been deformed. This force increases until the tine 24 is broken, sheared or otherwise separated from the stem 22 . As another example, this force increases until the stem 22 is broken, sheared or otherwise separated from a remainder of the cartridge 2 , such as from a corresponding rail 12 and/or the upper surface 8 of the cartridge 2 . The wedge 30 thereby may sequentially separate the frangible staples 16 from a remainder of the cartridge 2 .
A knife 6 also may be connected to the wedge assembly 4 , and may slide upward through the corresponding knife slot 32 in the upper surface 8 as the wedge assembly 4 moves distally through the cartridge 2 . The knife 6 may be actuated, and may cut tissue, substantially as set forth in the Feeder Belt Document. Optionally, the knife 6 may be omitted from the wedge assembly 4 , if desired. The knife 6 may be configured to move into the cartridge 2 , then move upward through and out of the knife slot 32 , then slide along the knife slot 32 , then move downward through the knife slot 32 . In this way, the knife 6 may be held in a position in which it does not extend through the knife slot 32 both before and after it has cut tissue, in order to enhance safety for the user and the patient.
After the wedge assembly 4 has been actuated to deploy one or more of the staples 16 , the cartridge 2 is spent. The wedge assembly 4 then may be retracted proximally through and then out of the proximal end of the cartridge 2 . The spent cartridge 2 then may be removed from a remainder of the surgical stapler. If desired, a new cartridge 2 may then be inserted into the surgical stapler in place of the previous, spent cartridge 2 . The new cartridge 2 may be actuated substantially as described above.
In addition, Cardica, Inc. of Redwood City, Calif. has developed a true multi-fire endocutter that is capable of firing multiple times without the need to utilize single-use-cartridges. That is, the true multi-fire endocutter is a cartridge-less device capable of firing multiple sets of staples without the need of reloading a new cartridge of staples for repeated firing. An example of such an endocutter is described in U.S. patent application Ser. No. 12/263,171, entitled “Multiple-Use Surgical Stapler”, filed on Oct. 31, 2008 (the “Endocutter Application”), which is hereby incorporated by reference in its entirety.
Referring to FIG. 5 , the Endocutter Application, among other items, discloses a feeder belt 52 to which a plurality of staples 54 are frangibly attached. The feeder belt 52 bends around a pulley 56 at its distal end. Each end of the feeder belt 52 is connected to a different rigid, toothed rack 58 , and each rack engages a gear 50 . The racks 58 are substantially rigid, and as a result, advancement of one rack 58 causes the gear 50 to rotate and thereby move the other rack 58 in the opposite direction. The gear 50 is located in a shaft 62 of the tool, between the handle and a distal end of the shaft. Because the racks 58 are substantially rigid, the linear travel of the racks 58 is limited by the length of the shaft 62 and of the handle connected to the shaft. Consequently, the number of firings that can be made by the tool is limited by the linear distance that the racks 58 can travel within the shaft 12 and structure connected to the shaft 12 .
Continuous Feeder Belt Assembly with Flexible Rack
Referring to FIG. 6 , a feeder belt 52 bends around a pulley 56 at its distal end, such that an upper portion 64 of the feeder belt 52 is above and spaced apart from a lower portion 66 of the feeder belt 52 . The upper portion 64 and lower portion 66 of the feeder belt 52 may be, but need not be, substantially parallel to one another. The upper portion 64 and lower portion 66 of the feeder belt 52 each have a proximal end, and the proximal end of each portion 64 , 66 may be connected to a flexible rack 68 . That is, the feeder belt 52 is connected at each end to a flexible rack 68 . The combination of the feeder belt 52 and the flexible rack 68 may be referred to as the belt assembly 70 . The belt assembly 70 is continuous, meaning that the belt assembly 70 defines a continuous, unbroken loop. The flexible rack 68 may be flexible in any suitable manner. As one example, the flexible rack 68 may be made from a flexible material with sufficient strength and other material properties to allow it to bend around the gear 50 , and to be attached to and exert tension on the feeder belt 52 . As another example, the flexible rack 68 may be a chain or other mechanism with individual, small links that are themselves rigid but that are collectively flexible. As another example, the flexible rack 68 may be fabricated from nickel-titanium alloy or other superelastic material.
Where the flexible rack 68 is utilized, the gear 50 may be located at the proximal end of the continuous belt assembly 70 . In this way, the gear 50 may be utilized to tension the feeder belt 52 between the gear 50 and the pulley 56 at the distal end of the feeder belt 52 . If so, the gear 50 may be located at or near the proximal end of the shaft 62 , which may be held within a handle 74 , or may be located proximal to or outside the shaft 62 inside the handle 74 or other structure attached to the shaft 62 . Further, the initial position of the feeder belt 52 may be as shown in FIG. 6 , where staples 54 extend from the upper portion 64 of the feeder belt 52 along substantially all of the upper portion 64 . In this way, the feeder belt 52 is able to include more staples 54 along its length than the feeder belt 52 of FIG. 5 , such that more staple firings can be made with a single feeder belt 52 .
The feeder belt 52 may be assembled into an endocutter or other surgical apparatus, and may be actuated by that endocutter or other surgical apparatus, substantially as described in the Endocutter Application. Optionally, the gear 50 may be directly driven by a handle such as described in the Endocutter Application, thereby reducing the number of parts and simplifying the overall assembly relative to that handle.
Optionally, referring also to FIG. 7 , staples 54 may be frangibly connected to the flexible rack 68 as well as to the feeder belt 52 . The staples 54 may be connected to the flexible rack 68 in substantially the same manner as described in the Endocutter Application. Alternately, the staples 54 may be connected to the flexible rack 68 in any other suitable manner. Where staples 54 are carried by the flexible rack 68 , the upper portion 64 of the feeder belt 52 may be spaced apart from the lower portion 66 of the feeder belt 52 a distance sufficient that the staples 54 extending from each portion 64 , 66 do not interfere with or engage one another. Alternately, the staples 54 instead, or also, may be laterally spaced relative to one another, such that in the initial position of the feeder belt 52 , the staples 54 extending from the upper portion 64 of the continuous belt assembly 70 are laterally spaced a first distance from a longitudinal centerline of that continuous belt assembly 70 , and the staples 54 extending from the lower portion 66 of the continuous belt assembly 70 are laterally spaced a second distance from a longitudinal centerline of that continuous belt assembly 70 , where the first distance and the second distance are sufficiently different from one another that the staples 54 extending from different portions 64 , 66 pass by one another without colliding or interfering with one another during actuating of the continuous belt assembly 70 . That is, the continuous belt assembly 70 is arranged in any suitable manner such that the staples 54 along the feeder belt 52 and the flexible rack 68 of the continuous belt assembly 70 do not interfere with one another.
Alternately, where staples 54 extend from the flexible rack 68 , the feeder belt 52 may be omitted, such that the flexible rack 68 is continuous and holds and deploys all of the staples 4 .
Rack-Less Continuous Feeder Belt Assembly
Referring to FIG. 8 , a feeder belt 52 such as described in the Endocutter Application may include a plurality of apertures 76 defined therein. The apertures 76 may be sized, shaped and spaced apart from one another such that they engage teeth on the gear 50 . The feeder belt 52 is sufficiently flexible to wrap around and be driven around the pulley 56 , and consequently is sufficiently flexible to wrap around and be driven by or around the gear 50 . In such an embodiment, the rack or racks 58 , 68 may be omitted, and the feeder belt 52 is itself continuous and forms a continuous loop, as shown in FIG. 9 . Alternately, the apertures 76 may be omitted, and the underside of the feeder belt 52 may include teeth similar to one of the racks 58 , 68 configured to engage the gear 50 . Alternately, the apertures 76 may be omitted, and the feeder belt 52 may be held in tension or otherwise manipulated such that the flat feeder belt 52 is capable of being advanced without the use of features on the feeder belt 52 configured to engage a gear, or without the use of a rack 58 , 68 connected to or otherwise engaging the feeder belt 52 .
Belt-Less Staple Chain
Referring to FIG. 10 and FIG. 12 , a continuous belt-less staple chain 100 may be used for both cartridge and cartridgeless applications in stapling devices, an example of a stapling device 230 is illustrated in FIG. 23 . The belt-less staple chain 100 may not require a feeder belt, hence it is belt-less. Instead, the staples 54 are frangibly connected to each other such that they do not need to be connected to a feeder belt. For example, a substantially sharp-end or tail-end 102 of one staple 54 is frangibly connected to a substantially dull-end or head-end of the next staple 54 in the staple chain 100 at a frangible connection 106 , as illustrated in FIG. 11 and FIG. 13 .
FIG. 14 and FIG. 16 illustrate one example of positioning or mounting the belt-less staple chain 100 , in a cartridge or a cartridge-less system. For example, the belt-less staple chain 100 may be supported by a lateral support element 142 and a bottom support element 144 , as illustrated in FIG. 14 , FIG. 15 , FIG. 16 , and FIG. 17 . The lateral support element 142 may be a support rail, a support strip, or any suitable support element that can provide lateral support to the belt-less staple chain 100 . The lateral support element 142 may be an element or component of a staple cartridge, in a cartridge-based staple device. Alternatively, the lateral support element 142 may be an element or component within an application shaft of a cartridge-less based staple device. As described and can be appreciated, the bottom support element 144 may be a surface of a staple cartridge, such as a bottom surface or any surface that can provide vertical support to the belt-less staple chain 10 , in either a cartridge-based staple device or a cartridge-less based staple device.
FIG. 18 illustrates a close-up view of the connection point between two staples in a belt-less staple chain 100 . As illustrated, a tail-end portion 102 of a first staple 54 is connected to a head-end portion of a second staple 54 by way of a frangible connection 106 . To be discussed in more detail, a stand-off element or boss element 152 (illustrated in FIG. 15 and FIG. 18 ) also acts as a support element to the belt-less staple chain that substantially holds the second staple 54 in place while the first staple 54 is deployed by a wedge element 194 .
FIG. 19A and FIG. 19B illustrate one example of structural elements that may be involved in a cartridge-based staple device using the belt-less staple chain. Also, similar or equivalent structural elements may be incorporated in a cartridge-less based staple device using the belt-less staple chain. Such similar or equivalent structural elements may be incorporated into an end-effector or staple deployment component of an endocutter, as illustrated in FIG. 21 through FIG. 23 .
FIG. 20A through FIG. 20E illustrate one example of staple deployment process. As illustrated in FIG. 20A and FIG. 20B , the process starts with advancement of one or more wedges 194 to engage one or more staples 54 in one or more belt-less staple chains 100 in a cartridge-based or cartridge-less based staple device or system. As illustrated in FIG. 20C through FIG. 20E , the wedge element 194 may be advanced progressively forward against a first staple 54 . The forward advancement of the wedge element 194 causes the head-end portion 102 of the staple 54 to pivot against the stand-off element 152 and the tail-end portion 104 to swing upwardly in a substantially arc-like motion. Referring to the close-up view of FIG. 18 , the head-end portion of the second staple 54 is being held substantially in place by a corresponding stand-off element or pivot element 152 , such as the upward motion of the tail-end portion of the first staple 54 is being resisted by the substantially stable or held-in-placed of the head-end portion of the second staple 54 . Accordingly, as the wedge element 152 continue to urge against the first staple 54 , the first staple 54 frangibly separates from the second staple 54 at the frangible connection 106 between the two staples 54 , as illustrated in FIG. 20C , and the tail-end portion 104 continues its upward arc-like motion or travel. As a staple device is deployed in a surgical procedure, the upward arc-like travel of the tail-end portion 104 of the staple 54 would encounter and pierce tissue. In an application setting, as the staple 54 is deployed by the wedge element 194 , the tail-end portion 104 would encounter the staple pocket elements 204 of an anvil 202 after piercing tissue. The staple pocket element 204 of the anvil 202 would deform the initially open configuration of the staple 54 into a closed staple, see FIG. 20D and FIG. 20E , thus stapling the tissue and leaving it hemostatic.
FIG. 21A and FIG. 21B illustrate an anvil element 202 and a staple holder element 212 of a staple device. Typically, a staple holder element 212 holds and deploys staples, such as one or more belt-less staple chains, and an anvil element 202 engages with one or more deployed staple 54 and deforms it from an initial configuration to a deployed configuration. An initial configuration may be an “open” configuration similar to the ones illustrated FIG. 10 through FIG. 20E . A deployed configuration may be a “closed” configuration similar to the one illustrated in FIG. 20E , where a deployed staple 54 has been deformed by a staple pocket element 204 . FIG. 22A and FIG. 22B illustrate the open-jaw configuration for the anvil 202 and stapler holder 212 . In the open-jaw configuration, a staple cartridge holder 224 is illustrated with its covers, shell, or skin, and separate cartridge holder 222 is illustrated without its covers, shell, or skin. FIG. 23 illustrates a staple device 230 where the belt-less staple chain 100 can be used. Similar or equivalent structural configuration and deployment arrangements are applicable to both a cartridge-base stapling device and a cartridge-less stapling device.
While the invention has been described in detail, it will be apparent to one skilled in the art that various changes and modifications can be made and equivalents employed without departing from the spirit and scope of the present invention. It is to be understood that the invention is not limited to the details of construction, the arrangements of components, and/or the methods set forth in the above description or illustrated in the drawings. Statements in this disclosure are merely exemplary; they are not and cannot be interpreted as limiting the spirit and scope of the claims. Further, the figures are merely exemplary and not limiting. Topical headings and subheadings are for the convenience of the reader only. They should not and cannot be construed to have any substantive significance, meaning or interpretation, and should not and cannot be deemed to indicate that all of the information relating to any particular topic is to be found under or limited to any particular heading or subheading. Therefore, the invention is not to be restricted or limited; instead, it is to be interpreted in accordance with the following claims and their equivalents. | A surgical stapling device is configured for use in open and/or laparoscopic surgical procedures. The device includes a staple holder with a first support element and a second support element for supporting a beltless continuous staple chain. Each staple of the staple chain is configured to be frangibly separated from the staple chain to pierce and secure a target tissue when each staple is deployed. The device also includes a plurality of standoff members wherein each of the plurality of standoff members is configured to support one of each staple of the staple chain when the one of each staple is being deployed. The surgical stapling device may be a cartridge-based or a cartridge-less based staple device. | 0 |
RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 61/774,521 filed Mar. 7, 2013, the disclosure of which is hereby incorporated in its entirety by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to novel aromatic derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals as modulators of sphingosine-1-phosphate receptors. The invention also relates to the use of these compounds and their pharmaceutical compositions to treat disorders associated with sphingosine-1-phosphate (S1P) receptor modulation.
BACKGROUND OF THE INVENTION
[0003] Sphingosine-1 phosphate is stored in relatively high concentrations in human platelets, which lack the enzymes responsible for its catabolism, and it is released into the blood stream upon activation of physiological stimuli, such as growth factors, cytokines, and receptor agonists and antigens. It may also have a critical role in platelet aggregation and thrombosis and could aggravate cardiovascular diseases. On the other hand the relatively high concentration of the metabolite in high-density lipoproteins (HDL) may have beneficial implications for atherogenesis. For example, there are recent suggestions that sphingosine-1-phosphate, together with other lysolipids such as sphingosylphosphorylcholine and lysosulfatide, are responsible for the beneficial clinical effects of HDL by stimulating the production of the potent antiatherogenic signaling molecule nitric oxide by the vascular endothelium. In addition, like lysophosphatidic acid, it is a marker for certain types of cancer, and there is evidence that its role in cell division or proliferation may have an influence on the development of cancers. These are currently topics that are attracting great interest amongst medical researchers, and the potential for therapeutic intervention in sphingosine-1-phosphate metabolism is under active investigation.
SUMMARY OF THE INVENTION
[0004] We have now discovered a group of novel compounds which are potent sphingosine-1-phosphate modulators. As such, the compounds described herein are useful in treating a wide variety of disorders associated with modulation of sphingosine-1-phosphate receptors. The term “modulator” as used herein, includes but is not limited to: receptor agonist, antagonist, inverse agonist, inverse antagonist, partial agonist, partial antagonist.
[0005] This invention describes compounds of Formula I, which have sphingosine-1-phosphate receptor biological activity. The compounds in accordance with the present invention are thus of use in medicine, for example in the treatment of humans with diseases and conditions that are alleviated by S1P modulation.
[0006] In one embodiment of the invention, there are provided compounds having the Formula I below and pharmaceutically accepted salts thereof, its enantiomers, diastereoisomers, hydrates, solvates, crystal forms and individual isomers, tautomers or a pharmaceutically acceptable salt thereof,
[0000]
[0000] wherein:
[0007] n is 0 or 1;
[0008] L is —NR—, —C(O)NR 1 —, —CR 23 R 24 — or —C≡C—;
[0009] R is H, or C 1-3 alkyl;
[0010] R 1 is H or C 1-3 alkyl;
[0011] R 2 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0012] R 3 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0013] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0014] R 5 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl; OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0015] R 6 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0016] R 7 is N or CR 7a ;
[0017] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0018] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0019] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0020] R 10 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 21 ;
[0021] R 11 is H, D, F or C 1-4 alkyl;
[0022] R 12 is H, D, F or C 1-4 alkyl;
[0023] R 13 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 14 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0024] R 14 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 13 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0025] R 15 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl or together with R 16 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0026] R 16 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl or together with R 15 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0027] R 17 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 18 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0028] R 18 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 17 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0029] R 19 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl,
[0030] R 20 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl;
[0031] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0032] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0033] R 23 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl;
[0034] R 24 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl; and
[0035] R 25 is H or C 1-4 alkyl;
[0000] with the provisos:
when n is 1 then L is —NR—, or —CR 23 R 24 —;
when n is 0 then L is —C(O)NR 1 — or —C≡C—.
In another aspect the invention provides a compound having Formula I wherein:
[0036] n is 1;
[0037] L is —CR 23 R 24 —;
[0038] R is H or C 1-3 alkyl;
[0039] R 1 is H or C 1-3 alkyl,
[0040] R 2 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0041] R 3 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0042] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0043] R 5 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl; OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0044] R 6 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0045] R 7 is N;
[0046] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0047] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0048] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), ON, SO 2 R 21 or C(O)R 22 ;
[0049] R 10 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 21 ;
[0050] R 11 is H, D, F or C 1-4 alkyl;
[0051] R 12 is H, D, F or C 1-4 alkyl;
[0052] R 13 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 14 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0053] R 14 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 13 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0054] R 15 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl or together with R 16 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0055] R 16 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl or together with R 15 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0056] R 17 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 18 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0057] R 18 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, or together with R 17 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0058] R 19 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl,
[0059] R 20 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl;
[0060] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0061] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0062] R 23 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl,
[0063] R 24 is H, D, F, C 1-4 alkyl, C 1-4 perfluoroalkyl, and
[0064] R 25 is H or C 1-4 alkyl;
[0000] with the provisos:
when n is 1 then L is —NR—, or —CR 23 R 24 —;
when n is 0 then L is —C(O)NR 1 — or —C≡C—.
In another aspect the invention provides a compound having Formula I wherein:
[0065] n is 1;
[0066] L is —CR 23 R 24 —;
[0067] R is H or C 1-3 alkyl;
[0068] R 1 is H or C 1-3 alkyl,
[0069] R 2 is H;
[0070] R 3 is H;
[0071] R 4 is H;
[0072] R 5 is H;
[0073] R 6 is H;
[0074] R 7 is CR 7a ;
[0075] R 7a is H;
[0076] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0077] R 9 is H;
[0078] R 10 is H;
[0079] R 11 is H;
[0080] R 12 is H;
[0081] R 13 is H;
[0082] R 14 is H;
[0083] R 15 is H;
[0084] R 16 is H;
[0085] R 17 is H;
[0086] R 18 is H;
[0087] R 19 is H;
[0088] R 20 is H;
[0089] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0090] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0091] R 23 is H;
[0092] R 24 is H; and
[0093] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0094] n is 1;
[0095] L is —NR—;
[0096] R is H, methyl, ethyl, n-propyl or isopropyl;
[0097] R 1 is H or C 1-3 alkyl;
[0098] R 2 is H;
[0099] R 3 is H;
[0100] R 4 is H;
[0101] R 5 is H;
[0102] R 6 is H;
[0103] R 7 is CR 7a ;
[0104] R 7a is H;
[0105] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0106] R 9 is H;
[0107] R 10 is H;
[0108] R 11 is H;
[0109] R 12 is H;
[0110] R 13 is H;
[0111] R 14 is H;
[0112] R 15 is H;
[0113] R 16 is H;
[0114] R 17 is H;
[0115] R 18 is H;
[0116] R 19 is H;
[0117] R 20 is H;
[0118] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0119] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0120] R 23 is H;
[0121] R 24 is H; and
[0122] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0123] n is 0;
L is —C(O)NR 1 —;
[0124] R is H or C 1-3 alkyl;
[0125] R 1 is H or C 1-3 alkyl,
[0126] R 2 is H;
[0127] R 3 is H;
[0128] R 4 is H;
[0129] R 5 is H;
[0130] R 6 is H;
[0131] R 7 is CR 7a ;
[0132] R 7a is H;
[0133] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0134] R 9 is H;
[0135] R 10 is H;
[0136] R 11 is H;
[0137] R 12 is H;
[0138] R 13 is H;
[0139] R 14 is H;
[0140] R 15 is H;
[0141] R 16 is H;
[0142] R 17 is H;
[0143] R 18 is H;
[0144] R 19 is H;
[0145] R 20 is H;
[0146] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0147] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0148] R 23 is H;
[0149] R 24 is H; and
[0150] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0151] n is 1;
[0152] L is —CR 23 R 24 —;
[0153] R is H or C 1-3 alkyl;
[0154] R 1 is H or C 1-3 alkyl,
[0155] R 2 is H;
[0156] R 3 is H;
[0157] R 4 is H;
[0158] R 5 is H;
[0159] R 6 is H;
[0160] R 7 is CR 7a ;
[0161] R 7a is H;
[0162] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0163] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0164] R 10 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0165] R 11 is H;
[0166] R 12 is H;
[0167] R 13 is H;
[0168] R 14 is H;
[0169] R 15 is H;
[0170] R 16 is H;
[0171] R 17 is H;
[0172] R 18 is H;
[0173] R 19 is H;
[0174] R 20 is H;
[0175] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0176] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0177] R 23 is H;
[0178] R 24 is H; and
[0179] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0180] n is 1;
[0181] L is —NR—;
[0182] R is H or C 1-3 alkyl;
[0183] R 1 is H or C 1-3 alkyl;
[0184] R 2 is H;
[0185] R 3 is H;
[0186] R 4 is H;
[0187] R 5 is H;
[0188] R 6 is H;
[0189] R 7 is CR 7a ;
[0190] R 7a is H;
[0191] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0192] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0193] R 10 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0194] R 11 is H;
[0195] R 12 is H;
[0196] R 13 is H;
[0197] R 14 is H;
[0198] R 15 is H;
[0199] R 16 is H;
[0200] R 17 is H;
[0201] R 18 is H;
[0202] R 19 is H;
[0203] R 20 is H;
[0204] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0205] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0206] R 23 is H;
[0207] R 24 is H; and
[0208] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0209] n is 0;
L is —C(O)NR 1 —;
[0210] R is H or C 1-3 alkyl;
[0211] R 1 is H or C 1-3 alkyl,
[0212] R 2 is H;
[0213] R 3 is H;
[0214] R 4 is H;
[0215] R 5 is H;
[0216] R 6 is H;
[0217] R 7 is CR 7a ;
[0218] R 7a is H;
[0219] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0220] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0221] R 10 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0222] R 11 is H;
[0223] R 12 is H;
[0224] R 13 is H;
[0225] R 14 is H;
[0226] R 15 is H;
[0227] R 16 is H;
[0228] R 17 is H;
[0229] R 18 is H;
[0230] R 19 is H;
[0231] R 20 is H;
[0232] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0233] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0234] R 23 is H;
[0235] R 24 is H; and
[0236] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0237] n is 1;
[0238] L is —CR 23 R 24 —;
[0239] R is H or C 1-3 alkyl;
[0240] R 1 is H or C 1-3 alkyl,
[0241] R 2 is H;
[0242] R 3 is H;
[0243] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0244] R 5 is H;
[0245] R 6 is H;
[0246] R 7 is CR 7a ;
[0247] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0248] R 8 is H;
[0249] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0250] R 10 is H;
[0251] R 11 is H;
[0252] R 12 is H;
[0253] R 13 is H;
[0254] R 14 is H;
[0255] R 15 is H;
[0256] R 16 is H;
[0257] R 17 is H;
[0258] R 18 is H;
[0259] R 19 is H;
[0260] R 20 is H;
[0261] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0262] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0263] R 23 is H or D;
[0264] R 24 is H or D; and
[0265] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0266] n is 1,
[0267] L is —CR 23 R 24 —;
[0268] R is H or C 1-3 alkyl;
[0269] R 1 is H or C 1-3 alkyl,
[0270] R 2 is H;
[0271] R 3 is H;
[0272] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0273] R 5 is H;
[0274] R 6 is H;
[0275] R 7 is CR 7a ;
[0276] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0277] R 8 is H;
[0278] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0279] R 10 is H;
[0280] R 11 is H;
[0281] R 12 is H;
[0282] R 13 is H;
[0283] R 14 is H;
[0284] R 15 is together with R 16 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0285] R 16 is together with R 15 can form a 3 to 6 membered ring cycloalkyl or heterocycle;
[0286] R 17 is H;
[0287] R 18 is H;
[0288] R 19 is H;
[0289] R 20 is H;
[0290] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0291] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0292] R 23 is H;
[0293] R 24 is H; and
[0294] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0295] n is 1;
[0296] L is —CR 23 R 24 —;
[0297] R is H or C 1-3 alkyl;
[0298] R 1 is H or C 1-3 alkyl,
[0299] R 2 is H;
[0300] R 3 is H;
[0301] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0302] R 5 is H;
[0303] R 6 is H;
[0304] R 7 is CR 7a ;
[0305] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0306] R 8 is H;
[0307] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0308] R 10 is H;
[0309] R 11 is H;
[0310] R 12 is H;
[0311] R 13 is H;
[0312] R 14 is H;
[0313] R 15 is together with R 16 can form a 3 to 6 membered ring heterocycle;
[0314] R 16 is together with R 15 can form a 3 to 6 membered ring heterocycle;
[0315] R 17 is H;
[0316] R 18 is H;
[0317] R 19 is H;
[0318] R 20 is H;
[0319] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0320] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0321] R 23 is H;
[0322] R 24 is H; and
[0323] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0324] n is 1;
[0325] L is —CR 23 R 24 —;
[0326] R is H or C 1-3 alkyl;
[0327] R 1 is H or C 1-3 alkyl,
[0328] R 2 is H;
[0329] R 3 is H;
[0330] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0331] R 5 is H;
[0332] R 6 is H;
[0333] R 7 is CR 7a ;
[0334] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0335] R 8 is H;
[0336] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0337] R 10 is H;
[0338] R 11 is H;
[0339] R 12 is H;
[0340] R 13 is H;
[0341] R 14 is H;
[0342] R 15 is together with R 16 can form a 3 to 6 membered ring cycloalkyl;
[0343] R 16 is together with R 15 can form a 3 to 6 membered ring cycloalkyl;
[0344] R 17 is H;
[0345] R 18 is H;
[0346] R 19 is H;
[0347] R 20 is H;
[0348] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0349] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0350] R 23 is H;
[0351] R 24 is H; and
[0352] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0353] n is 1,
[0354] L is —CR 23 R 24 —;
[0355] R is H or C 1-3 alkyl;
[0356] R 1 is H or C 1-3 alkyl,
[0357] R 2 is H;
[0358] R 3 is H;
[0359] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0360] R 5 is H;
[0361] R 6 is H;
[0362] R 7 is CR 7a ;
[0363] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0364] R 8 is H;
[0365] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0366] R 10 is H;
[0367] R 11 is H;
[0368] R 12 is H;
[0369] R 13 is H;
[0370] R 14 is H;
[0371] R 15 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl;
[0372] R 16 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl;
[0373] R 17 is H;
[0374] R 18 is H;
[0375] R 19 is H;
[0376] R 20 is H;
[0377] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0378] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0379] R 23 is H;
[0380] R 24 is H; and
[0381] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0382] n is 1,
[0383] L is —CR 23 R 24 —;
[0384] R is H or C 1-3 alkyl;
[0385] R 1 is H or C 1-3 alkyl,
[0386] R 2 is H;
[0387] R 3 is H;
[0388] R 4 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0389] R 5 is H;
[0390] R 6 is H;
[0391] R 7 is CR 7a ;
[0392] R 7a is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0393] R 8 is H;
[0394] R 9 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0395] R 10 is H;
[0396] R 11 is H;
[0397] R 12 is H;
[0398] R 13 is H;
[0399] R 14 is H;
[0400] R 15 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl;
[0401] R 16 is H, D, F, C 1-4 alkyl or C 1-4 perfluoroalkyl;
[0402] R 17 is H, D, F, C 1-4 alkyl;
[0403] R 18 is H, D, F, C 1-4 alkyl;
[0404] R 19 is H;
[0405] R 20 is H;
[0406] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0407] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0408] R 23 is H;
[0409] R 24 is H; and
[0410] R 25 is H or C 1-4 alkyl.
[0000] In another aspect the invention provides a compound having Formula I wherein:
[0411] n is 0;
[0412] L is —C≡C—;
[0413] R is H or C 1-3 alkyl;
[0414] R 1 is H or C 1-3 alkyl,
[0415] R 2 is H;
[0416] R 3 is H;
[0417] R 4 is H;
[0418] R 5 is H;
[0419] R 6 is H;
[0420] R 7 is CR 7a ;
[0421] R 7a is H;
[0422] R 8 is H, D, F, Cl, Br, C 1-4 alkyl, C 2-4 alkenyl, C 2-4 alkynyl, OH, NH 2 , NO 2 , C 1-4 perfluoroalkyl, O(C 1-4 )perfluoroalkyl, OCF 2 H, OCF 2 CF 2 H, O(C 1-4 alkyl), CN, SO 2 R 21 or C(O)R 22 ;
[0423] R 9 is H;
[0424] R 10 is H;
[0425] R 11 is H;
[0426] R 12 is H;
[0427] R 13 is H;
[0428] R 14 is H;
[0429] R 15 is H;
[0430] R 16 is H;
[0431] R 17 is H;
[0432] R 18 is H;
[0433] R 19 is H;
[0434] R 20 is H;
[0435] R 21 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0436] R 22 is H, C 1-4 alkyl, OH, C 1-4 perfluoroalkyl or N(R 25 ) 2 ;
[0437] R 23 is H or D,
[0438] R 24 is H or D; and
[0439] R 25 is H or C 1-4 alkyl.
[0440] The term “alkyl”, as used herein, refers to saturated, monovalent hydrocarbon moieties having linear or branched moieties or combinations thereof and containing 1 to 6 carbon atoms. One methylene (—CH 2 —) group, of the alkyl can be replaced by oxygen, sulfur, sulfoxide, nitrogen, carbonyl, carboxyl, sulfonyl, or by a divalent C 3-6 cycloalkyl. Alkyl groups can be substituted by halogen, amino, hydroxyl, cycloalkyl, amino, carboxylic acid, phosphonic acid groups, sulphonic acid groups, phosphoric acid.
[0441] The term “perfluoroalkyl” groups as used herein, refers to alkyl chains containing 1 to 4 carbon atoms wherein all the hydrogen atoms have been replaced by fluorine atoms on the carbon chain.
[0442] The term “alkylene”, as used herein, refers to saturated, divalent hydrocarbon moieties having linear or branched moieties or combinations thereof and containing 2 to 4 carbon atoms. One methylene (—CH 2 —) group of the alkylene can be replaced by oxygen, sulfur, sulfoxide, nitrogen, carbonyl, carboxyl, sulfonyl.
[0443] The term “cycloalkyl”, as used herein, refers to a monovalent or divalent group of 3 to 8 carbon atoms, or 3 to 6 carbon atoms, derived from a saturated cyclic hydrocarbon. Cycloalkyl groups can be monocyclic or polycyclic. Cycloalkyl can be substituted by 1 to 3 C 1-3 alkyl groups or 1 or 2 halogens.
[0444] The term “heterocycle” as used herein, refers to a 3 to 8 membered ring, or a 3 to 6 membered ring which can be aromatic or non-aromatic, saturated or unsaturated, containing at least one heteroatom selected form oxygen, nitrogen, sulfur, or combinations of at least two thereof, interrupting the carbocyclic ring structure. Heterocycles can be substituted by 1 to 3 C 1-3 alkyl groups or 1 or 2 halogens.
[0445] The term “cycloalkenyl”, as used herein, refers to a monovalent or divalent group of 5 to 8 carbon atoms, preferably 3 to 6 carbon atoms derived from a saturated cycloalkyl having one double bond. Cycloalkenyl groups can be monocyclic or polycyclic. Cycloalkenyl groups can be substituted by C 1-3 alkyl groups or halogens.
[0446] The term “halogen”, as used herein, refers to an atom of chlorine, bromine, fluorine, iodine.
[0447] The term “alkenyl”, as used herein, refers to a monovalent or divalent hydrocarbon radical having 2 to 6 carbon atoms, derived from a saturated alkyl, having at least one double bond. C 2-6 alkenyl can be in the E or Z configuration. Alkenyl groups can be substituted by C 1-3 alkyl.
[0448] The term “alkynyl”, as used herein, refers to a monovalent or divalent hydrocarbon radical having 2 to 6 carbon atoms, derived from a saturated alkyl, having at least one triple bond.
[0000] The term “hydroxyl” as used herein, represents a group of formula “OH”.
The term “carbonyl” as used herein, represents a group of formula “—C═O”.
The term “carboxyl” as used herein, represents a group of formula “—C(O)O—”.
The term “sulfonyl” as used herein, represents a group of formula “—SO 2 ”.
The term “sulfate” as used herein, represents a group of formula “—O—S(O) 2 —O—”.
The term “carboxylic acid” as used herein, represents a group of formula “—C(O)OH”.
The term “sulfoxide” as used herein, represents a group of formula “—S═O”.
The term “phosphonic acid” as used herein, represents a group of formula “—P(O)(OH) 2 ”.
The term “phosphoric acid” as used herein, represents a group of formula “—(O)P(O)(OH) 2 ”.
The term “sulphonic acid” as used herein, represents a group of formula “—S(O) 2 OH”.
The term “amino” as used herein, represents a group of formula “—NH 2 ”.
The formula “H”, as used herein, represents a hydrogen atom.
The formula “O”, as used herein, represents an oxygen atom.
The formula “N”, as used herein, represents a nitrogen atom.
The formula “S”, as used herein, represents a sulfur atom.
Compounds of the invention are:
(3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid; (3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid; (3-{[3-methyl-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid; (3-{[4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid; (3-{[3-bromo-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid; (3-{[3-fluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid; (3-{[3-methyl-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid; (3-{[4-(6-phenylhexyl)-3-(trifluoromethyl)benzyl]amino}propyl)phosphonic acid; (3-{[3-chloro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid; (3-{[4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid; (3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid; [3-({3-bromo-4-[(5-phenylpentanoyl)amino]benzyl}amino)propyl]phosphonic acid; (3-((2,5-difluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((2,5-difluoro-4-(6-(3-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((2,5-difluoro-4-(6-(2-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((2-bromo-5-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((5-fluoro-2-methyl-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((5-chloro-2-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((5-bromo-2-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((2-fluoro-5-methyl-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-(((5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-(((4-fluoro-5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-((2-chloro-5-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((2-bromo-5-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((5-fluoro-4-(6-(4-fluorophenyl)hexyl)-2-methylbenzyl)amino)propyl) phosphonic acid; (3-((5-chloro-2-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((5-bromo-2-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((2-fluoro-4-(6-(4-fluorophenyl)hexyl)-5-methylbenzyl)amino)propyl)phosphonic acid; (3-(((4-fluoro-5-(6-(4-fluorophenyl)hexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-(((5-(6-(4-fluorophenyl)hexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-methyl-6-phenylheptyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-phenylcyclopentyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(3-phenyloxetan-3-yl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((2,5-difluoro-4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((3-fluoro-4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((2,5-difluoro-4-(6-methyl-6-phenylheptyl)benzyl)amino)propyl)phosphonic acid; (3-((2,5-difluoro-4-(5-(1-phenylcyclopentyl)pentyl)benzyl)amino)propyl) phosphonic acid; (3-((2,5-difluoro-4-(5-(3-phenyloxetan-3-yl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5,5-dimethyl-6-phenylhexyl)-3-fluorobenzyl)amino)propyl)phosphonic acid; (3-{[3-fluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid-d 2 ; (3-{[3-chloro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid-d 2 ; (3-((3-chloro-2,5-difluoro-4-(6-(4-fluorophenyl)-6-methylheptyl)benzyl)amino) propyl)phosphonic acid; (3-((3-chloro-4-((5-(4-fluorophenyl)-5-methylhexyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((4,4-dimethyl-5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((4-(3-phenyloxetan-3-yl)butyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((4-(1-phenylcyclopentyl)butyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((4-(1-phenylcyclohexyl)butyl)amino)benzyl)amino)propyl)phosphonic acid; (3-(((4-chloro-5-((5-phenylpentyl)amino)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-(((4-chloro-5-((5-(4-fluorophenyl)pentyl)amino)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-((5-chloro-2-fluoro-4-((5-(4-fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((5-(4-fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((5-(3-fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(6-(4-fluorophenyl)-6-methylheptyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(5,5-dimethyl-6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(5-(3-phenyloxetan-3-yl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(5-(1-phenylcyclopentyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-(((4-chloro-5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-(((4-chloro-5-(6-(4-fluorophenyl)hexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid; (3-((5-chloro-2-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(6-(3-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-((5-(2-fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid. (3-((4-(6-phenylhexyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-(p-tolyl)hexyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-phenylcyclohexyl)pentyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-(6-(p-tolyl)hexyl)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-phenylpentyl)amino)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-(p-tolyl)pentyl)amino)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-((4-(1-phenylcyclohexyl)butyl)amino)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-((5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-((5-(p-tolyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-(perfluoroethyl)-4-((4-(1-phenylcyclohexyl)butyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-(4-fluorophenyl)hexyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-(4-fluorophenyl)hexyl)-3-(perfluoroethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3-(perfluoroethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-(4-fluorophenyl)pentyl)amino)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-(4-fluorophenyl)pentyl)amino)-3-(perfluoroethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid; (3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3-(perfluoroethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-(4-fluorophenyl)hexyl)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(6-(p-tolyl)hexyl)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-phenylcyclohexyl)pentyl)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-phenylpentyl)amino)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-(4-fluorophenyl)pentyl)amino)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((5-(p-tolyl)pentyl)amino)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((4-(1-phenylcyclohexyl)butyl)amino)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid; (3-((3-fluoro-4-(methyl(5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((4-(ethyl(5-phenylpentyl)amino)-3-fluorobenzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(methyl(5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(ethyl(5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((3-methyl-4-(methyl(5-phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid; (3-((4-(ethyl(5-phenylpentyl)amino)-3-methylbenzyl)amino)propyl)phosphonic acid; (3-((4-(ethyl(5-(4-fluorophenyl)pentyl)amino)-3-fluorobenzyl)amino)propyl)phosphonic acid; (3-((3-chloro-4-(ethyl(5-(4-fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid; and (3-((4-(ethyl(5-(4-fluorophenyl)pentyl)amino)-3-methylbenzyl)amino)propyl)phosphonic acid.
[0552] Some compounds of Formula I and some of their intermediates may have at least one stereogenic center in their structure. This stereogenic center may be present in an R or S configuration, said R and S notation is used in correspondence with the rules described in Pure Appli. Chem. (1976), 45, 11-13.
[0553] The term “pharmaceutically acceptable salts” refers to salts or complexes that retain the desired biological activity of the above identified compounds and exhibit minimal or no undesired toxicological effects. The “pharmaceutically acceptable salts” according to the invention include therapeutically active, non-toxic base or acid salt forms, which the compounds of Formula I are able to form.
[0554] The acid addition salt form of a compound of Formula I that occurs in its free form as a base can be obtained by treating the free base with an appropriate acid such as an inorganic acid, for example, an inorganic acid, such as hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, nitric acid and the like; or an organic acid such as for example, acetic, hydroxyacetic, propanoic, lactic, pyruvic, malonic, fumaric acid, maleic acid, oxalic acid, tartaric acid, succinic acid, malic acid, ascorbic acid, benzoic acid, tannic acid, pamoic acid, citric, methylsulfonic, ethanesulfonic, benzenesulfonic, formic and the like (Handbook of Pharmaceutical Salts, P. Heinrich Stahl & Camille G. Wermuth (Eds), Verlag Helvetica Chimica Acta-Zürich, 2002, 329-345).
[0555] Compounds of Formula I and their salts can be in the form of a solvate, which is included within the scope of the present invention. Such solvates include for example hydrates, alcoholates and the like.
[0556] With respect to the present invention reference to a compound or compounds, is intended to encompass that compound in each of its possible isomeric forms and mixtures thereof unless the particular isomeric form is referred to specifically.
[0557] Compounds according to the present invention may exist in different polymorphic forms. Although not explicitly indicated in the above formula, such forms are intended to be included within the scope of the present invention.
[0558] The compounds of the invention are indicated for use in treating or preventing conditions in which there is likely to be a component involving the sphingosine-1-phosphate receptors.
[0559] In another embodiment, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier.
[0560] In a further embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one compound of the invention.
[0561] These compounds are useful for the treatment of mammals, including humans, with a range of conditions and diseases that are alleviated by S1P modulation: not limited to the treatment of diabetic retinopathy, other retinal degenerative conditions, dry eye, angiogenesis and wounds.
[0562] Therapeutic utilities of S1P modulators are ocular diseases, such as but not limited to: wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis; or systemic vascular barrier related diseases such as but not limited to: various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury; or autoimmune diseases and immunosuppression such as but not limited to: rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, autoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermatitis, and organ transplantation; or allergies and other inflammatory diseases such as but not limited to: urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases; or cardiac protection such as but not limited to: ischemia reperfusion injury and atherosclerosis; or wound healing such as but not limited to: scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries; or bone formation such as but not limited to: treatment of osteoporosis and various bone fractures including hip and ankles; or anti-nociceptive activity such as but not limited to: visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains; or central nervous system neuronal activity in Alzheimer's disease, age-related neuronal injuries; or in organ transplant such as renal, corneal, cardiac or adipose tissue transplant; inflammatory skin diseases, scleroderma, dermatomyositis, atopic dermatitis, lupus erythematosus, epidermolysis bullosa, and bullous pemphigold. Topical use of S1P (sphingosine) compounds is of use in the treatment of various acne diseases, acne vulgaris, and rosacea.
[0563] In still another embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a therapeutically effective amount of at least one compound of the invention, or any combination thereof, or pharmaceutically acceptable salts, hydrates, solvates, crystal forms and individual isomers, enantiomers, and diastereomers thereof.
[0564] The present invention concerns the use of a compound of Formula I or a pharmaceutically acceptable salt thereof, for the manufacture of a medicament for the treatment of ocular disease, wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis; or systemic vascular barrier related diseases, various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury; or autoimmune diseases and immunosuppression, rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, autoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermatitis, and organ transplantation; or allergies and other inflammatory diseases, urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases; or cardiac protection, ischemia reperfusion injury and atherosclerosis; or wound healing, scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries; or bone formation, treatment of osteoporosis and various bone fractures including hip and ankles; or anti-nociceptive activity, visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains; or central nervous system neuronal activity in Alzheimer's disease, age-related neuronal injuries; or in organ transplant such as renal, corneal, cardiac or adipose tissue transplant; inflammatory skin diseases, scleroderma, dermatomyositis, atopic dermatitis, lupus erythematosus, epidermolysis bullosa, and bullous pemphigoid.
[0565] The actual amount of the compound to be administered in any given case will be determined by a physician taking into account the relevant circumstances, such as the severity of the condition, the age and weight of the patient, the patient's general physical condition, the cause of the condition, and the route of administration.
[0566] The patient will be administered the compound orally in any acceptable form, such as a tablet, liquid, capsule, powder and the like, or other routes may be desirable or necessary, particularly if the patient suffers from nausea. Such other routes may include, without exception, transdermal, parenteral, subcutaneous, intranasal, via an implant stent, intrathecal, intravitreal, topical to the eye, back to the eye, intramuscular, intravenous, and intrarectal modes of delivery. Additionally, the formulations may be designed to delay release of the active compound over a given period of time, or to carefully control the amount of drug released at a given time during the course of therapy.
[0567] In another embodiment of the invention, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier thereof. The phrase “pharmaceutically acceptable” means the carrier, diluent or excipient must be compatible with the other ingredients of the formulation and not deleterious to the recipient thereof.
[0568] Pharmaceutical compositions of the present invention can be used in the form of a solid, a solution, an emulsion, a dispersion, a patch, a micelle, a liposome, and the like, wherein the resulting composition contains one or more compounds of the present invention, as an active ingredient, in admixture with an organic or inorganic carrier or excipient suitable for enteral or parenteral applications. Invention compounds may be combined, for example, with the usual non-toxic, pharmaceutically acceptable carriers for tablets, pellets, capsules, suppositories, solutions, emulsions, suspensions, and any other form suitable for use. The carriers which can be used include glucose, lactose, gum acacia, gelatin, mannitol, starch paste, magnesium trisilicate, talc, corn starch, keratin, colloidal silica, potato starch, urea, medium chain length triglycerides, dextrans, and other carriers suitable for use in manufacturing preparations, in solid, semisolid, or liquid form. In addition auxiliary, stabilizing, thickening and coloring agents and perfumes may be used. Invention compounds are included in the pharmaceutical composition in an amount sufficient to produce the desired effect upon the process or disease condition.
[0569] Pharmaceutical compositions containing invention compounds may be in a form suitable for oral use, for example, as tablets, troches, lozenges, aqueous or oily suspensions, dispersible powders or granules, emulsions, hard or soft capsules, or syrups or elixirs. Compositions intended for oral use may be prepared according to any method known in the art for the manufacture of pharmaceutical compositions and such compositions may contain one or more agents selected from the group consisting of a sweetening agent such as sucrose, lactose, or saccharin, flavoring agents such as peppermint, oil of wintergreen or cherry, coloring agents and preserving agents in order to provide pharmaceutically elegant and palatable preparations. Tablets containing invention compounds in admixture with non-toxic pharmaceutically acceptable excipients may also be manufactured by known methods. The excipients used may be, for example, (1) inert diluents such as calcium carbonate, lactose, calcium phosphate or sodium phosphate; (2) granulating and disintegrating agents such as corn starch, potato starch or alginic acid; (3) binding agents such as gum tragacanth, corn starch, gelatin or acacia, and (4) lubricating agents such as magnesium stearate, stearic acid or talc. The tablets may be uncoated or they may be coated by known techniques to delay disintegration and absorption in the gastrointestinal tract and thereby provide a sustained action over a longer period. For example, a time delay material such as glyceryl monostearate or glyceryl distearate may be employed.
[0570] In some cases, formulations for oral use may be in the form of hard gelatin capsules wherein the invention compounds are mixed with an inert solid diluent, for example, calcium carbonate, calcium phosphate or kaolin. They may also be in the form of soft gelatin capsules wherein the invention compounds are mixed with water or an oil medium, for example, peanut oil, liquid paraffin or olive oil.
[0571] The pharmaceutical compositions may be in the form of a sterile injectable suspension. This suspension may be formulated according to known methods using suitable dispersing or wetting agents and suspending agents. The sterile injectable preparation may also be a sterile injectable solution or suspension in a non-toxic parenterally-acceptable diluent or solvent, for example, as a solution in 1,3-butanediol. Sterile, fixed oils are conventionally employed as a solvent or suspending medium. For this purpose any bland fixed oil may be employed including synthetic mono- or diglycerides, fatty acids (including oleic acid), naturally occurring vegetable oils like sesame oil, coconut oil, peanut oil, cottonseed oil, etc., or synthetic fatty vehicles like ethyl oleate or the like. Buffers, preservatives, antioxidants, and the like can be incorporated as required.
[0572] Invention compounds may also be administered in the form of suppositories for rectal administration of the drug. These compositions may be prepared by mixing the invention compounds with a suitable non-irritating excipient, such as cocoa butter, synthetic glyceride esters of polyethylene glycols, which are solid at ordinary temperatures, but liquefy and/or dissolve in the rectal cavity to release the drug.
[0573] The compounds of the invention may also be administered as pharmaceutical compositions in a form suitable for topical use, for example, as oily suspensions, as solutions or suspensions in aqueous liquids or nonaqueous liquids, or as oil-in-water or water-in-oil liquid emulsions.
[0574] Pharmaceutical compositions may be prepared by combining a therapeutically effective amount of at least one compound according to the present invention, or a pharmaceutically acceptable salt thereof, as an active ingredient with conventional ophthalmically acceptable pharmaceutical excipients and by preparation of unit dosage suitable for topical ocular use. The therapeutically efficient amount typically is between about 0.001 and about 5% (w/v), preferably about 0.001 to about 2.0% (w/v) in liquid formulations.
[0575] For ophthalmic application, preferably solutions are prepared using a physiological saline solution as a major vehicle. The pH of such ophthalmic solutions should preferably be maintained between 4.5 and 8.0 with an appropriate buffer system, a neutral pH being preferred but not essential. The formulations may also contain conventional pharmaceutically acceptable preservatives, stabilizers and surfactants.
[0576] Preferred preservatives that may be used in the pharmaceutical compositions of the present invention include, but are not limited to, benzalkonium chloride, chlorobutanol, thimerosal, phenylmercuric acetate and phenylmercuric nitrate.
[0577] A preferred surfactant is, for example, Tween 80. Likewise, various preferred vehicles may be used in the ophthalmic preparations of the present invention. These vehicles include, but are not limited to, polyvinyl alcohol, povidone, hydroxypropyl methyl cellulose, poloxamers, carboxymethyl cellulose, hydroxyethyl cellulose cyclodextrin and purified water.
[0578] Tonicity adjustors may be added as needed or convenient. They include, but are not limited to, salts, particularly sodium chloride, potassium chloride, mannitol and glycerin, or any other suitable ophthalmically acceptable tonicity adjustor.
[0579] Various buffers and means for adjusting pH may be used so long as the resulting preparation is ophthalmically acceptable. Accordingly, buffers include acetate buffers, citrate buffers, phosphate buffers and borate buffers. Acids or bases may be used to adjust the pH of these formulations as needed.
[0580] In a similar manner an ophthalmically acceptable antioxidant for use in the present invention includes, but is not limited to, sodium metabisulfite, sodium thiosulfate, acetylcysteine, butylated hydroxyanisole and butylated hydroxytoluene.
[0581] Other excipient components which may be included in the ophthalmic preparations are chelating agents. The preferred chelating agent is edentate disodium, although other chelating agents may also be used in place of or in conjunction with it.
[0000] The ingredients are usually used in the following amounts:
[0000]
Ingredient
Amount (% w/v)
active ingredient
about 0.001 to about 5
preservative
0-0.10
vehicle
0-40
tonicity adjustor
0-10
buffer
0.01-10
pH adjustor
q.s. pH 4.5-7.8
antioxidant
as needed
surfactant
as needed
purified water
to make 100%
[0582] The actual dose of the active compounds of the present invention depends on the specific compound, and on the condition to be treated; the selection of the appropriate dose is well within the knowledge of the skilled artisan.
[0583] The ophthalmic formulations of the present invention are conveniently packaged in forms suitable for metered application, such as in containers equipped with a dropper, to facilitate application to the eye. Containers suitable for drop wise application are usually made of suitable inert, non-toxic plastic material, and generally contain between about 0.5 and about 15 ml solution. One package may contain one or more unit doses. Especially preservative-free solutions are often formulated in non-resealable containers containing up to about ten, preferably up to about five units doses, where a typical unit dose is from one to about 8 drops, preferably one to about 3 drops. The volume of one drop usually is about 20-35 μl.
[0000] Since individual subjects may present a wide variation in severity of symptoms and each drug has its unique therapeutic characteristics, the precise mode of administration and dosage employed for each subject is left to the discretion of the practitioner.
[0584] The compounds and pharmaceutical compositions described herein are useful as medicaments in mammals, including humans, for treatment of diseases and/or alleviations of conditions which are responsive to treatment by agonists or functional antagonists of sphingosine-1-phosphate receptors. Thus, in further embodiments of the invention, there are provided methods for treating a disorder associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one invention compound. As used herein, the term “therapeutically effective amount” means the amount of the pharmaceutical composition that will elicit the biological or medical response of a subject in need thereof that is being sought by the researcher, veterinarian, medical doctor or other clinician. In some embodiments, the subject in need thereof is a mammal. In some embodiments, the mammal is human.
[0585] The present invention concerns also processes for preparing the compounds of Formula I. The compounds of Formula I according to the invention can be prepared analogously to conventional methods as understood by the person skilled in the art of synthetic organic chemistry. The synthetic schemes set forth below, illustrate how compounds according to the invention can be made. Those skilled in the art will be able to routinely modify and/or adapt the following scheme to synthesize any compounds of the invention covered by Formula I.
[0000] In Scheme 1, aryl esters react with alkyne compounds in the presence of copper iodide and a palladium catalyst to give the corresponding aryl alkyne intermediate. This intermediate is reduced with a hydride reagent such as LAH or DIBAL to give the corresponding alcohol intermediate. An oxidation with an appropriate reagent such as MnO 2 forms the aldehyde. This aldehyde intermediate reacts with 3-aminopropylphosphonic acid followed by an appropriate hydride such as sodium borohydride in a reductive amination reaction to give a derivative of Formula I.
[0000]
[0000] In Scheme 2, alkynes react with hydrogen in the presence of Pd or PtO 2 to give the corresponding intermediate. This intermediate is reduced with a hydride such as LAH or DIBAL and subsequently oxidized give the corresponding aldehyde intermediate. This aldehyde intermediate reacts with 3-aminopropylphosphonic acid followed by an appropriate hydride such as sodium borohydride in a reductive amination reaction to give a derivative of Formula I.
[0000]
[0000] In Scheme 3, anilines are bonded to alkyls containing a terminal aryl ring to form amides or amines with coupling reagents (such as HATU) or treatment of the aniline with base to give the corresponding amine intermediate. This intermediate is subsequently oxidized to give the corresponding aldehyde intermediate. This aldehyde intermediate reacts with 3-aminopropylphosphonic acid followed by an appropriate hydride such as sodium borohydride in a reductive amination reaction to give a derivative of Formula I.
[0000]
BRIEF DESCRIPTION OF THE DRAWINGS
[0586] FIG. 1 shows the results of Compound 10, (3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid, in the Lymphopenia Assay in Mice.
[0587] Lymphopenia was induced by S1P1 agonist, Compound 10, (0.5 mg/kg) in mice (5, 24, 48, 72 hours).
DETAILED DESCRIPTION OF THE INVENTION
[0588] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention claimed. As used herein, the use of the singular includes the plural unless specifically stated otherwise.
[0589] It will be readily apparent to those skilled in the art that some of the compounds of the invention may contain one or more asymmetric centers, such that the compounds may exist in enantiomeric as well as in diastereomeric forms. Unless it is specifically noted otherwise, the scope of the present invention includes all enantiomers, diastereomers and racemic mixtures. Some of the compounds of the invention may form salts with pharmaceutically acceptable acids or bases, and such pharmaceutically acceptable salts of the compounds described herein are also within the scope of the invention.
[0590] The present invention includes all pharmaceutically acceptable isotopically enriched compounds. Any compound of the invention may contain one or more isotopic atoms enriched or different than the natural ratio such as deuterium 2 H (or D) in place of protium 1 H (or H) or use of 13 C enriched material in place of 12 C and the like. Similar substitutions can be employed for N, O and S. The use of isotopes may assist in analytical as well as therapeutic aspects of the invention. For example, use of deuterium may increase the in vivo half-life by altering the metabolism (rate) of the compounds of the invention. These compounds can be prepared in accord with the preparations described by use of isotopically enriched reagents.
[0591] The following examples are for illustrative purposes only and are not intended, nor should they be construed as limiting the invention in any manner. Those skilled in the art will appreciate that variations and modifications of the following examples can be made without exceeding the spirit or scope of the invention.
[0592] As will be evident to those skilled in the art, individual isomeric forms can be obtained by separation of mixtures thereof in conventional manner. For example, in the case of diasteroisomeric isomers, chromatographic separation may be employed.
[0593] Compound names were generated with ACDLabs version 8.00 or 12.00 and in some cases Chem Bio Draw Ultra version 12.0; and Intermediates and reagent names used in the examples were generated with software such as ACD version 12.05, Chem Bio Draw Ultra version 12.0.
[0594] In general, characterization of the compounds is performed according to the following methods: NMR spectra are recorded on 300 and/or 600 MHz Varian and acquired at room temperature. The spectra of all products were consistent with their structures. Chemical shifts are given in ppm referenced either to internal TMS or to the solvent signal. All the reagents, solvents, catalysts for which the synthesis is not described are purchased from chemical vendors such as Sigma Aldrich, Fluka, Bio-Blocks, Combi-blocks, TCI, VWR, Lancaster, Oakwood, Trans World Chemical, Alfa, AscentScientific LLC., Fisher, Maybridge, Frontier, Matrix, Ukrorgsynth, Toronto, Ryan Scientific, SiliCycle, Anaspec, Syn Chem, Chem-Impex, MIC-scientific, Ltd; however some known intermediates, were prepared according to published procedures.
[0595] Usually the compounds of the invention were purified by column chromatography (Auto-column) on a Teledyne-ISCO CombiFlash with a “silica” column generally called a silia-amine column, unless noted otherwise. Compounds of the invention were purified according to either of the following methods below:
[0596] Added amino modified silica gel to organic solution (MeOH/CHCl 3 ) and concentrated. Auto column on a silica gel-amine column with 70% MeOH, 0.5% acetic acid in dichloromethane gave product after removal of solvents, and drying under vacuum.
[0597] Product tituration with methanol, filtered, and washed with methanol to give product after removal of solvents, and drying under vacuum.
[0000] The following abbreviations are used in the examples:
s, m, h, d second, minute, hour, day ser. series brs broad singlet CH 3 CN acetonitrile psi pound per square inch CH 2 Cl 2 dichloromethane DMF N,N-dimethylformamide EtOH ethanol IPA isopropyl alcohol Na 2 CO 3 sodium carbonate PdCl 2 (PPh 3 ) 2 bis(triphenylphosphine)palladium(II) chloride K 2 CO 3 potassium carbonate CuI copper iodide MnO 2 manganese oxide MgCl 2 magnesium chloride NaCl sodium chloride CHCl 3 chloroform TBAH tetrabutylammonium hydroxide NBS N-bromosuccinimide MeOH methanol CD 3 OD deuterated methanol CF 3 C(O)OD deuterated trifluoroacetic acid CDCl 3 deuterated chloroform DMSO-d 6 deuterated dimethyl sulfoxide HCl hydrochloric acid Na 2 SO 4 sodium sulfate RT or rt room temperature MgSO 4 magnesium sulfate EtOAc ethyl acetate Auto-column automated flash liquid chromatography TFA trifluoroacetic acid THF tetrahydrofuran M molar AcOH acetic acid K 2 CO 3 potassium carbonate D 2 O deuterated water Pd(C) palladium on carbon PtO 2 platinum oxide DIBAL diisobutylaluminium hydride LAH or LiAlH 4 lithium aluminum hydride DIPEA diisopropyl ethyl amine HATU 1-[bis(dimethylamino)methylene]-1H-1,2,3-triazolo[4,5-b]pyridinium 3-oxid hexafluorophosphate TOF MS time of flight mass spectrometry CAS number reported in brackets, [CAS #]
[0642] The following synthetic schemes illustrate how compounds according to the invention can be made. Those skilled in the art will be routinely able to modify and/or adapt the following schemes to synthesize any compound of the invention covered by Formula I.
Example 1
Intermediate 1
Ethyl 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzoate
[0643]
[0644] A mixture of 5-hexyn-1-yl-benzene [100848-88-2], (650 mg, 4.11 mmol), CuI (34 mg), PdCl 2 (Ph 3 ) 2 (120 mg) in triethylamine (5.4 mL), and THF (9 mL) was purged with N 2 for about 5 m. Ethyl 3-fluoro-4-iodobenzoate (1000 mg, 3.40 mmol) was added to the mixture, and the resulting solution was heated at 50° C. for 3 h. The mixture was subjected to an aqueous work-up, and the residue was purified by auto-column (1% ethyl acetate:hexanes) to give ethyl 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzoate Intermediate 1, 850 mg. (77%).
[0645] Intermediates 1-6 were prepared according to the procedure described in Example 1. The starting materials and the results are tabulated below in Table 1.
[0000]
TABLE 1
Interm.
IUPAC name
data
No.
Structure
Starting materials
MS or 1 H NMR δ (ppm)
1
ethyl 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzoate
ethyl 3-fluoro-4- iodobenzoate [1027513-43-4]
1 H NMR (600 MHz, CDCl 3 ) δ: 7.74-7.69 (m, 2H), 7.42-7.40 (m, 1H), 7.29-7.26 (m, 2H), 7.20- 7.18 (m, 3H), 4.36 (q, J = 1.2 Hz, 2H), 2.67 (t, J = 7.2 Hz, 2H), 2.49 (t, J = 7.2 Hz, 2H), 1.82-1.78 (m, 2H), 1.69-1.65 (m, 2H), 1.39-1.37 (m, 3H).
2
methyl 3-methyl-4-(6-phenylhex-1-yn-1-yl)benzoate
methyl 4-iodo-3- methylbenzoate [5471-81-8]
3
methyl 4-(6-phenylhex-1-yn-1-yl)-3-(trifluoromethyl)benzoate
methyl 4-bromo-3- (trifluoromethyl) benzoate [107317-58-8]
4
ethyl 3-chloro-4-(6-phenylhex-1-yn-1-yl)benzoate
ethyl 3-chloro-4- iodobenzoate [874831-02-4]
5
methyl 3-bromo-4-(6-phenylhex-1-yn-1-yl)benzoate
methyl 3-bromo-4- iodobenzoate [249647-24-3]
6
2,5-difluoro-4-(6-phenylhex-1-yn-1-yl)benzaldehyde
4-bromo-2,5- difluorobenzaldehyde [357405-75-5], DIPEA as amine base, 80° C.~18 h.
Example 2
Intermediate 7
Ethyl 3-fluoro-4-(6-phenylhexyl)benzoate
[0646]
[0647] A mixture of ethyl 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzoate Intermediate 1 (425 mg, 1.31 mmol) Pd/C (10%, 43 mg) H 2 (50 psi) in MeOH (15 mL) was reacted at rt for ˜18 h. (77%). The mixture was filtered and washed through a pad of celite with MeOH. The filtrate was concentrated onto silica gel and auto-column (2% ethyl acetate in hexanes) gave ethyl 3-fluoro-4-(6-phenylhexyl)benzoate Intermediate 7, 320 mg (74%).
[0648] Intermediates 7-11 were prepared according to the procedure described in Example 2. The starting materials and the results are tabulated below in Table 2.
[0000]
TABLE 2
Interm.
IUPAC name
Starting
data
No.
Structure
materials
MS or 1 H NMR δ (ppm)
7
ethyl 3-fluoro-4-(6-phenylhexyl)benzoate
Intermediate 1
1 H NMR (600 MHz, CDCl 3 ) δ: 7.80-7.65 (m, 2H), 7.35- 7.18 (ser. of m, 6H), 4.40 (m, 2H), 2.70-2.55 (ser. of m, 4H), 1.70-1.60 (m, 4H), 1.45-1.35 (m, 7H).
8
methyl 3-methyl-4-(6-phenylhexyl)benzoate
Intermediate 2
9
methyl 4-(6-phenylhexyl)-3-(trifluoromethyl)benzoate
Intermediate 3
10
ethyl 3-chloro-4-(6-phenylhexyl)benzoate
Intermediate 4 PtO 2 at 40 psi H 2 THF, ~7 h
11
2,5-difluoro-4-(6-phenylhexyl)benzaldehyde
6 balloon H 2
Example 3
Intermediate 12
(3-Fluoro-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol
[0649]
[0650] A mixture of ethyl 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzoate Intermediate 1 (425 mg, 1.31 mmol) in THF (10 mL) was treated with LiAlH 4 (0.85 mL, 2M in THF) at 0° C., and the reaction was continued at rt for 18 h. Solvents were removed under vacuum and the residue was quenched with crushed ice. 2M HCl (mL) was added and the aqueous layer was extracted (2×) with hexanes:ethyl acetate (1:1, 200 mL total). The combined organic layers were dried over MgSO 4 , filtered and concentrated under reduced pressure to give the product as an oil, (3-fluoro-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol Intermediate 12, ˜400 mg (˜99%).
[0651] Intermediates 12-18 were prepared according to the procedure described in Example 3. The starting materials and the results are tabulated below in Table 3.
[0000]
TABLE 3
Interm.
IUPAC name
Starting
data
No.
Structure
materials
MS or 1 H NMR δ (ppm)
12
(3-fluoro-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol
Intermediate 1
1 H NMR (300 MHz, CDCl 3 ) δ: 7.36-7.03 (ser. of m, 8H), 4.68 (s, 2H), 2.67 (t, J = 7.5 Hz, 2H), 2.48 (t, 6.9 Hz, 2H), 1.82-1.66 (ser. of m, 4H).
13
(3-methyl-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol
Intermediate 2
14
(3-bromo-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol
Intermediate 5 use of DIBAL (1.5M in toluene) at −40 C
15
(3-fluoro-4-(6-phenylhexyl)phenyl)methanol
Intermediate 7
16
(3-methyl-4-(6-phenylhexyl)phenyl)methanol
Intermediate 8
17
(4-(6-phenylhexyl)-3-(trifluoromethyl)phenyl)methanol
Intermediate 9
18
(3-chloro-4-(6-phenylhexyl)phenyl)methanol
Intermediate 10
Example 4
Intermediate 19
(4-(6-phenylhex-1-yn-1-yl)phenyl)methanol
[0652]
[0653] A solution of (3-bromo-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol Intermediate 14 (1.27 g, 3.7 mmol) in THF (15 mL) at −78° C. was treated with nBuLi (7.4 mL, 2.5 M in hexanes) for ˜5 m. The mixture was quenched with MeOH (3 mL) and warmed to rt. The solvent was removed under vacuum, and the residue was treated with sat. NH 4 Cl solution before extraction with ethyl acetate (2×). The combined extracts were dried over MgSO 4 , filtered and concentrated under reduced pressure to give (4-(6-phenylhex-1-yn-1-yl)phenyl)methanol Intermediate 19 as an oil.
Example 5
Intermediate 20
N-(2-bromo-4-(hydroxymethyl)phenyl)-5-phenylpentanamide
[0654]
[0655] A mixture of 2-bromo-4-(hydroxymethyl)aniline [146019-46-7] (43 mg, 0.213 mmol), 5-phenylpentanoic acid [2270-20-4] (430 mg, 2.41 mmol), DIPEA (1.3 mL, 7.46 mmol), and HATU (97%, 1.22 g, 3.11 mmol) in DMF (20 mL) was reacted at rt for 18 h. The mixture was subjected to an aqueous work-up, and purified by auto-column (8:2 gradient to 6:4 hexane:ethyl acetate) to give N-(2-bromo-4-(hydroxymethyl)phenyl)-5-phenylpentanamide Intermediate 20, 90 mg. TOF MS m/z (m+Fir 362.08.
Example 6
Intermediate 21
(3-bromo-4-((5-phenylpentyl)amino)phenyl)methanol
[0656]
[0657] A mixture of 2-bromo-4-(hydroxymethyl)aniline [146019-46-7] (0.37 g, 1.83 mmol), K 2 CO 3 (0.51 g, 3.69 mmol) and (5-bromopentyl)benzene [14469-83-1] (0.33 g, 1.45 mmol) in HMPA (5 mL) was heated to 120° C. for ˜18 h. After an aqueous work-up with hexanes/ethyl acetate, and auto-column (on silica gel) (8.5 hexanes/1.5 ethyl acetate) the crude material, (3-bromo-4-((5-phenylpentyl)amino)phenyl)methanol Intermediate 21 was obtained 0.25 g (approx 50%). TOF MS m/z (M+Na) + 370.20; (M+H) − 348.10
Example 7
Intermediate 22
3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzaldehyde
[0658]
[0659] A mixture of (3-fluoro-4-(6-phenylhex-1-yn-1-yl)phenyl)methanol Intermediate 12 (1.31 mmol), MnO 2 (85%, 840 mg, 8.21 mmol) in dioxane (10 mL) was heated to 100° C. for ˜18 h. The mixture was cooled, and filtered through a bed of celite with ethyl acetate. The filtrate was concentrated under vacuum to give an oil residue, 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzaldehyde Intermediate 22, 290 mg, (˜80% two steps).
[0660] Intermediates 22-31 were prepared according to the procedure described in Example 7. The starting materials and the results are tabulated below in Table 4.
[0000]
TABLE 4
Starting
Interm.
IUPAC name
materials
data
No.
Structure
(Intermediate)
MS or 1 H NMR δ (ppm)
22
3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzaldehyde
Intermediate 12
1 H NMR (300 MHz, CDCl 3 ) δ: 9.95 (s, 1H), 7.60-7.19 (ser of m, 8H), 2.68 (t, J = 7.8 Hz, 2H), 2.52 (t, J = 6.9 Hz, 2H), 1.85-1.65 (ser of m, 4H).
23
3-methyl-4-(6-phenylhex-1-yn-1-yl)benzaldehyde
Intermediate 13
24
4-(6-phenylhex-1-yn-1-yl)benzaldehyde
Intermediate 19
25
3-bromo-4-(6-phenylhex-1-yn-1-yl)benzaldehyde
Intermediate 14
26
3-fluoro-4-(6-phenylhexyl)benzaldehyde
Intermediate 15
27
3-methyl-4-(6-phenylhexyl)benzaldehyde
Intermediate 16
28
4-(6-phenylhexyl)-3-(trifluoromethyl)benzaldehyde
Intermediate 17
29
3-chloro-4-(6-phenylhexyl)benzaldehyde
Intermediate 18
30
N-(2-bromo-4-formylphenyl)-5-phenylpentanamide
Intermediate 20
31
3-bromo-4-((5-phenylpentyl)amino)benzaldehyde
Intermediate 21
TOF MS m/z (M + H) − 346.2314
Example 8
Compound 1
(3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
[0661]
[0662] A mixture of 3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzaldehyde Intermediate 22 (290 mg, 1.03 mmol), (3-aminopropyl)phosphonic acid [13138-33-5] (170 mg, 1.22 mmol), and tetrabutyl ammonium hydroxide (3.1 mL of 1.0 M in methanol) in THF (4 mL) and methanol (6 mL) were heated at 60° C. for 30 m followed by 30 m at rt. Sodium borohydride (60 mg, 1.59 mmol) was added, and the mixture was reacted for ˜18 h at rt. The solvent was removed under vacuum. Water was added followed by 2 M HCl to pH ˜3. The mixture was extracted (2×) with 3:1 chloroform:isopropanol (200 mL total). The organic layers were concentrated onto silia-amine silica gel (ISCO). The material was purified by auto-column (silia-amine column, 70% MeOH, 0.5% AcOH in CH 2 Cl 2 ) to give (3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid Compound 1, 324 mg (73%).
[0663] Compounds 1 through 12 were prepared according to the procedure described in Example 8 from the corresponding intermediate. The starting materials and the results are tabulated below in Table 5.
[0000]
TABLE 5
Comp.
No.
IUPAC name
Interm. No.
1 H NMR δ (ppm)
1
(3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
22
(600 MHz, CF 3 C(O)OD) δ: 7.45 (t, J = 7.2 Hz, 1H), 7.23 (t, J = 7.8 Hz, 2H), 7.19 (d, J = 7.8 Hz, 2H), 7.13-7.11 (m, 3H), 4.33 (s, 2H), 3.41 (brs, 2H), 2.66 (t, J = 7.8 Hz, 2H), 2.47 (t, J = 7.2 Hz, 2H), 2.30-2.25 (m, 2H), 2.20-2.10 (m, 2H), 1.85- 1.80 (m, 2H), 1.69-1.66 (m, 2H).
2
(3-{[3-methyl-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
23
(600 MHz, CF 3 C(O)OD) δ: 7.37 (d, J = 7.8 Hz, 1H), 7.21-7.19 (m, 2H), 7.16-7.15 (m, 3H), 7.10- 7.06 (m, 2H), 4.24 (s, 2H), 3.37 (s, 2H), 2.64 (t, J = 7.8 Hz, 2H), 2.46 (t, J= 6.6 Hz, 2H), 2.37 (s, 3H), 2.23-2.19 (m, 2H), 2.12-2.09 (m, 2H), 1.82- 1.79 (m, 2H), 1.66-1.64 (m, 2H).
3
(3-{[4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
24
(600 MHz, CF 3 C(O)OD) δ: 7.44 (dd, J =1.8, 8.4 Hz, 2H), 7.29 (dd, J = 2.4, 8.4 Hz, 2H), 7.24- 7.21 (m, 2H), 7.19-7.18 (m, 2H), 7.13-7.11 (m, 1H), 4.32 (s, 2H), 3.40 (brs, 2H), 2.67-2.64 (m, 2H), 2.44-2.42 (m, 2H), 2.28-2.22 (m, 2H), 2.16- 2.22 (m, 2H), 1.82-1.80 (m, 2H), 1.67-1.64 (m, 2H).
4
(3-{[3-bromo-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
25
(600 MHz, CF 3 C(O)OD) δ: 7.60 (s, 1H), 7.45 (d, J = 8.4 Hz, 1H), 7.26-7.21 (m, 3H), 7.18 (d, J = 7.2 Hz, 2H), 7.11 (t, J = 6.6 Hz, 1H), 4.29 (brs, 2H), 3.40 (brs, 2H), 2.66 (t, J = 7.8 Hz, 2H), 2.48 (t, J = 6.6 Hz, 2H), 2.28-2.21 (m, 2H), 2.15-2.11 (m, 2H), 1.89-1.84 (m, 2H), 1.70-1.66 (m, 2H).
5
(3-{[3-fluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
26
(600 MHz, CF 3 C(O)OD) δ: 7.30-7.26 (m, 1H), 7.24-7.19 (m, 2H), 7.17- 7.14 (m, 2H), 7.12-7.08 (m. 2H), 7.06-7.02 (m, 1H), 4.30 (t, J = 5.4 Hz, 2H), 3.45-3.37 (m, 2H), 2.67 (t, J = 7.2 Hz, 2H), 2.59 (t, J = 7.8 Hz, 2H), 2.29-2.21 (m, 2H), 2.17-
2.12 (m, 2H), 1.65-1.56
(m, 4H), 1.44-1.35 (m,
4H).
6
(3-{[3-methyl-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
27
(600 MHz, CF 3 C(O)OD) δ: 7.21-7.18 (m, 3H), 7.14 (d, J = 7.2 Hz, 2H), 7.10-7.07 (m, 3H), 4.23 (t, J = 5.4 Hz, 2H), 3.40- 3.37 (m, 2H), 2.61 (t, J = 7.8 Hz, 2H), 2.57 (t, J = 7.8 Hz, 2H), 2.28 (s, 3H), 2.25-2.20 (m, 2H), 2.14-2.09 (m, 2H), 1.64-
1.54 (m, 4H), 1.45-1.35
(m, 4H).
7
(3-{[4-(6-phenylhexyl)-3-(trifluoromethyl)benzyl]amino}propyl)phosphonic acid
28
(600 MHz, CF 3 C(O)OD) δ: 7.65 (s, 1H), 7.51 (d, J = 7.2 Hz, 1H), 7.46 (d, J = 7.2 Hz, 1H), 7.23-7.21 (m, 2H), 7.16 (d, J = 7.2 Hz, 2H), 7.10 (t, J = 6.6 Hz, 1H), 4.37 (s, 2H), 3.44 (s, 2H), 2.83 (t, J = 6.6 Hz, 2H), 2.60 (t, J = 6.6 Hz, 2H), 2.29-2.22
(m, 2H), 2.17-2.13 (m,
2H), 1.70-1.60 (m, 4H),
1.47-1.41 (m, 4H).
8
(3-{[3-chloro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
29
(600 MHz, DMSO-d 6 & CF 3 C(O)OD) δ: 7.54 (s, 1H), 7.36-7.29 (m, 2H), 7.23-7.18 (m, 2H), 7.13- 7.07 (m, 3H), 4.08 (s, 2H), 3.01 (t, J = 6.6 Hz, 2H), 2.65 (t, J = 7.5 Hz, 2H), 2.54-2.49 (m, 2H), 1.91-1.80 (m, 2H), 1.76- 1.65 (m, 2H), 1.60-1.46
(m, 4H), 1.37-1.25 (m,
4H).
9
(3-{[4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
Compound 3 Note 1
(600 MHz, CF 3 C(O)OD) δ: 7.32-7.10 (ser of m, 9H), 4.30 (t, J =6.0 Hz, 2H), 3.41 (brs, 2H), 2.65 (t, J = 6.6 Hz, 2H), 2.59 (t, J = 7.2 Hz, 2H), 2.28- 2.23 (m, 2H), 2.17-2.12 (m, 2H), 1.68-1.60 (m, 4H), 1.45-1.37 (m, 4H).
10
(3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
11 See Note 2
(600 MHz, DMSO-d 6 & CF 3 C(O)OD) δ: 7.35 (dd, J = 10.2, 6.6 Hz, 1H), 7.23-7.17 (m, 3H), 7.14- 7.10 (m, 3H), 4.13 (s, 2H), 3.04 (t, J = 7.8 Hz, 2H), 2.57 (t, J = 7.8 Hz, 2H), 2.52 (t, J = 7.8 Hz, 2H), 1.88-1.83 (m, 2H), 1.72-1.67 (m, 2H), 1.55- 1.51 (m, 4H), 1.30-1.27 (m, 4H).
11
[3-({3-bromo-4-[(5-phenylpentanoyl)amino]benzyl}amino)propyl]phosphonic acid
30 Note 3
(600 MHz, CD 3 OD and CDCl 3 ) δ: 7.91 (d, J = 8.4 Hz, 1H), 7.70 (s, 1H), 7.39 (d, J = 8.4 Hz, 1H), 7.23 (t, J = 7.2 Hz, 2H), 7.16-7.12 (m, 3H), 4.00 (s, 2H), 2.99 (t, J = 5.4 Hz, 2H), 2.65 (t, J = 7.2 Hz, 2H), 2.46 (t, J = 5.4 Hz, 2H), 1.95-1.91
(m, 2H), 1.76-1.67 (m,
6H).
12
[3-({3-bromo-4-[(5-phenylpentyl)amino]benzyl}amino)propyl]phosphonic acid
31 Note 3
(600 MHz, CF 3 C(O)OD) δ: 7.98 (s, 1H), 7.74 (s, 2H), 7.27 (t, J = 7.2 Hz, 2H), 7.19-7.16 (m, 3H), 4.49 (s, 2H), 3.64 (t, J = 7.2 Hz, 2H), 3.55 (t, J = 6.0 Hz, 2H), 2.68 (t, J = 7.8 Hz, 2H), 2.36-2.31 (m, 2H), 2.22-2.18 (m, 2H), 1.98-1.93 (m, 2H),
1.78-1.73 (m, 2H), 1.57-
1.52 (m, 2H).
Note 1:
Compound 9 was prepared by a reduction of Compound 3 with H 2 and Pd/C in a method as above-refer to Example 2 above.
Note 2:
A reduction of residual styrene (3-((2,5-difluoro-4-(6-phenylhex-1-en-1-yl)benzyl)amino)propyl)phosphonic acid), <10% (from Example 2) was completed with Pd/C, TBAH, 50 psi H2, ~18 h, and followed by an aqueous work-up and auto-column purification.
Note 3:
Further purification on C-18 column (10% to 100% CH 3 CN in water) gave pure material.
[0664] Compounds 13 through 65 may be prepared according to analogous procedures described above. The compounds are tabulated below in Table 8.
[0000]
TABLE 8
Comp.
Compound name
No.
Structure
13
(3-((2,5-difluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
14
(3-((3-fluoro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
15
(3-((2,5-difluoro-4-(6-(3-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
16
(3-((2,5-difluoro-4-(6-(2-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
17
(3-((2-bromo-5-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
18
(3-((5-fluoro-2-methyl-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
19
(3-((5-chloro-2-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
20
(3-((5-bromo-2-fluoro-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
21
(3-((2-fluoro-5-methyl-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
22
(3-(((5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid
23
(3-(((4-fluoro-5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid
24
(3-((2-chloro-5-fluoro-4-(6-(4- fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
25
(3-((2-bromo-5-fluoro-4-(6-(4- fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
26
(3-((5-fluoro-4-(6-(4-fluorophenyl)hexyl)-2- methylbenzyl)amino)propyl)phosphonic acid
27
(3-((5-chloro-2-fluoro-4-(6-(4- fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
28
(3-((5-bromo-2-fluoro-4-(6-(4- fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
29
(3-((2-fluoro-4-(6-(4-fluorophenyl)hexyl)-5- methylbenzyl)amino)propyl)phosphonic acid
30
(3-(((4-fluoro-5-(6-(4-fluorophenyl)hexyl)pyridin-2- yl)methyl)amino)propyl)phosphonic acid
31
(3-(((5-(6-(4-fluorophenyl)hexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid
32
(3-((4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid
33
(3-((4-(6-methyl-6-phenylheptyl)benzyl)amino)propyl)phosphonic acid
34
(3-((4-(5-(1-phenylcyclopentyl)pentyl)benzyl)amino)propyl)phosphonic acid
35
(3-((4-(5-(3-phenyloxetan-3-yl)pentyl)benzyl)amino)propyl)phosphonic acid
36
(3-((2,5-difluoro-4-(5-(1- phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid
37
(3-((3-fluoro-4-(5-(1-phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid
38
(3-((2,5-difluoro-4-(6-methyl-6-phenylheptyl)benzyl)amino)propyl)phosphonic acid
39
(3-((2,5-difluoro-4-(5-(1- phenylcyclopentyl)pentyl)benzyl)amino)propyl)phosphonic acid
40
(3-((2,5-difluoro-4-(5-(3-phenyloxetan-3- yl)pentyl)benzyl)amino)propyl)phosphonic acid
41
(3-((4-(5,5-dimethyl-6-phenylhexyl)-3-fluorobenzyl)amino)propyl)phosphonic acid
42
(3-{[3-fluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid-d 2
43
(3-{[3-chloro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid-d 2
44
(3-((3-chloro-2,5-difluoro-4-(6-(4-fluorophenyl)-6- methylheptyl)benzyl)amino)propyl)phosphonic acid
45
(3-((3-chloro-4-((5-(4-fluorophenyl)-5- methylhexyl)amino)benzyl)amino)propyl)phosphonic acid
46
(3-((3-chloro-4-((4,4-dimethyl-5- phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid
47
(3-((3-chloro-4-((4-(3-phenyloxetan-3- yl)butyl)amino)benzyl)amino)propyl)phosphonic acid
48
(3-((3-chloro-4-((4-(1- phenylcyclopentyl)butyl)amino)benzyl)amino)propyl)phosphonic acid
49
(3-((3-chloro-4-((4-(1- phenylcyclohexyl)butyl)amino)benzyl)amino)propyl)phosphonic acid
50
(3-(((4-chloro-5-((5-phenylpentyl)amino)pyridin-2- yl)methyl)amino)propyl)phosphonic acid
51
(3-(((4-chloro-5-((5-(4-fluorophenyl)pentyl)amino)pyridin-2- yl)methyl)amino)propyl)phosphonic acid
52
(3-((5-chloro-2-fluoro-4-((5-(4- fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid
53
(3-((3-chloro-4-((5-(4- fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid
54
(3-((3-chloro-4-((5-(3- fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid
55
(3-((3-chloro-4-(6-(4-fluorophenyl)-6- methylheptyl)benzyl)amino)propyl)phosphonic acid
56
(3-((3-chloro-4-(5,5-dimethyl-6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
57
(3-((3-chloro-4-(5-(3-phenyloxetan-3- yl)pentyl)benzyl)amino)propyl)phosphonic acid
58
(3-((3-chloro-4-(5-(1- phenylcyclopentyl)pentyl)benzyl)amino)propyl)phosphonic acid
59
(3-((3-chloro-4-(5-(1- phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid
60
(3-(((4-chloro-5-(6-phenylhexyl)pyridin-2-yl)methyl)amino)propyl)phosphonic acid
61
(3-(((4-chloro-5-(6-(4-fluorophenyl)hexyl)pyridin-2- yl)methyl)amino)propyl)phosphonic acid
62
(3-((5-chloro-2-fluoro-4-(6-(4- fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
63
(3-((3-chloro-4-(6-(4-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
64
(3-((3-chloro-4-(6-(3-fluorophenyl)hexyl)benzyl)amino)propyl)phosphonic acid
65
(3-((3-chloro-4-((5-(2- fluorophenyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid
66
(3-((4-(6-phenylhexyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
67
(3-((4-(6-(p-tolyl)hexyl)-3-(trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
68
(3-((4-(5-(1-phenylcyclohexyl)pentyl)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
69
(3-((3-(perfluoroethyl)-4-(6-phenylhexyl)benzyl)amino)propyl)phosphonic acid
70
(3-((3-(perfluoroethyl)-4-(6-(p-tolyl)hexyl)benzyl)amino)propyl)phosphonic acid
71
(3-((3-(perfluoroethyl)-4-(5-(1- phenylcyclohexyl)pentyl)benzyl)amino)propyl)phosphonic acid
72
(3-((4-((5-phenylpentyl)amino)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
73
(3-((4-((5-(p-tolyl)pentyl)amino)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
74
(3-((4-((4-(1-phenylcyclohexyl)butyl)amino)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
75
(3-((3-(perfluoroethyl)-4-((5- phenylpentyl)amino)benzyl)amino)propyl)phosphonic acid
76
(3-((3-(perfluoroethyl)-4-((5-(p- tolyl)pentyl)amino)benzyl)amino)propyl)phosphonic acid
77
(3-((3-(perfluoroethyl)-4-((4-(1- phenylcyclohexyl)butyl)amino)benzyl)amino)propyl)phosphonic acid
78
(3-((4-(6-(4-fluorophenyl)hexyl)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
79
(3-((4-(6-(4-fluorophenyl)hexyl)-3- (perfluoroethyl)benzyl)amino)propyl)phosphonic acid
80
(3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
81
(3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3- (perfluoroethyl)benzyl)amino)propyl)phosphonic acid
82
(3-((4-((5-(4-fluorophenyl)pentyl)amino)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
83
(3-((4-((5-(4-fluorophenyl)pentyl)amino)-3- (perfluoroethyl)benzyl)amino)propyl)phosphonic acid
84
(3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3- (trifluoromethoxy)benzyl)amino)propyl)phosphonic acid
85
(3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3- (perfluoroethyl)benzyl)amino)propyl)phosphonic acid
86
(3-((4-(6-(4-fluorophenyl)hexyl)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
87
(3-((4-(6-(p-tolyl)hexyl)-3-(trifluoromethyl)benzyl)amino)propyl)phosphonic acid
88
(3-((4-(5-(1-phenylcyclohexyl)pentyl)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
89
(3-((4-(5-(1-(4-fluorophenyl)cyclohexyl)pentyl)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
90
(3-((4-((5-phenylpentyl)amino)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
91
(3-((4-((5-(4-fluorophenyl)pentyl)amino)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
92
(3-((4-((5-(p-tolyl)pentyl)amino)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
93
(3-((4-((4-(1-phenylcyclohexyl)butyl)amino)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
94
(3-((4-((4-(1-(4-fluorophenyl)cyclohexyl)butyl)amino)-3- (trifluoromethyl)benzyl)amino)propyl)phosphonic acid
Biological Examples
In Vitro Assay
[0665] Compounds were tested for S1P1 activity using the GTP γ 35 S binding assay. These compounds may be assessed for their ability to activate or block activation of the human S1P1 receptor in cells stably expressing the S1P1 receptor.
[0666] GTP γ 35 S binding was measured in the medium containing (mM) HEPES 25, pH 7.4, MgCl 2 10, NaCl 100, dithitothreitol 0.5, digitonin 0.003%, 0.2 nM GTP γ 35 S, and 5 μg membrane protein in a volume of 150 μl. Test compounds were included in the concentration range from 0.08 to 5,000 nM unless indicated otherwise. Membranes were incubated with 100 μM 5′-adenylylimmidodiphosphate for 30 min, and subsequently with 10 μM GDP for 10 min on ice. Drug solutions and membrane were mixed, and then reactions were initiated by adding GTP γ 35 S and continued for 30 min at 25° C. Reaction mixtures were filtered over Whatman GF/B filters under vacuum, and washed three times with 3 mL of ice-cold buffer (HEPES 25, pH7.4, MgCl 2 10 and NaCl 100). Filters were dried and mixed with scintillant, and counted for 35 S activity using a β-counter. Agonist-induced GTP γ 35 S binding was obtained by subtracting that in the absence of agonist. Binding data were analyzed using a non-linear regression method. In case of antagonist assay, the reaction mixture contained 10 nM S1P in the presence of test antagonist at concentrations ranging from 0.08 to 5000 nM.
[0000]
TABLE 9
Activity potency: S1P1 receptor from GTP γ 35 S: nM, (EC 50 )
S1P1
Comp
IUPAC name
EC 50
No.
Structure
(nM)
1
(3-{[3-fluoro-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
4.3
2
(3-{[3-methyl-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
3.4
3
(3-{[4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
26.7
4
(3-{[3-bromo-4-(6-phenylhex-1-yn-1-yl)benzyl]amino}propyl)phosphonic acid
22.1
5
(3-{[3-fluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
4.2
6
(3-{[3-methyl-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
0.7
7
(3-{[4-(6-phenylhexyl)-3-(trifluoromethyl)benzyl]amino}propyl)phosphonic acid
11.2
8
(3-{[3-chloro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
0.5
9
(3-{[4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
6.8
10
(3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid
1.9
11
[3-({3-bromo-4-[(5-phenylpentanoyl)amino]benzyl}amino)propyl]phosphonic acid
104.8
12
[3-({3-bromo-4-[(5-phenylpentyl)amino]benzyl}amino)propyl]phosphonic acid
4.1
In Vivo Assay
Lymphopenia Assay in Mice
[0667] Test drugs are prepared in a solution containing 3% (w/v) 2-hydroxy propyl β-cyclodextrin (HPBCD) and 1% DMSO to a final concentration of 1 mg/ml, and subcutaneously injected to female C57BL6 mice (CHARLES RIVERS) weighing 20-25 g at the dose of 0.5 to 10 mg/Kg. Blood samples are obtained by puncturing the submandibular skin with a Goldenrod animal lancet at 5, 24, 48, and 72 hrs post drug application. Blood is collected into microvettes (SARSTEDT) containing EDTA tripotassium salt. Lymphocytes in blood samples are counted using a HEMAVET Multispecies Hematology System, HEMAVET HV950FS (Drew Scientific Inc.).
(Hale, J. et al Bioorg.& Med. Chem. Lett. 14 (2004) 3351).
DETAILED DESCRIPTION
[0669] A lymphopenia assay in mice; as previously described, was employed to measure the in vivo blood lymphocyte depletion after dosing with the test compound (3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid Compound-10. This S1P1 modulator, (3-{[2,5-difluoro-4-(6-phenylhexyl)benzyl]amino}propyl)phosphonic acid Compound-10 is useful for S1P-related diseases and exemplified by the lymphopenia in vivo response. Test compound, was prepared in a solution containing 3% (w/v) 2-hydroxy propyl β-cyclodextrin (HPBCD) and 1% DMSO to a final concentration of 1 mg/ml, and subcutaneously injected to female C57BL6 mice (CHARLES RIVERS) weighing 20-25 g at the dose of 0.5 mg/Kg. Blood samples were obtained by puncturing the submandibular skin with a Goldenrod animal lancet at different time intervals such as: 5, 24, 48, 72 h post drug application. Blood was collected into microvettes (SARSTEDT) containing EDTA tripotassium salt. Lymphocytes in blood samples were counted using a HEMAVET Multispecies Hematology System, HEMAVET HV950FS (Drew Scientific Inc.). Results are shown in the FIG. 1 that depicts lowered lymphocyte count after 5 hours (<1 number of lymphocytes 10 3 /μL blood). | The present invention relates to novel derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals as modulators of sphingosine-1-phosphate receptors. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a semiconductor heterostructure laser cavity more specifically usable in microlasers. These microlasers can be optically or electronically pumped and can emit in a wide wavelength range from the visible to the infrared. The emission range is a function of the materials used for the heterostructure.
More specifically, the laser cavity is pumped by a source outside the cavity more particularly permitting the emission of a visible laser light of 0.4 to 0.6 μm and which has numerous applications. Thus, such a laser can be used for the optical reading and recording of information, e.g. on audio and video compact disks, CD-ROM (compact disks--read-only memories), WORM memories (write once-read memories), erasable memories of the magnetooptical or phase change type), in laser printers and in reprography in general.
It can also be used in other applications such as e.g. in bar code readers, laboratory instrumentation, spectroscopy, biomedical instrumentation, pointers, spectacles, projection display, submarine communications, etc.
For the optical reading and recording of information, the laser cavity according to the invention makes it possible to increase the recording density and simplify the optical instrumentation. In laser printers, the cavity according to the invention permits a better definition of the image and an increase in the printing speed compared with known systems and a better adaptation of the wavelengths to photosensitive materials.
2. State of the Art
The different known semiconductor laser types are injection laser diodes which are the only semiconductor lasers at present on the market, lasers having a laser cavity pumped by an external optical source and lasers, whose cavity is externally electronically pumped. Lasers pumped by an external source have advantages compared with laser diodes, particularly as a result of the separation of the functions and the pumping elements and the laser cavity.
Thus, in injection laser diodes, these basic functions (pumping, cavity) are obtained on the semiconductor by appropriate P and N-type electrical doping of the different epitaxied layers and by ohmic electrical contacting.
The different operations involved in the manufacture of these diodes require a perfect control of the heterostructure production technology and are at present only possible with certain semiconductors from the group of III-V compounds (of type GaAlAs). This limits the wavelength range accessible to these laser diodes to between 0.6 and 1.5 μm.
In external pumping lasers, the injection of the carriers (electrons and holes), which recombine in the active zone of the semiconductor for producing light emission, by definition takes place by a source outside the active semiconductor medium. Consequently it is not necessary to carry out a P or N-type doping of the various epitaxied layers of the laser structure. It is also not necessary for there to be electrical contacts on these layers.
This greatly simplifies the metallurgy of the semiconductor active medium, where consideration only has to be given to the electrical confinement characteristics (electron pumping, quantum wells), optical confinement characteristics (emitted light guidance) and wavelength characteristics.
Thus, it is possible to use in external pumping lasers all direct gap semiconductors and in particular II-VI alloys based on Zn, Cd, Mn, Mg, Hg, S, Se, Te, in which the doping and contact technologies are either not or are only poorly controlled. However, it is not at present known how laser diodes can be made from II-VI material which are equivalent to the known III-V laser diodes. These problems increase as the gap of the materials widens and therefore the emission wavelength shortens. These problems are obviated by the design of external pumping lasers.
The possibility of using all direct gap semiconductors for external pumping lasers makes accessible the wavelength range between the blue and the mid-infrared. In particular, lasers emitting in blue-green make it possible to satisfy existing needs for all applications concerning optical recording. This range is not at present covered by injection laser diodes.
Research is at present taking place for obtaining laser diodes emitting in the blue-green, either on the basis of II-VI semiconductors with the difficulties referred to hereinbefore, or on the basis of III-V laser diodes emitting in the infrared by frequency doubling or similar non-linear effects.
Independently of the pumping mode used, three types of structure are presently used as the active semiconductor medium. These structures can comprise a solid semiconductor material, thin film-type semiconductor materials, or heterostructure-type materials.
The performance characteristics of heterostructure lasers are considerably superior to those of thin film or solid material semiconductor lasers. Heterostructures are widely used in III-V material laser diodes, particularly in the form of a GRINSCH-type structure (graded-index separate-confinement heterostructure) having a graded index optical guide and a separate confinement of the carriers (holes and electrons) and the light.
A GRINSCH-type laser diode structure is described by W. T. Tsang in Appl. Phys. Lett., 39(2), July 1981, "A graded-index waveguide separate-confinement laser with very low threshold and a narrow Gaussian beam", pp 134-136. This known laser diode structure has an active zone constituted by a quantum well located in the centre of a symmetrical composition gradient structure. This quantum well is a thin layer of a semiconductor material with a forbidden band or energy gap below that of the adjacent materials. This composition gradient induces a gap gradient and optical index. The gap gradient improves the collection efficiency of the carriers supplied by the injection current. The index gradient makes it possible to centre the guided optical mode on the active zone. This leads to a good "electron confinement", a good "optical confinement" and an optimum superimposing of the gain zone (quantum well) and the guided optical mode.
The GRINSCH structure makes it possible to obtain a very small laser threshold and it is the "conventional" structure presently used in III-V laser diodes.
Unfortunately, this conventional structure cannot be pumped by an external source because the active zone is much too far from the surface of the structure. The distance separating the active zone from the surface is >1 μm and typically 2 to 3 μm. In addition, the use of N and P doping only makes it possible with considerable difficulty to produce GRINSCH-type laser diode structures from II-VI materials.
A compact heterostructure laser of the GRINSCH type and with external electronic pumping is in particular described in FR-A-2 661 566 filed in the name of the present Applicant. This laser has as the external pumping source an electron gun with a microdot electron source. Such a semiconductor microdot laser or SML has all the advantages of external pumping and the use of a heterostructure referred to hereinbefore. However, this SML requires, in the absence of an adapted, optimized heterostructure, a high operating current in order to reach the laser threshold current density, as well as a high accelerating voltage pumping. Its energy costs can be relatively high, so that it is difficult to produce a compact system with a long life.
SUMMARY OF THE INVENTION
The present invention relates to a novel semiconductor heterostructure for a laser cavity making it possible to obviate these disadvantages. This heterostructure makes it possible to improve the performance characteristics of a laser equipped with said heterostructure and more specifically that of a SML-type laser.
More specifically, the invention relates to a semiconductor heterostructure laser cavity having semiconductor layers epitaxied on a substrate, essentially defining four zones:
a first zone whose composition varies continuously from a first face to a second face with a gap decreasing from the first to the second face, said first zone ensuring an optical confinement and light guidance,
a second zone constituting an active emission zone in contact with the second face of the first zone, having at least one quantum well with a gap smaller than that of the first zone,
a third zone having a gap larger than that of the quantum well or wells, said third zone ensuring an optical confinement and a light guidance and its composition varies continuously from a first to a second face with a gap which increases from the first to the second face, the first face of the third zone being in contact with the active zone,
a fourth zone constituting a buffer zone in contact with the second face of the third zone and the substrate, said fourth zone serving as an optical barrier for light guiding, the first and third zones being asymmetrical with respect to the active zone and defining with the latter an asymmetrical GRINSCH structure, one of the first and third zones also ensuring an electron excitation and the creation of electron-hole pairs and thus constituting one of the surfaces of the semiconductor heterostructure.
The increase and decrease of the gap can be linear, quasi-linear or parabolic.
This laser cavity leads to an improvement and a simplification of GRINSCH-type heterostructure laser cavities, more particularly making it possible to lower the operating threshold of an external pumping laser using said cavity.
The invention also relates to a laser having the cavity defined hereinbefore and external pumping means. These pumping means can be of the optical or electronic type.
Optical pumping can be provided by a lamp, a laser or a laser diode, associated with exciting light focusing optics. The wavelength of the exciting laser must be below that of the heterostructure laser cavity, whereas its energy must be higher.
Electronic pumping can be provided by a conventional electron gun like that described in "Electron beam, pumped II-VI lasers" by S. Colak, L. J. Fitzpatrick and R. N. Bargava, J. of Crystal Growth, vol. 72, pp 504 (85) and "Laser cathode ray tubes and their applications", by A. Nasibon, SPIE, vol. 893, High power laser diodes and applications (88), p 200, or by an electron gun having an electron source formed by an array or matrix of emissive microdot cathodes with cold electron emission by field effect. Such a source is described in FR-A-2 661 566. An adapted electron optics permits the focusing of the electron beam in ribbon form.
The essential function of the heterostructure is to guarantee a low threshold laser operation (<10-20 kW/cm 2 ) between 77 and 300K, as well as a low electron accelerating voltage (<10 kV) in the case of electronic pumping. This is obtained by optimizing the heterostructure and coupling between the functions fulfilled by it. In the case of ribbon focusing, it is necessary to have a low optical or electronic pumping power operation (a few Watts).
The four separate zones of the heterostructure fulfil three different functions, namely the confinement of carriers and gain, confinement of photons and collection of carriers.
The active light emission zone fulfils the electron carrier confinement and light gain function (holes and electrons). It is constituted by one or more quantum wells and optionally a superlattice or pseudoalloy formed by an alternation of quantum wells and barriers.
It is pointed out that a quantum barrier is a thin semiconductor material layer having a gap greater than that of the adjacent materials and that a quantum well is a thin semiconductor material layer having a gap smaller that that of the adjacent materials.
The composition and thickness of the quantum wells determine the laser emission wavelength. The spectral width of the gain curve is directly dependent on the growth or increase conditions of these wells and can be improved by heat treatment (or annealing) following epitaxial growth, at temperatures below 400° C. in the case of II-VI compounds and in particular between 150° and 400° C. This heat treatment ensures an interdiffusion of the semiconductor layers.
The first zone with decreasing gap gradient and increasing reflection index from the first to the second face, in principle forms the excitation zone of the laser cavity, the generation zone for the electron-hole pairs and the zone of accelerated diffusion of carriers to the active zone. Thus, this first zone fulfils the function of collecting the carriers created by the pumping beam.
For optical pumping, the exciting beam is absorbed on a few hundred nanometers. The depth is dependent on the absorption coefficient of the semiconductor material interacting with the pumping beam, said coefficient varying with the wavelength of the exciting beam and the gap of the semiconductor.
For electronic pumping, the electron-hole pairs are created over a depth Rp±dRp, in which Rp is the average penetration depth of the exciting electrons and dRp the extension of said average depth. Rp and dRp are of the same order of magnitude (a few hundred nanometers for exciting electron accelerating voltages below 10 kV) and increase with the energy of the incident electrons. The electro-hole pairs created are attracted by the active emission zone, as a result of the gap gradient of the first zone.
The first zone ensures part of the confinement of the photons and light guidance in the active zone. This photon confinement is due to the use of materials having a refraction index higher than that of the vacuum on the one hand and that of the fourth zone on the other and varies within the zones 1 and 3 in the manner defined hereinbefore.
The second part of the optical confinement and light guidance is ensured by the third zone, whose refraction index is also higher than that of vacuum on the one hand and that of the fourth zone on the other and varies within zones 1 and 3 in the manner described hereinbefore.
In certain embodiments, said third zone can also be used for creating and collecting carriers. In this case, the first zone only fulfils an optical confinement function. Advantageously the third zone has a thickness less than that of the first zone, which causes the asymmetry of the laser cavity.
In order to bring about pumping by an external source, it is necessary for the GRINSCH structure to be close to the surface of the heterostructure exposed to the exciting beam. For this purpose the first and third zones have a thickness of at the most 1 μm.
The asymmetry, whilst ensuring a good optical and electronic confinement, also ensures a centring of the guided optical mode on the emission zone, so as to obtain maximum coupling between the emitted photons and the guided mode. Conversely, in a symmetrical GRINSCH structure close to the surface (with a thin surface layer for external pumping), said coupling is not of an optimum nature. This leads to a drop in the laser efficiency and laser operation under a high current.
The asymmetry also ensures electronic pumping with low accelerating voltages. Asymmetry also ensures an optimization of the collection and confinement of the carriers created close to the surface of the cavity in the active zone. The asymmetry results from the different thicknesses of the first and third zones, as well as the slope respectively of the decrease and the increase of the gap of the first and third zones, which differ.
As it also serves as a light barrier, the fourth zone must have a refraction index equal to or below the minimum index of the third zone. This buffer zone ensures a step index adequate for ensuring the confinement of the photons in the active zone, ensures an adaption of the crystal lattice parameter between the substrate and the third confinement zone, improves the quality of the semiconductor material (structural quality and impurities) and moves the substrate away from the confinement zone and therefore the guided modes.
This buffer zone can be formed from a single material or from several layers having different compositions, or can include a superlattice or pseudoalloy. Advantageously, the buffer zone has a buffer layer essentially serving as an optical barrier and as an adapting layer.
The heterostructure according to the invention can be produced from materials which do nor do not have significant lattice unbalances or asymmetries. In the case where such asymmetries exist, it is generally preferable to keep the complete heterostructure in coherent stress, i.e. with thicknesses below the critical thickness in the active part of the structure constituted by the first, second and third zones, whereas the fourth zone (buffer layer) can be relaxed with respect to the substrate.
Thus, below the critical thickness, the lattice unbalance or asymmetry between two materials is accommodated by an elastic deformation, whereas above the critical thickness, defects (e.g. dislocations, stacking faults, twins, etc.) are created. These defects or faults can lead to a deterioration of the performance characteristics and can reduce the laser cavity life.
Still in the case of a stressed structure and for certain materials (e.g. II-VI and III-V compounds), the valence band is broken down into a so-called heavy hole band and a so-called light hole band. The radiative recombination between the electrons and the heavy holes is more effective than between the electrons and the light holes. A stressed heterostructure can therefore favour the population or occupancy of the band with heavy holes.
The materials to which the invention applies are all direct gap semiconductors and in particular III-V semiconductors (Ga, Al, In-As, P, N, Sb), II-VI semiconductors (Cd, Zn, Hg, Mn, Mg-Te, S, Se) and IV-VI semiconductors (Pb, Sn-Te, Se), etc.
For example, the heterostructure according to the invention is made from at least one of the semiconductor materials chosen from among: Cd 1-x Mn x Te, Cd x Hg 1-x Te, Cd x Zn 1-x Te, Cd x Zn z Mn 1-x-z Te, Cd x Zn 1-x Se, CdS y Se 1-y , Cd x Zn 1-x S y Se 1-y , Zn z Mn 1-z Se, Zn z Mg 1-z S y Se 1-y , Ga x Al 1-x As, Ga x Al 1-x N, with 0≦x≦1, 0≦y≦1, 0≦z≦1 and 0≦x+z≦1.
II-VI semiconductors permit a large emission wavelength adjustment range. In particular, cavities including CdHgTe can emit in the infrared and those including CdMnTe, ZnSe, ZnS, etc. can emit visible light up to the blue-ultraviolet.
In order to ensure the temperature control of the laser cavity, the latter is advantageously fitted on a thermal mass.
Advantageously, the laser cavity is fitted or mounted on said thermal mass in such a way that the epitaxied layers rest thereon. In this case, the substrate constitutes the upper part of the laser cavity and the third zone then fulfils the function of creating and collecting the carriers. In order to ensure the external pumping on said third zone, there must be a local freeing of the substrate and the buffer zone.
The asymmetrical composition gradient, quantum well laser cavity according to the invention optimizes the coupling between the optical or electronic pumping beam, the guided optical mode and the gain zone in order to improve the functions of said heterostructure.
The laser cavity according to the invention can be of the Fabry-Perot or distributed type. In this case, it has two cleaved, parallel side faces oriented perpendicular to the semiconductor layers. Semireflecting mirrors can optionally be deposited on these side faces. These semireflecting mirrors are in particular constituted by multilayer dielectric material deposits.
The laser cavity can also be guided by the light gain or index. In this case, it can have a mesa structure defining a ribbon, can be epitaxied in several stages with an alternation of etching and have implanted, interdiffused or laterally diffused regions.
An original variant associated with ribbon pumping (by optical or electron focusing) consists of obtaining a lateral confinement by a metal deposit (Ag, Au, Al or other appropriate metal) on the surface to be excited, whilst leaving an exciting ribbon free.
This metal deposit fulfils three functions:
a) local reduction, below the metal deposit, of the effective index of the guide, leading to a confinement of the guided modes at the exciting ribbon, as in the case of index-guided structures in injection laser diodes,
b) removing the heat produced by the external pumping to the thermal mass, in order to control the cavity temperature,
c) stopping electrons (electron pumping) or photons (optical pumping) arriving outside the width of the focusing ribbon.
This metal deposit can optionally be associated with a mesa-type structure or an index-guidance structure.
The production of index-guided structures is known, cf. e.g. the article "Laser diode modulation and noise" by K. Peterman, pp 36/37, ADOP Advances in Optoelectronics KTK Scientific Publishers).
Moreover, the use of a metal deposit for the lateral confinement of guided modes is known for applications other than lasers, cf. e.g. the article "Guided-wave optoelectronics" by T. Tamin, pp 326/7, Springer Series in Electronics and Photonics, 26).
By using as the pumping means a microdot source electron gun, it is possible to obtain a microlaser with a volume of a few cm 3 .
The laser cavity according to the invention can be produced with means and processes already used in microelectronics for producing semiconductor lasers.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described in greater detail hereinafter relative to non-limitative embodiments and with reference to the attached drawings, wherein show:
FIG. 1A Diagrammatically and in perspective view a Fabry-Perot laser cavity according to the invention.
FIG. 1B The evolution of the composition (x), of the gap energy (E g ) and the optical index (I o ) of the heterostructure of the cavity of FIG. 1A.
FIG. 2A The evolution of the gap (E g ) in electron-volts and that of the lattice parameter a in nanometers for II-VI compounds usable in the cavity according to the invention.
FIG. 2B Variations of the optical index for the optical confinement in a CdTe/CdMnTe heterostructure.
FIGS. 3A and 3B The emission wavelength (λe) in nanometers as a function of the composition of the active zone for a heterostructure according to the invention of CdTe/CdMnTe respectively at 300K and 77K.
FIG. 4 The variations of the manganese composition (x %) as a function of the depth (p) in nanometers or a Cd 1-x Mn x Te heterostructure, measured by SIMS spectroscopy.
FIG. 5 The creation profile of electron-hole pairs in a cavity according to the invention electronically pumped by an electron beam.
FIGS. 7 and 8 Two other variants of the laser cavity according to the invention.
FIGS. 8A to 8E Variants for fixing the cavity according to the invention to a thermal mass.
FIG. 9 Diagrammatically an embodiment of a laser according to the invention.
FIG. 10 Variations of the laser power (P 1 ) in mW as a function of the electronic excitation (E c ) of the laser in kW/cm 2 for a GaAlAs heterostructure and a CdMnTe heterostructure, measured in the quasi-continuous mode.
FIGS. 11A and 11B The laser emission spectrum of a CdTe/CdMnTe heterostructure of a cavity according to the invention excited by an electron beam for two different scales.
FIG. 12 The variations of the laser threshold power (P s ) in optical pumping, in kW/cm 2 (logarithmic scale) as a function of the operating temperature (T), in degrees K for a CdTe/CdMnTe heterostructure laser according to the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1A diagrammatically shows a distributed or Fabry-Perot laser cavity according to the invention. This laser cavity 10 comprises, starting from its upper surface 12, towards its lower surface 14, semiconductor zones 1, 2, 3 and 4 epitaxied on a semiconductor substrate 16.
These zones are epitaxied in known manner, either by molecular beam epitaxy (MBE), or by metalorganic chemical vapour deposition (MOCVD) epitaxy, or by any other similar known procedure. These zones are made from semiconductor materials of type II-VI, III-V or IV-VI with a direct gap.
The laser cavity 10 is in the form of a parallelepipedic bar, whose two sides faces 18, 20, which are parallel to one another and perpendicular to the epitaxied zones, are obtained by cleaving the zone-substrate assembly and constitute semireflecting mirrors for the entrance and exit of the laser cavity. The other side faces are not active.
In exemplified manner, said laser cavity has a thickness-reduced substrate 16 of 50 to 300 μm. The width of the laser cavity separating the non-active faces is obtained by cutting the zone-substrate assembly with a diamond saw and to a typical thickness of 1 mm. The length of the Fabry-Perot cavity, i.e. the distance separating the cleaved faces 18, 20 varies between 100 and 1000 μm. The typical value is 500 μm.
The reflectivities of the cleaved mirrors are determined by the optical index of the semiconductor and is generally approximately 30% for II-VI or III-V semiconductors. This reflectivity could optionally be improved by depositing dielectric and metallic multilayers on the cleaved faces. This deposit also protects the active faces.
The laser cavity according to the invention is optimized for an excitation or pumping by an external source of the optical or electronic pumping type. This pumping is symbolized by the particle beam 19 interacting with the laser structure in a direction perpendicular to the epitaxied zones.
According to the invention, the surface zone 1 constitutes both the excitation zone of the structure, the generation zone for the electron-hole pairs due to the exciting beam-semiconductor material interaction of the zone 1 and the accelerated diffusion zone of the carriers created in said zone towards the active zone 2. The zone 1 also fulfils the first part of the optical confinement of the light emitted in the active zone.
Zone 2 constitutes the light emission active zone, as well as the electronic confinement zone for the carriers. This active zone 2 is contiguous and adjacent to the optical confinement and excitation zone 1.
Zone 3, which is contiguous and adjacent to the active zone 2, constitutes the second part of the optical confinement zone.
Zone 4, placed between the confinement zone 3 and the substrate 16, constitutes the buffer zone and serves as an optical barrier.
According to the invention and with reference to FIG. 1B, zone 1 is made from a semiconductor material, whose composition x varies continuously from the upper surface 12 to the interface 22 of the zones 1 and 2. This variation is linear or quasi-linear. x c is used to designate the composition of the zone 1 at the surface 12 and x b to designate its composition at the interface 22.
The variation of the composition of zone 1 can be obtained in known manner either by modifying the temperature of the effusion cell which produces the atomic or molecular beam in the case of MBE, or by successive modifications of the composition of the atomic beam.
This composition is such that the gap energy E g decreases linearly or quasi-linearly from the surface 12 to the interface 22 and that conversely the optical refraction index I o increases linearly or quasi-linearly from the surface 12 to the interface 22.
E gc and N c are used to respectively designate the gap energy and the refraction index of zone 1 having the composition x c and E gb and N b respectively designate the gap energy and the refraction index of zone 2 having the composition x b .
According to the invention, the active zone 2 is constituted by one or more quantum wells, e.g. of the superlattice type, for the purpose of confining the carriers. FIG. 1B only shows two quantum wells 24, 26 separated by a quantum barrier 28. The quantum wells 24, 26 are made from a semiconductor material having a gap energy E gp below that of the zone 1 at interface 22.
The optical index N p of these wells can be of a random nature and can e.g. exceed that of the zone 1 at the interface 22. Thus, the quantum wells which are very thin are only very slightly involved in the optical confinement and light guidance, guidance being ensured by zones 1 and 3.
The quantum barrier 28 must have a gap energy above that of the quantum wells 24, 26 and can be equal to or different from that of the zone 1. In practice, the gap energy of the barrier layer 28 is equal to that of the zone 1 at the interface 22 of zones 1 and 2. This can be obtained by using the same material as that of zone 1 with the composition x b .
According to the invention, zone 3 has a semiconductor composition varying continuously from its upper surface 30 or interface between the zones 2 and 3 to its lower surface 32 or interface between zones 3 and 4. This composition is such that the gap energy of zone 3 increases linearly or quasi-linearly from the interface 30 to the interface 32 and conversely the optical index decreases linearly or quasi-linearly from the interface 30 to the interface 32.
Zone 3 can be made from a semiconductor material different from that of zone 1. In the represented example, the same composition x c is used at the surface 12 and at the interface 32 and the same composition x b at the interfaces 22 and 30.
Zone 4 can have a constant composition up to the substrate, which can be identical to or different from that of the zone 3. It must have a composition such that its refraction index is at the most equal to the index N c of zone 3 at the interface 32. It can also be constituted by two separate layers, namely an optical confinement layer 17 and an adaptation layer 19 between the layer 17 and the substrate.
According to the invention, the thickness W 1 of the zone 1 and the thickness W 3 of the zone 3 are different and in particular W 1 exceeds W 3 . Moreover, the gap energy decrease slope p 1 of zone 1 and conversely the optical index increase slope of zone 1 differs from the gap energy increase slope p 2 of zone 3 and conversely the optical index decrease slope of zone 3.
The laser structure according to the invention is consequently a GRINSCH structure with quantum wells and gap and index gradients. It is also asymmetrical with respect to the active zone and more specifically with respect to the quantum barrier 28 in the case shown in FIG. 1B.
This asymmetrical structure is particularly adapted for electronic external pumping with low electron accelerating voltages or for optical external pumping whilst having a good optical and electronic confinement. The asymmetry ensures an optimization of the structure so as to centre the guided optical mode on the active emission zone for obtaining maximum coupling between the photons emitted in the zone 2 and the guided mode. The composition variations of zones 1 and 3, the thicknesses W 1 and W 3 of zones 1 and 3, as well as the thickness W 2 of the active zone and the thickness W 4 of the buffer zone 4 are dependent on the lattice parameter differences between the different semiconductor materials, the chosen emission wavelength and the chosen group of compounds.
The laser cavity according to the invention can be made from materials which do or do not have significant lattice asymmetries or unbalances. When these exist, preferably semiconductor material thicknesses below the critical thickness are used in zones 1, 2 and 3 of the structure, whereas zone 4 can be relaxed with respect to the substrate.
As a result of the external pumping of the laser cavity according to the invention, the doping of the semiconductor zones can be of a random nature. In particular, the semiconductor layers may be non-intentionally doped. Thus, the laser cavity according to the invention can be advantageously made from II-VI material. These materials permit a wide laser emission wavelength adjustment range. In particular, the materials including CdHgTe can emit in the infrared and those including CdMnTe, ZnSe, ZnS, CdZnSe or ZnSSe can emit from the visible to the blue-ultraviolet.
In particular, the cavity according to the invention can be of Cd 1-x Mn x Te with 0≦x≦1. In this case, the higher the manganese composition x, the more the gap energy E g increases and the more the optical index decreases. Thus, in a particular embodiment, the quantum wells can be made from CdTe.
For a Cd 1-x Mn x Te heterostructure, it is possible to use a 100 nm to 1 μm zone 1, one or more small quantum wells each having a width L z from 0.1 to 100 nm, as well as a zone 3 with a thickness W from 100 nm to 1 μm, provided that W 1 >W 3 .
If x c is the manganese composition of zone 1 at surface 12 and that of zone 3 at interface 32, x b the manganese composition at interfaces 22 and 30 respectively between zones 1 and 2 and zones 2 and 3, as well as that of the barrier layer 28 and x p the manganese composition of the quantum wells, x c , x b and x p can vary from 0 to 1 with x b -x p ≧0.10 and x c -x b ≦0.10, in order to ensure a step index adequate for the optical confinement of the light emitted, as well as a capture of the carriers.
The laser cavity can also be made from Cd x Hg 1-x Te with 0≦x≦1. Here again, the more x increases, the more the gap energy E g increases and the optical index decreases.
It is also possible to use quaternary alloys of type Cd x Zn z Mn 1-x-z Te with 0≦x≦1, 0≦z≦1 and 0≦x+z<1. Published results demonstrate that an emission into the blue can be observed for CdTe quantum wells separated by MnTe barriers or ZnTe quantum wells separated by MnTe barriers.
FIG. 2A shows the gap energy variations E g expressed in electron-volts and lattice parameter a in nm for different II-VI compounds. The graph of FIG. 2 shows the binary compounds. The lines linking two binary compounds are representative of intermediate compounds between them.
For example, line a corresponds to CdHgTe compounds, line b to CdMnTe compounds, line c to ZnMnTe compounds, line d to ZnTeS compounds, line e to MnZnSe compounds, line f to ZnCdS compounds, line g to ZnSSe compounds, line h to ZnCdSe compounds, line l to CdSSe compounds, line j to HgCdSe compounds, line k to CdSeTe compounds, line l to CdSTe compounds, line m to ZnCdTe compounds and line n to ZnSeTe compounds.
All these compounds can be used for producing the cavity according to the invention respecting the gap energy conditions (cf. FIG. 1B) for the quantum barriers and wells.
FIG. 2B shows variations of the optical index for the optical confinement in the case of a CdMnTe heterostructure with quantum wells in the active CdTe zone. More specifically, FIG. 2B gives the variations N b -N c as a function of the composition difference x c -x b . The lines a', b', c' and d' respectively correspond to a composition x b of 0.30, 0.40, 0.30, 0.40 and a width L z of quantum wells of respectively 5, 5, 10 and 10 monolayers. In the present case, a monolayer with a thickness of approximately 0.32 nm represents the deposition of a layer of cadmium atoms and a layer of tellurium atoms, whilst x c equal≦1.
For each curve, the emission wavelength differs, which induces different index variations. These wavelengths are given in FIG. 2B. Thus, the optical index increases linearly when the Mn composition x decreases linearly.
The thickness limitation of the quantum well or wells is given by the critical thickness and are well known. For the pair CdTe/ZnTe, the well is limited to a thickness of 1.7 nm and for the pair CdTe/Cd 0 .96 Zn 0 .04 Te to a few hundred nm (e.g. 300 nm).
By using materials having smaller lattice asymmetries, such as e.g. the CdTe/CdMnTe structure, the critical thickness is increased, which makes it possible either to increase the thickness of the quantum well, or the number of wells. This also makes it possible to obtain a better optical confinement either by increasing the thicknesses of zones 1 and 3, or by accentuating the composition variation x c -x b .
No matter what the thickness of the well, the light gain therein remains high as a result of the confinement of the carriers in said well. Thus, the quantum well can be reduced to a few atomic layers.
The emission wavelength is dependent on the composition of the quantum wells, but particularly on their width. Thus, small fluctuations in the thickness of the well, at the atomic monolayer scale, play a fundamental part in the spectral widening of the gain curve. If the gain curve width is excessive, the maximum gain in the centre of the curve can become too small.
A good control of the morphology of the interfaces between the two materials forming the quantum well is consequently important. This is ensured by the epitaxial growth conditions. In certain cases, a subsequent heat treatment can be used for reducing the spectral dispersion of the state density, which defines the spectral width of the emission line and therefore the gain curve. For example, it is possible to use a heat treatment at 150° to 400° C. for 1 to 60 minutes. This can take place in an over or furnace following the epitaxy of the different layers of the structure or following the fitting of the laser cavity in the laser during the stoving and degassing phase of the assembly under electron bombardment.
FIGS. 3A and 3B show the variations of the emission wavelength λe in nanometers for a CdTe/CdMnTe heterostructure at respectively 300 and 77K for different well widths and different compositions of the barrier 28 between the wells. This composition of the barrier 28 is also the composition x b of zones 1 and 3 respectively at the interfaces 22 and 30 with the active zone. The wells are here of CdTe and the upper surface 12 of the zone 1 and the interface 32 between the zones 3 and 4 are respectively of Cd 1-x .sbsb.c Mn x .sbsb.c Te with X c -x b ≧0.05.
FIGS. 3A and 3B are given for a single quantum well of width L z for the active zone. For example, for x b =0.9, one obtains an emission from 540 to 775 nm at 300K for a quantum well width between 1 and 6 nm. With x b =0.2, at 77K there is an emission from 675 to 755 nm for a quantum well width between 1 and 6 nm.
On the basis of these curves, it can be seen that the emission wavelength increases with the width of the quantum well also decreases with the value of x b . It is possible to further shorten the emission wavelength by using CdMnTe instead of CdTe quantum wells.
Specific examples of the construction of a laser cavity according to the invention will now be given using a CdTe/Cd 1-x Mn x Te heterostructure.
EXAMPLE I
Zone 1 has a thickness of 500 nm and a Mn composition varying continuously from the surface 12 to the interface 22 between zones 1 and 2 of 0.22 to 0.17. The active zone 2 is constituted by two CdTe wells of 6 nm each, separated by a 15 nm CdMnTe barrier with an Mn composition of 0.17. Zone 3 has a thickness of 150 nm and a Mn composition varying from the interface 30 between zones 2 and 3 to the interface 32 between zones 3 and 4 from 0.17 to 0.22. The buffer layer 4 is a 1.5 μm CdMnTe layer with a Mn composition x of 0.22. The substrate is of CdTe of orientation 100.
EXAMPLE II
Example II differs from example I by the use of a lattice adapting layer 19 between the buffer layer and the substrate. This adapting layer is a superlattice constituted by 5 CdTe, wells, each having a thickness of 6 nm, alternating with 4 15 nm CdMnTe barriers with a Mn composition of 0.22.
This structure was controlled by SIMS spectroscopy, as shown in FIG. 4. It gives the variations of the manganese composition x as a function of the depth p in nm. These measurements are only given for information purposes, in view of the calibration and resolution problems inherent in this analysis type.
The laser cavity according to the invention can be electronically pumped with an electron beam. The latter produces electron-hole pairs at an average depth R p increasing with the electron accelerating voltage and which is dependent on the semiconductor materials of the laser cavity. These pairs are created over a depth d Rp around R p .
For a maximum electronic pumping efficiency, R p and d Rp must be matched to the heterostructure dimensions. Thus, the electron-hole pair creation profile must have its maximum in heterostructure zone 1, as can be clearly gathered from FIG. 5.
Curve A is the electron-hole pair creation profile and gives the variations of the number N of electron-hole pairs as a function of the heterostructure depth p. FIG. 5 also shows the variations of the gap energy E g of the heterostructure as a function of the depth p. The capture of these electron-hole pairs takes place at the heterostructure zones 1 and 3, as indicated by the arrows F.
By using, in accordance with the invention, a heterostructure having a limited thickness (below 5 μm), it is possible to use low electron accelerating voltages (below 20 kV), which leads to an easier, more compact and more reliable fitting of the laser. Typically, use is made of a 10 kV electron beam. For II-VI compounds, such a beam has an average penetration depth of 250 nm and an extension d RP of approximately 400 nm.
The function of the passage of the carriers to the quantum wells of the active zone is particularly important for narrow wells and therefore for structures emitting at low wavelengths, because they have a smaller effective capture cross-section than that of wider wells. This is particularly the case for a CdMnTe heterostructure with CdTe quantum wells.
The variations of the optical index of the zones 1 and 3 ensure the existence of a guided wave, which has been revealed by the inventors for the heterostructure of example I by the so-called "m-line" method.
A TEO (transverse-electric-optical) guided mode with an effective index of 2.84 was obtained. It is pointed out that the real optical index of CdTe is 2.955 and that of the Cd 1-x .sbsb.c Mn x .sbsb.c Te zone 4 with x c =0.22 is 2.825 at the laser emission wavelength of around 770 nm.
This guided mode is defined by the index gradient in zones 1 and 3, by the step index between the heterostructure surface 12 and the environment and by the step index, when it exists, between zone 3 and the buffer layer 17. The thickness of the zones 1 and 3 are calculated so as to centre the TEO mode on zone 2.
In FIG. 5, curve B gives the intensity variations of the guided mode as a function of the heterostructure thickness p.
The optical confinement increases as the step index between the real indexes N c and N b of zones 1 and 3 increases. This imposes significant composition variations. However, due to the critical thickness, the maximum step index for a given heterostructure is limited. In exemplified manner, FIG. 2B shows the maximum step index obtainable with a CdMnTe heterostructure.
As a result of the asymmetry of the heterostructure, i.e. of zones 1 and 3, the guided mode has its maximum amplitude at the active zone thus ensuring an optimum coupling with the light gain.
The heterostructure must be formed with coherent epitaxy, i.e. below the critical thickness such that it can be modelled on the basis of experimental measurements well known to the Expert.
With the structures of examples I and II, a laser emission was obtained at ambient temperature and low temperature, both with an optical excitation with the aid of a laser and with an electronic excitation with the aid of electron gun using a microdot electron source as described in FR-A-2 661 566.
Other constructional examples of a laser cavity according to the invention will now be described.
EXAMPLE III: GaAs/GaAlAs STRUCTURE
This structure has little lattice asymmetry or unbalance and the critical thickness problems do not occur, unlike in the case of CdMnTe structures. Moreover, it as larger optical index variations and therefore a better optical confinement that CdMnTe structures. However, this structure has a less pronounced possibility of adjusting the emission wavelength, which varies very little around 0.8 μm.
Zones 1 to 4 can be of Ga 1-x Al x As with 0≦x≦1, provided that the quantum wells of active zone 2 have an aluminium composition lower than that of zones 1 and 3 for ensuring electron confinement. Zones 1 and 3 can have thicknesses from 100 to 1000 nm and the active zone a thickness from 0.5 to 200 nm, whilst respecting the asymmetry condition W 1 >W 3 .
In particular, a heterostructure was produced having a zone 1 350 nm thick with a composition x c on surface 12 of aluminum of 0.5 and a composition x b at the interface 22 with zone 2 of 0.20. The active zone is constituted by a 10 nm thick GaAs quantum well. The zone 3 has a composition x b of 0.20 at the interface 30 between zones 2 and 3 and a composition x c at the interface between zones 3 and 4 of 0.50, its thickness being 200 nm.
The buffer zone comprises a first buffer layer 17 of thickness 800 nm of Ga 1-x Al x As with x=x c (i.e. 0.50) epitaxied on an adaptation layer constituted by a superlattice and having a thickness of 150 nm. It has in alternating from 5 GaAs quantum wells, each 10 nm thick and 5 quantum barriers of composition x c (i.e. x c =0.50), each having a thickness of 10 nm. The superlattice is deposited on a 50 nm GaAs layer.
The GaAs substrate is of crystal orientation 100.
According to the invention, the GaAlAs layers and in general terms the III-V material heterostructures according to the invention are not intentionally doped.
As hereinbefore, the structure is asymmetrical and the active zone is close to the surface, thus ensuring its pumping by an external optical or electronic source having a guided mode with its maximum amplitude in the quantum well of the active zone.
EXAMPLES IV TO VI
Heterostructures based on selenide and sulphide (cf. FIG. 2A) were envisaged for emission in the blue, without doping of the material, according to the invention.
Using one or more Cd x Zn 1-x Se wells with x between 0 and 1, it is possible to use zones 1 and 3 of variable ZnS y Se 1-y composition with 0≦y≦1 (example IV).
For quantum wells in the active zone of CdS y Se 1-y with 0≦y≦1, it is possible to use variable CdSSe compositions for zones 1 and 3 (example V), provided that zones 1 and 3 have a gap greater than that of the quantum well (E g increasing linearly with y).
It is also possible to produce a Zn z Mn 1-z Se heterostructure with 0≦z≦1 (example VI) by respecting the gap energy values of zones 1, 2 and 3 (E g increasing when the Mn composition increases). In these heterostructures, it is also necessary to take account of the critical thickness constraints, as in CdMnTe structures.
EXAMPLES VII TO IX
Quaternary II-VI semiconductor material heterostructures were also envisaged using the following materials: Cd x Zn z Mn 1-x-z Te, Cd x Zn 1-x S y Se 1y and Zn z Mg 1-z S y Se 1-y with 0≦x≦1, 0≦y≦1, 0≦z≦1 and 0≦x+z≦1.
EXAMPLES X TO XIII
These examples relate to laser emissions in the infrared. Lasers emitting in the infrared can be produced from II-VI materials including mercury, such as Cd x Hg 1-x Te materials with x between 0 and 1 (example X) or from IV-VI materials of type Pb x Sn 1-x Te (example XI), Pb x Eu 1-x Se (example XII), Pb x Eu 1-x Se y Te 1-y (example XIII) with x between 0 and 1 and y between 0 and 1 with 0≦x+y≦1.
In CdHgTe heterostructures, more particular use is made of CdHgTe quantum wells. The critical thickness problems are of a secondary nature with these materials.
With lasers emitting in the infrared and in particular those with an emission wavelength exceeding 1 μm, it is possible to use III-V material laser diodes emitting at around 800 nm as the external pumping source.
According to the invention, it is possible to consider other laser cavity types than that of FIG. 1A. In particular, the cavity according to the invention can have a mesa structure like that shown in FIG. 6. In this case, the epitaxied layers (zones 1 to 4) and optionally part of the substrate 16 are chemically dry or wet etched in order to obtain a ribbon 40 extending from the cleaved faces 18 and 20, in a direction perpendicular thereto. The width L of the ribbon can vary between 2 and 50 μm and the typical value is 5 to 10 μl m.
The etching of the epitaxied layers also permits a lateral confinement of the laser cavity excitation zone.
The laser cavity according to the invention can also have the structure shown in FIG. 7. In this embodiment, the ribbon 40a for confining the external optical or electronic excitation is obtained by a metal deposit 42 on the surface 12 of the stack of epitaxied layers. This deposit has a ribbon-like opening 43 in its median part. The ribbon 40a is oriented perpendicular to the cleaved faces 18, 20. It characteristics are identical to those described relative to FIG. 6. The thickness of the layer 42 exceeds 20 nm. The metal used can be silver, gold or aluminium.
Apart from the lateral confinement, said etched metal deposit removes the excess energy resulting from the heat produced by the pumping beam. Moreover, it can stop electrons or photons, as a function of the pumping type used, which are emitted outside the excitation ribbon 40a.
When the deposit 42 is used for cooling or spatial filtering of the electron or photon beam, its thickness must be adequate to stop the electrons or photons and also so as to ensure a good heat conduction. In this case, the layer 42 has a thickness between 0.2 and 2 μm.
According to the invention, the laser cavity 10 is placed on a thermal mass, as shown in FIGS. 8A to 8E. This thermal mass carries the reference 44 and is made from a good heat conducting metal, particularly copper.
In FIG. 8A, the laser cavity 10 is fixed by its lower surface 14 to the mass 44 with the aid of a weld 46, e.g. indium or a heat and electricity conducting adhesive or glue.
The adhesion of the weld 46 to indium can be ensured by successively depositing on the lower face 14 of the laser cavity an approximately 10 to 50 nm thick chromium layer and then an approximately 50 to 200 nm gold layer, followed by an indium layer used for the weld and having a thickness of 0.05 to 2 μm. An indium deposit is also made in this way on the thermal mass 44.
After positioning the laser cavity 10 equipped with its three metal layers on the mass 44, heating takes place to between 160° and 180° C., in order to melt the indium and then cooling takes place to ambient temperature. Heating can also be used for the annealing of the heterostructure.
When an etched metal deposit 42 is used for the lateral confinement of the excitation, the cavity 10 can be placed on the thermal mass 44, as shown in FIG. 8B. In this case, apart from the weld 46 by the rear face 14 of the cavity, it is possible to use an indium deposit 48 on the metal confinement layer 42, as well as on the non-active side faces (i.e. perpendicular to the cleaved faces) of the laser cavity.
It is also possible to replace the indium surface weld 48 by metal parts 50, like those shown in FIG. 8C. These parts 50 are e.g. made from copper.
Obviously, the indium weld 48 and metal parts 50 must have an opening facing the exciting ribbon 40a.
In an original installation variant shown in FIG. 8D, in order to obtain a very effective cooling of the laser cavity 10, the thermal mass 44 can be fitted in the reverse manner to what is shown in FIGS. 8A and 8C. In other words, the epitaxied layers rest on the thermal mass 44, fixing being ensured by the weld 46 bearing on the upper surface 12. With such a reversed fitting procedure, as in the variants of FIGS. 8B and 8C, it would be possible to have a not shown metal coating 48 or 50 bearing on the surface 14 and therefore on the substrate 16 of the cavity 10.
In order to ensure an optical or electronic pumping with an external source, the laser cavity according to the invention must have a clearance 52 up to the zone 3. This clearance 52 is obtained by local chemical etching of the substrate 16 and the zone 4 over the entire thickness thereof.
In this operating case, the zone 3 serves as an exciting and collecting zone. The functions of the zones 1 and 3 are reversed compared with the normal excitation case on the surface 12. In particular, the respective thicknesses W 1 and W 3 of the layers 1 and 3 must be specially designed for this reverse case with W 3 >W 1 .
In order to facilitate the etching of zone 4, an etching stop layer 54 able to withstand the etching agents of zone 4 can be interposed between zones 3 and 4, as shown in FIG. 8D. It must therefore be made from a material different from that of zone 3.
For a CdMnTe heterostructure, the layer 54 can be of CdMnTe with a higher Mn concentration than that of the layer 4 and can have a thickness of 10 to 500 nm. For a GaAlAs heterostructure, use is made of GaAlAs with a Al concentration different from that of layer 4.
In the reverse fitting procedure, in the manner shown in FIG. 8E, it is also possible to deposit a supplementary layer 56 on zone 1, in order to move it away from the surface 12 in contact with the weld 46. This layer 56 can have the same characteristics as zone 4. In this case, the asymmetry of the structure is also reversed with W 3 >W 1 .
The optical pumping of heterostructures of CdMnTe, GaAlAs or the quaternary alloys referred to hereinbefore, can take place with a laser emitting in the visible range (e.g. at 532 nm with a double YAG laser or with an argon laser emitting in the blue-green).
In the case of electronic pumping, it is possible to use a conventional electron gun or an electron gun equipped with a microdot source. An electron gun laser having a microdot source with a heterostructure according to the invention is shown in FIG. 9. This laser has a vacuum enclosure 60 equipped with a vacuum pump 62 and not shown windows for the exit of the laser emission produced by the cavity 10. The enclosure could also be vacuum sealed in order to permit autonomous operation without a vacuum pump. For example, the enclosure 6 is raised to earth potential.
The electron gun 61 for exciting the cavity 10 has a microdot cold source 63, whose precise structure is that described in FR-A-2 661 566. It is constituted by a molybdenum microdot matrix or array supported by cathode electrodes having the form of parallel strips. Grids, isolated from the cathode electrodes and also in the form of parallel strips, are positioned perpendicular to the cathode electrodes and have openings facing the microdots.
The cavity 10 is fitted on an anode 64 raised to high voltage by means of an external source 66. Between the anode 66 and the cold source 63 there is an array 68 of electrodes for focusing onto the upper surface 12 or zone 3 (FIG. 8D) of the laser cavity, the electron beam 70 emitted by the source 63.
This array 68 is arranged so that the electron beam 70 strikes the surface facing the cavity 10 in the form of a ribbon 72, whose length L' is at the least equal to the distance separating the active faces 18, 20 of the laser cavity and whose width l is between 5 and 200 μm.
This electrode array 68 is arranged so as to also serve as an electrostatic shield for the cold source against the high voltage applied to the anode 64. For this purpose, it has at least two pairs of electrodes with different dimensions, namely a first pair 74 and 76 brought to an external positive electric supply source 78 and a second pair 80, 82 connected to a negative external electric power source 84.
The electrodes 74 and 76 are arranged symmetrically with respect to the longitudinal axis 86 of the electron gun. This also applies with respect to the electrodes 80 and 82.
An operational example of the laser of FIG. 9 according to the invention will now be given. The laser cavity 10 is raised to a positive voltage of 3 to 10 kV by means of the anode 64.
The electron beam 70 produced by the source 63 and then focused by the electrode array 68 in the form of a ribbon creates in the zone 1 of cavity 10 electron-hole pairs, which are captured by the quantum well active zone. These electron-hole pairs recombine in the active zone in order to produce light, whose wavelength is dependent on the heterostructure of the laser cavity. For CdMnTe structures, emission takes place between the red and the blue-green.
For an electron-hole pair density beyond a certain threshold dependent on the heterostructure, stimulated emission takes place and an optical gain appears. The photons emitted in the active zone are confined in the laser cavity and if the optical gain is sufficiently high to compensate the losses, then laser emission takes place. The net gain necessary at the laser threshold is typically 20 to 40 cm -1 . The power density at the laser threshold is typically 1 to 20 kW/cm 2 .
The total power "P" received by the laser cavity is much dependent on the focusing of the beam and in particular the excitation ribbon width l. For a given target of length L (Fabry-Perot cavity length) and for a useful electron density D, the power will be P=D.L.l.
For a given acceleration voltage V applied to the anode, the electron current I is defined by I=D.L.l/V.
NUMERICAL EXAMPLE
With V=10 kV, L=600 μm and D=2 kW/cm 2 , we obtain:
for L=150 μm, P=1.8 W and I=180 μA, and
for l=10 μm, P=120 mW and I=12 μA.
These numerical values shows that a good focusing, corresponding to the minimum ribbon width l makes it possible to reduce the total power supplied by the gun and therefore simplify its cooling, accept higher laser threshold densities as a result of the fact that, for the same power, the excitation current density is increased by a good focusing of the electron beam and significantly decrease the laser operating current, so that there is less stressing of the microdot source.
The heat given off by electron bombardment is removed by the thermal mass, which can be associated with a Peltier element or a cryostat.
FIG. 10 shows a typical result of the operation of two Fabry-Perot laser cavities of GaAs/GaAlAs emitting at 830 nm and CdTe/CdMnTe emitting at 760 nm. FIG. 10 gives the variations of the laser power P 1 in mW, as a function of the electron excitation E c in kW/cm 2 .
Curve I relates to GaAlAs and curve II to CdMnTe. The laser cavities are those of examples II and III. These laser powers were established at approximately 90K for an electron acceleration voltage of 10 kV and a 150/600 μm ribbon. The electron gun is that of FIG. 9. The emitted powers are a few hundred milliwatts with differential efficiencies of 8.9% for GaAlAs and 8.3% for CdMnTe.
The laser thresholds are respectively approximately 1 and 1.5 kW/cm 2 . These thresholds increase by a factor of 5 to 10 at ambient temperature. For the laser of FR-A-2 661 566, the laser threshold is a few dozen kW/cm 2 and in the aforementioned document "Electron beam pumped II-VI lasers" by S. Colak et al, the given thresholds are a few hundred kW/cm 2 , i.e. much higher than those of the laser according to the invention.
As the power received by the laser cavity is high (a few watts), the laser operation is quasi-continuous. Electron pulses of 5 μs spaced by 250 to 500 μs permit this quasi-continuous operation, whilst ensuring the cooling of the cavity.
FIGS. 11A and 11B give the emission spectrum of a laser cavity according to example I. These curves give the laser intensity I l in arbitrary units as a function of the wavelength λ in nanometers. FIG. 11B is an enlargement of FIG. 11A at the emission peak.
FIG. 11A shows the refinement of the emission line and the sudden laser intensity increase as from 763 nm. FIG. 11B shows details of this emission line. These curves were plotted for a laser like that of FIG. 9 operating at 90K and using a 10 kV electron beam.
Identical results were obtained for optical pumping on a CdMnTe laser cavity. The results are given in FIG. 12. It gives the variations of the threshold power P s in kW/cm 2 as a function of the laser operating temperature T in degrees K. The exciting wavelength is in this case 532 nm. | A semiconductor heterostructure laser cavity is disclosed which has semiconductor layers epitaxied to define four zones on a substrate. The laser cavity includes a first zone with a composition that varies continuously from a first face to a second face with a gap decreasing from the first face to the second face, the first zone ensuring an optical confinement and light guidance. A second zone constitutes an active emission zone in contact with the second face of the first zone and having at least one quantum well with a gap smaller than that of the first zone. A third zone has a gap larger than that of the at least one quantum well. The third zone ensuring an optical confinement and a light guidance, and having a composition which varies continuously from a first face to a second face with a gap which increases from the first face to the second face, the first face of the third zone being in contact with the active emission zone. A fourth zone constitutes a buffer zone which contacts the second face of the third zone and a substrate, the fourth zone serving as an optical barrier for light guiding, the first and third zones being asymmetrical with respect to the active emission zone to define an asymmetrical GRINSCH structure, one of the first and third zones constituting a surface of the semiconductor heterostructure for ensuring electron excitation and creation of electron-holes. | 7 |
TECHNICAL FIELD
[0001] The invention relates to a cleaning head for a mop, comprising a clamping strip and a cleaning body, the cleaning body being accommodated in the clamping strip with a force fit and/or interlocking fit, the clamping strip being substantially channel shaped and being open towards the cleaning body and having two side walls and one connecting strip which connects the side walls to each other, the connecting strip having an inner side which faces the cleaning body and an outer side which faces away from the cleaning body, the clamping strip having a connecting region which extends in the longitudinal direction of the cleaning head for the purpose of connecting the clamping strip to a mop adapter which accommodates the cleaning head, the connecting region having, on the outer side of the connecting strip, at least one stop which can be placed on a counter stop on the adapter, and the stop being arranged in an imaginary plane which extends parallel to the connecting strip.
BACKGROUND
[0002] An example of a cleaning head is described in U.S. Pat. No. 4,908,901. Attachment means are arranged on the outer side of the connecting strip, said attachment means protruding outwards from the outer side of the connecting strip, away from the cleaning body. These attachment means may, for example, be in the form of fastening tabs which are formed integrally with the clamping strip.
[0003] The design of the clamping strip makes it inconvenient and time-consuming for users to change the cleaning head.
[0004] Usually, cleaning heads are sold separately from mops as spare parts. In such cases, the cleaning heads are packaged individually in plastics film or cardboard. The protrusion of the attachment means from the outer side of the connecting strip not only increases the dimensions of the packaging of a cleaning head of this type by the height of the attachment means, but also poses the risk of the packaging becoming damaged whilst the cleaning head is being transported or being stored in a retail outlet, especially since the attachment means are frequently manufactured with sharp edges.
[0005] A further disadvantage is that when changing the cleaning head, it is easy for users of the mop to injure themselves on the attachment means which protrude perpendicularly from the outer side of the connecting strip.
SUMMARY
[0006] In an embodiment, the present invention provides a cleaning head for a mop comprising a clamping strip and a cleaning body. The cleaning body fits in the clamping strip. The clamping strip is channel shaped and open towards the cleaning body and having two side walls and one connecting element connecting the side walls to each other. The connecting element has an inner side which faces the cleaning body and an outer side which faces away from the cleaning body. The clamping strip has a connecting region to connect the clamping strip to a mop adapter which accommodates the cleaning head. The connecting region has a stop which acts in an axial direction of a handle of the mop and is configured to be placed on a counter stop on the adapter. The stop is disposed in an imaginary plane extending parallel to the connecting strip. An attachment mechanism is in the imaginary plane.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] The present invention will be described in even greater detail below based on the exemplary figures. The invention is not limited to the exemplary embodiments. All features described and/or illustrated herein can be used alone or combined in different combinations in embodiments of the invention. The features and advantages of various embodiments of the present invention will become apparent by reading the following detailed description with reference to the attached drawings which illustrate the following:
[0008] FIG. 1 is a cleaning head according to the invention as an individual component and a mop which comprises an adapter for accommodating the cleaning head;
[0009] FIG. 2 is the mop from FIG. 1 , in which the cleaning head is connected to the handle of the mop by means of the adapter;
[0010] FIG. 3 is the cleaning head, which is connected to the adapter, in a simplified view; and
[0011] FIG. 4 is a cleaning head which is similar to the cleaning head in FIG. 1 , but the locking lugs being arranged differently.
DETAILED DESCRIPTION
[0012] An aspect of the invention is to develop a cleaning head that can be changed quickly and easily and has a low volume when it is packaged, the packaging that surrounds the cleaning head does not become damaged during transportation and storage, and the risk of users injuring themselves when using the cleaning head is reduced to a minimum.
[0013] The aspect is achieved in that at least one attachment means is arranged in the imaginary plane.
[0014] An advantage of this is that the connecting region, despite having at least one attachment means, is substantially flat and, as a result, the attachment means in the connecting region hardly protrudes perpendicularly above the plane in which the stop is arranged. Overall, the cleaning head is compact in size and the cleaning head packaging does not become damaged if, for example, cleaning heads are packaged and stored one on top of the other. It is also advantageous that, as a result of the attachment means being arranged in the plane, it is especially easy and unproblematic for users to handle the cleaning head when, for example, they have damp and/or slippery hands.
[0015] The arrangement of the attachment means in the plane allows the cleaning head to be manufactured easily and inexpensively.
[0016] The arrangement of the attachment means in the plane results in the outer side of the connecting strip being formed in the connecting region without any disruptive projections and in it being particularly easy to attach the cleaning head to the adapter. The components can be attached to each other quickly and easily with a precise fit and without any canting. Whilst the mop is being used for its intended purpose, the cleaning head and the adapter are connected to each other precisely and largely without play. This means that the mop is particularly comfortable to use.
[0017] An embodiment of the cleaning head according to the invention is explained in more detail below with reference to FIG. 1 to 4 .
[0018] FIG. 1 shows an embodiment of the cleaning head according to the invention as an individual component in a non-assembled state.
[0019] The handle 21 of the mop 1 is also shown, the mop handle 21 forming a preassembled unit 26 together with the adapter 11 .
[0020] The mop handle 21 comprises a system of rods 32 operated by a hand lever 31 , the system of rods 32 being connected to the adapter 11 as can be seen more clearly in FIG. 3 . Operating the hand lever 31 allows the adapter 11 to be moved up and down as required in the axial direction 33 of the mop handle 21 between the two mop-wringing rollers 34 , 35 , the cleaning body 3 of the cleaning head which is connected to the adapter 11 being drawn through the mop-wringing rollers 34 , 35 by the upward movement and thereby being wrung out. After the cleaning body 3 has been wrung out, a downward movement shapes the cleaning head into the ready-to-use form thereof (cf. FIG. 2 ).
[0021] In the embodiment described herein, the cleaning head comprises a stainless steel clamping strip 2 , the cleaning body 3 taking the form of a cleaning sponge and being accommodated in the clamping strip with a force fit and interlocking fit. The interlocking fit can be formed for example by the two side walls 4 , 5 having, on the sides thereof facing each other, retaining hooks which penetrate the surface of the cleaning body 3 .
[0022] The clamping strip 2 is formed in the shape of a channel, is open in the axial direction 33 towards the cleaning body 3 and is delimited by the two side walls 4 , 5 which are connected to each other by the connecting element 6 .
[0023] The connecting region 10 is arranged on the outer side 8 of the connecting strip 6 , said outer side facing away from the cleaning body 3 and said connecting region marking the region on the outer side 8 of the connecting strip 6 which is covered by the adaptor 11 when the mop 1 is ready for use. This connecting region 10 is shown for example particularly clearly in FIG. 3 .
[0024] The connecting region 10 on the outer side 8 of the connecting strip 6 is in the form of a flat stop 13 which is arranged in the imaginary plane 12 . The attachment means is also arranged in the imaginary plane 12 .
[0025] In the embodiment described, the attachment means is formed of the two locking lugs 15 , 16 , which are components of the connecting strip 6 and extend in the connecting region 10 transversely to the longitudinal direction 9 . The locking lugs 15 , 16 extend transversely to the longitudinal direction 9 beyond their respective side walls 4 , 5 , each forming an undercut 17 , 18 . The locking projections 27 , 28 on the adapter 11 snap into place to connect to the locking lugs 15 , 16 . To release the cleaning head from the adapter 11 , the locking projections 27 , 28 on the adapter 11 are moved away from each other transversely to the longitudinal direction 9 in the opposite direction to the direction in which they were locked together by operating the lever 30 , thereby releasing the locked connection between the cleaning head and the adapter 11 . The cleaning head can, for example, subsequently be changed.
[0026] On the sides which face each other, the cleaning head and the adapter 11 have a stop 13 and a counter stop 14 , said stops coming into contact with each other.
[0027] As can be seen in FIG. 1 , the locking lugs 15 , 16 on the side walls 4 , 5 are offset from each other in the longitudinal direction 9 in such a way that the strength of the material of the connecting strip 6 in the region of the locking lugs 15 , 16 is only negligibly weakened.
[0028] In the embodiment described herein, the only components to protrude beyond the plane 12 are the positioning knobs 19 , 20 , making it easier for users to position the cleaning head relative to the adapter 11 . The preassembled unit 26 , which comprises the mop handle 21 and the adapter 11 , is placed on the cleaning head in the axial direction 33 , in such a way that the adapter 11 and its inner side 25 , which is in the form of a counter stop 14 , comes into contact with the stop 13 on the clamping strip 2 . Pressure is then applied to the mop handle 21 in the axial direction 33 and the locking projections 27 , 28 on the adapter 11 , which are formed integrally with the side webs 22 , 23 , interlock with the locking lugs 15 , 16 on the cleaning head.
[0029] FIG. 2 shows the mop 1 ready for use, the components shown in FIG. 1 being attached together.
[0030] FIG. 3 shows a detailed view of the mop 1 , in which, for the sake of clarity, the mop-wringing rollers 34 , 35 from FIGS. 1 and 2 are not shown.
[0031] The cleaning head is connected to the adapter 11 with an interlocking fit, the locking projections 27 , 28 on the adapter 11 being able to be opened by a release mechanism 29 and thereby released from the locking lugs 15 , 16 on the cleaning head without being destroyed. In the embodiment described herein, the release mechanism 29 is formed of a lever 30 which pulls the connecting web 24 downwards. The connecting web 24 connects the side webs 22 , 23 on the adapter 11 to each other.
[0032] As described above, the cleaning head is released from the adapter 11 as a result of the lever 30 being moved upwards by, for example, the user's foot. The locking projections 27 , 28 on the adapter 11 are consequently moved away from each other transversely to the longitudinal direction 9 and release the locking lugs 15 , 16 on the cleaning head and thereby the entire cleaning head as shown in FIG. 1 .
[0033] FIG. 4 shows a cleaning head which is similar to the cleaning head in FIG. 1 , the locking lugs 15 , 16 being arranged differently on the outer side 8 of the clamping strip 2 . The locking lugs 15 , 16 are arranged directly opposite each other when viewed in the longitudinal direction 9 . The way in which the locking lugs 15 , 16 are arranged directly opposite each other means that no moments occur when connecting/releasing the cleaning head to/from the adapter 11 , thereby preventing canting when attaching/removing the cleaning head. An arrangement of this type at the same time allows the locking lugs 15 , 16 to engage with or to be released from the adapter 11 . This makes the cleaning head easier to handle.
[0034] Lead-in chamfers 36 , 37 for the self-centring assembly of the clamping strip 2 in the longitudinal direction 9 relative to the adapter 11 can be arranged on the sides of the side walls 4 , 5 which face away from each other. In the embodiment described herein, the lead-in chamfers 36 , 37 are arranged trapezoidally to each other and interact with correspondingly designed guide bars on the adapter 11 .
[0035] During assembly, the components to be attached together 2 , 11 are thereby automatically positioned relative to one other in the longitudinal direction 9 and subsequently interlocked.
[0036] While the invention has been illustrated and described in detail in the drawings and foregoing description, such illustration and description are to be considered illustrative or exemplary and not restrictive. It will be understood that changes and modifications may be made by those of ordinary skill within the scope of the following claims. In particular, the present invention covers further embodiments with any combination of features from different embodiments described above and below.
[0037] The terms used in the claims should be construed to have the broadest reasonable interpretation consistent with the foregoing description. For example, the use of the article “a” or “the” in introducing an element should not be interpreted as being exclusive of a plurality of elements. Likewise, the recitation of “or” should be interpreted as being inclusive, such that the recitation of “A or B” is not exclusive of “A and B,” unless it is clear from the context or the foregoing description that only one of A and B is intended. Further, the recitation of “at least one of A, B and C” should be interpreted as one or more of a group of elements consisting of A, B and C, and should not be interpreted as requiring at least one of each of the listed elements A, B and C, regardless of whether A, B and C are related as categories or otherwise. Moreover, the recitation of “A, B and/or C” or “at least one of A, B or C” should be interpreted as including any singular entity from the listed elements, e.g., A, any subset from the listed elements, e.g., A and B, or the entire list of elements A, B and C. | A cleaning head for a mop comprising a clamping strip and a cleaning body. The cleaning body fits in the clamping strip. The clamping strip is channel shaped and open towards the cleaning body and having two side walls and one connecting element connecting the side walls to each other. The connecting element has an inner side which faces the cleaning body and an outer side which faces away from the cleaning body. The clamping strip has a connecting region to connect the clamping strip to a mop adapter which accommodates the cleaning head. The connecting region has a stop which acts in an axial direction of a handle of the mop and is configured to be placed on a counter stop on the adapter. The stop is disposed in an imaginary plane extending parallel to the connecting strip. An attachment mechanism is in the imaginary plane. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a pellicle used in a step of photolithography in the production of integrated circuits for the purpose of preventing dust and dirt from adhering onto the mask or the reticle (hereinafter simply referred to as mask and the like). More specifically, the invention relates to a pellicle of which an adhesive resin layer for mounting the pellicle on the mask is formed of a hard resin layer and a soft resin layer.
2. Description of the Prior Art
In the above-mentioned pellicle, in general, a transparent pellicle film of a nitrocellulose or the like is stretched, via an adhesive layer, on an end of a pellicle frame made of aluminum or the like, and the other end of the pellicle frame is adhered with an adhesive (mask-adhering) layer onto the pattern-forming surface of the mask or the like, so that the pellicle will not be removed from the mask or the like during the handling.
When the mask-adhering agent exhibits a too strong adhering force, therefore, the mask is damaged due to the application of an excessive force at the time of peeling the pellicle off the mask and the like or the mask-adhering agent remains on the mask after it has been peeled off. As a result, the semiconductor devices could become defective or the yield of production decreases.
From such a point of view, there have been proposed a pellicle with a mask-adhering agent exhibiting a weaker adhering force to the mask than to the pellicle (Japanese Unexamined Patent Publication (Kokai) No. 75835/1985), and a pellicle using a mask-adhering agent having a hardness of not larger than 200 gf (Japanese Unexamined Patent Publication (Kokai) No. 282640/1998).
Despite the mask-adhering layer formed between the mask and the pellicle frame has an adhering force as taught in the above prior art (Japanese Unexamined Patent Publication (Kokai) No. 75835/1985), however, the mask is distorted and loses flatness. That is, when the mask loses flatness, the pattern formed on the mask is distorted, and a correct pattern is not transferred onto the wafer.
In the step of photolithography, furthermore, exposure to light is effected not only where flat surfaces of the mask and of the pellicle film are maintained in a horizontal direction but also where flat surfaces of the mask and of the pellicle film are maintained in a vertical direction. When the surface of the mask is maintained in the vertical direction, however, the layer of the mask-adhering layer hangs down due to its own weight in the case of the mask-adhering agent taught in the above Japanese Unexamined Patent Publication (Kokai) No. 282640/1998 spoiling the flatness of the mask.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a pellicle which gives no damage to the mask, which can be mounted on, and removed from, the mask, and which does not lose flatness of the mask even when the mask surface is maintained in either the horizontal direction or the vertical direction.
According to the present invention, there is provided a pellicle comprising a pellicle film, a pellicle frame supporting the pellicle film, and an adhesive resin layer provided on the surface of the pellicle frame on the side opposite to the surface supporting the pellicle film, wherein the adhesive resin layer is formed of a combination of a hard resin layer and a soft resin layer.
In the pellicle of the present invention, it is desired that:
1. The hard resin has a hardness (JIS A) of not smaller than 170 gf and the soft resin has a hardness (JIS A) of not larger than 100 gf; and
2. The soft resin layer is formed maintaining a thickness larger than that of the hard resin layer.
Further, the adhesive resin layer has such a layer structure that the soft resin layer is located on the side of the pellicle frame and the hard resin layer is located on the soft resin layer. With this layer structure, the pellicle is mounted on the mask via the hard resin layer. In this adhesive resin layer, it is desired that the hard resin layer has a thickness which is from 5 to 30% of the thickness of the adhesive resin layer, and the soft resin layer has a thickness which is from 95 to 70% of the thickness of the adhesive resin layer. Further, the soft resin layer can be sandwiched between the two hard resin layers. In this case, the hard resin layer comes in contact with both the pellicle frame and the mask.
Further, the adhesive resin layer can have such a layer structure that both the soft resin layer and the hard resin layer come in contact with the pellicle frame. With this layer structure, both the soft resin layer and the hard resin layer come in contact with the mask that is mounted. In this adhesive resin layer, it is desired that the hard resin layer is disposed on the lower side of the soft resin layer. There can be further employed such a layer structure that the soft resin layer is disposed between the two hard resin layers. It is further desired that the width of contact between the hard resin layer and the mask that is mounted, is from 10 to 30% of the width of contact between the adhesive resin layer and the mask that is mounted.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 to 4 are sectional views illustrating layer structures of the adhesive resin layer in the pellicle of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
In studying a mask mounting a pellicle, the present inventors have discovered the fact that the hardness of the adhesive resin layer for securing the pellicle frame to the mask plays an important role for maintaining the flatness of the mask. It is desired that the adhesive resin layer (hereinafter often called mask-adhering layer) exhibits a suitable adhering force on the interface to the mask.
When, for example, the mask-adhering layer between the mask and the pellicle frame is formed of a hard resin, the mask and the mask-adhering layer are secured together. Here, when the interface is flat between the pellicle frame and the mask-adhering layer (hard resin), the mask maintains flatness. When the interface has a wide area, however, it becomes difficult to maintain the whole interface completely flat; i.e., the mask is distorted tracing the mask-adhering layer (hard resin) and loses flatness. When the mask-adhering layer which is hard is mounted on the mask, a gap is formed between the mask-adhering layer and the mask or the pellicle frame, permitting dust and dirt to enter.
On the other hand, the mask-adhering layer that is formed of a soft resin absorbs the load of the mask and of the pellicle frame imparting such an adhering force that permits peeling from the mask and the pellicle frame. Such a mask-adhering layer (soft resin), however, is subject to be deformed. When the pellicle is maintained in the vertical direction, in particular, the layer of the mask-adhering layer hangs down due to its own weight. If there occurs an interfacial peeling, therefore, the mask-adhering layer deviates down. Besides, if the mask-adhering layer is deformed or deviated downward, undesired stress acts upon the mask, whereby the mask is distorted to spoil the flatness of the mask.
From the above point of view, therefore, the mask-adhering layer according to the present invention is formed of a hard resin layer and a soft resin layer, so that the mask-adhering layer (adhesive resin layer) interposed between the pellicle frame and the mask will not affect the mask even when the mask mounting the pellicle is placed in a horizontal state or in a vertical state.
That is, according to the present invention, the mask needs softly trace the hard resin layer owing to the soft resin layer yet the deformation of the soft resin layer due to its own weight is suppressed by the hard resin layer. In particular, deviation of the pellicle of when it is maintained in the vertical direction is suppressed by the hard resin layer, minimizing the effect of the mask-adhering layer upon the mask, preventing the mask from losing flatness.
Flatness of the mask is expressed by a displacement (μm) of a z-axis perpendicular to an XY-plane of the mask defined by an X-axis and a Y-axis. The value becomes 0 when the mask is completely flat. In general, a range of flatness of the mask that does not impose a problem in practice is about 2 μm in average in a region surrounded by a square pellicle having a side of 5 inches, and is about 5 μm in average in a region surrounded by a square pellicle having a side of 6 inches. Use of the pellicle of the present invention makes it possible to obtain flatness satisfying the above values.
In the present invention, it is desired that the hard resin has a hardness of not smaller than 170 gf and, particularly, in a range of from 200 to 240 gf and that the soft resin has a hardness of not larger than 100 gf and, particularly, in a range of from 40 to 80 gf. The hardness can be measured by using a rubber hardness meter GS-70 (JIA A TYPE). Upon having hardnesses lying within the above-mentioned range, the hard resin layer effectively suppresses the soft resin layer from being deformed while the soft resin layer exhibits a preferred adhering strength, thereby to effectively relax the effect of the hard resin layer upon the mask or the pellicle.
In the pellicle of the present invention, the adhesive resin layer (mask-adhering layer) has a structure as shown in FIGS. 1 to 4 , wherein reference numeral 1 denotes an adhesive resin layer (mask-adhering layer), 2 denotes a mask, 3 denotes a hard resin layer, 4 denotes a pellicle frame and reference numeral 5 denotes a soft resin layer.
In the layer structure of FIG. 1, the hard resin layer 3 in the mask-adhering layer 1 is disposed on the side of the mask 2 , and the soft resin layer 5 in the mask-adhering layer 1 is disposed on the side of the pellicle frame 4 . As will be obvious from FIG. 1, further, the hard resin layer 3 has a small thickness and the soft resin layer 5 has a large thickness.
In the layer structure shown in FIG. 2, the mask-adhering layer 1 includes a soft resin layer 5 and two hard resin layers 3 a , 3 b , the soft resin layer 5 being sandwiched between the two hard resin layers 3 a and 3 b . Further, one ( 3 a ) of the two hard resin layers 3 a , 3 b is in contact with the pellicle frame 4 and the other one ( 3 b ) is in contact with the mask 2 . Like in FIG. 1, further, the hard resin layers 3 a and 3 b have small thicknesses and the soft resin layer 5 has a large thickness.
In the above-mentioned layer structures of FIGS. 1 and 2, it is desired that the surface of the mask 2 is maintained in a horizontal direction.
The layer structures shown in FIGS. 3 and 4 are desired when the surface of the mask 2 (surface of the pellicle film) is maintained in the vertical direction. In these examples, both the hard resin layer 3 ( 3 a , 3 b ) and the soft resin layer 5 are in contact with the pellicle frame 4 and with the mask 2 . In the example of FIG. 3, the mask-adhering layer 1 is formed by one hard resin layer 3 and one soft resin layer 5 . In the example of FIG. 4, the soft resin layer 5 is sandwiched between the two hard resin layers 3 a and 3 b . In these examples, too, the hard resin layer 3 ( 3 a , 3 b ) has a small thickness and the soft resin layer 5 has a large thickness.
In the embodiments of FIGS. 3 and 4, it is desired that a thin layer 3 of a hard resin is provided at least under the thick layer 5 of the soft resin. That is, when the pellicle is maintained in the vertical direction, the hard resin layer 3 is positioned at least under the soft resin layer 5 in order to suppress the deformation or downward deviation of the soft resin layer 5 due to its own weight by utilizing the hard resin layer.
In the present invention, further, it is allowable to change the layer structure of the adhesive resin layer (mask-adhering layer) depending upon the position of the pellicle frame, as a matter of course. When the exposure to light is effected with the mask and pellicle being maintained, for example, in the vertical state, the mask-adhering layer formed on the end surface of a portion of the pellicle frame extending in the horizontal direction may have a layer structure as shown in FIG. 3 or 4 , and the mask-adhering layer formed on the end surface of a portion of the pellicle frame extending in the vertical direction may have a layer structure as shown in FIG. 1 or 2 .
In the pellicle of the present invention, e.g., in the embodiments shown in FIGS. 1 and 2, it is desired that the mask-adhering layer 1 itself has a thickness of usually from about 200 microns (μm) to about 2000 microns (μm) and in which the hard resin layer 3 has a thickness in a range of from 5 to 30% and, particularly, from 5 to 25% and the soft resin layer 5 has a thickness in a range of from 95 to 70% and, particularly, from 95 to 75%.
In the embodiments shown in FIGS. 3 and 4, the width (corresponding to the width of adhesion) for providing the mask-adhering layer 1 is usually from 1200 μm to 5000 μm. It is also allowable to change the ratio of the width (adhering width) of the hard resin layer 3 and the width (adhering width) of the soft resin layer 5 . Here, however, it is desired that the width of the hard resin layer 3 is from 10 to 30% of the whole width (mask-adhering layer 1 ) and the width of the soft resin layer 5 is from 90 to 70% of the whole width.
When the mask surface is maintained in the vertical direction with the pellicle being mounted thereon, the embodiment of FIG. 3 is desired. In this case, the thin layer 3 of the hard resin exhibits an enhanced effect when it is formed on the lower side so as to support the pellicle. In the process of the pellicle, however, it is difficult to form the mask-adhering layer 1 so that the hard resin layer 3 is positioned on the lower side of the soft resin layer 5 in both of the upper side of the frame 5 and the lower side of the frame 5 . Therefore, the thin layer 3 of the hard resin may be provided on the side of a space defined by the pellicle and the mask and on the outside of the thick layer 5 of the soft resin. In this case, it is desired that the thickness of the layer of the hard resin is from 10 to 30% of the whole thickness of the mask-adhering layer, and the layer of the soft resin is from 90 to 70% of the whole thickness of the mask-adhering layer.
When the ratios of the thickness and the width of the hard resin layer become greater than the above-mentioned ranges, the distortion of the mask or of the pellicle frame caused by the hard resin layer is relaxed by the soft resin layer to a decreased extent. As a result, the strength becomes irregular.
Conversely, when the ratios of the thickness and the width of the hard resin layer become smaller than the above-mentioned ranges, the distortion of the soft resin layer due to the weights of the mask and the pellicle is not suppressed to a sufficient degree by the hard resin layer.
(Hard Resin)
Though there is no particular limitation, the hard resin used in the present invention is an adhesive agent such as acrylic, rubber, polybutene or polyurethane, which can be used alone or in a combination of two or more kinds.
It is desired that the hard resin exhibits an adhering force of from 50 to 700 g/cm and, particularly, from 220 to 700 g/cm as measured in compliance with the adhering force testing method stipulated under JIS Z-0237.
(Soft Resin)
Though there is no particular limitation, the soft resin used in the present invention is an adhesive agent such as acrylic, rubber, polybutene or polyurethane, which can be used alone or in a combination of two or more kinds. It is desired that the soft resin exhibits an adhering force of from 100 to 1200 g/cm and, particularly, from 350 to 600 g/cm as measured in compliance with the adhering force testing method stipulated under JIS Z-0237.
The hardnesses and adhering forces of the adhesive agents used as the hard resin and the soft resin for forming the mask-adhering layer, can be adjusted to desired values by adjusting the molecular weights of resins, amounts of functional groups and compositions thereof.
(Formation of the Mask-Adhering Layer)
In the present invention, the mask-adhering layer can be formed by directly applying the soft resin and the hard resin as mask-adhering agents onto the pellicle frame. Referring, for example, to FIGS. 1 and 2, the mask-adhering layer is laminated in parallel with the end surface of the pellicle frame by successively applying the resins. Referring, further, to FIG. 3 and 4, the mask-adhering layer is laminated vertically to the end surface of the pellicle frame by simultaneously or separately applying the resins thereon. The resins can be applied by any known application means, such as spray-application method, brush-application method, roller-coating method, or spread-application method. When the spray-application method is employed, the liquid droplets put on the frame are drawn by using a jig and is evenly applied thereon followed by drying to thereby form the mask-adhering layer.
(Pellicle Frame)
Any widely known pellicle frame can be used. Though not limited thereto only, the pellicle frame may be made of a metal such as aluminum, aluminum alloy or stainless steel, or may be made of a synthetic resin or ceramics.
In the pellicle of the present invention, the weight of the pellicle frame is not larger than 100 g and is, particularly, in a range of from 10 to 30 g from the above-mentioned relationship between the resin layer and the adhering force.
The pellicle of the present invention is such that the pellicle film is stretched on one side of the pellicle frame via the adhesive resin layer, and the adhesive resin layer (mask-adhering layer) comprising the hard resin and the soft resin is provided on the other side so as to be mounted on the mask.
(Pellicle Film)
Any known pellicle film can be used for the pellicle of the present invention. Though not limited thereto only, the pellicle film may be formed of nitrocellulose, cellulose propionate or fluorine-contained material.
EXAMPLES
Examples will now be described. The soft resins and hard resins that are used are hot-melt resins (having melting points of from 180 to 200° C.). Wax, ethylene-vinyl acetate copolymer and resin are adjusted for their compositions, and are used as soft resins and hard resins.
Example 1
A mask-adhering layer was formed on an aluminum frame as shown in FIG. 1 in a manner that the soft resin layer 5 possessed a hardness of from 40 to 100 gf and a thickness of from 75 to 95% and that the hard resin layer 3 possessed a hardness of from 170 to 240 gf and a thickness of from 5 to 25%. There were used two kinds of aluminum frames, the frames of the one kind having a side of 5 inches (outer size of 120×98 and a frame width of 2 mm) and the frames of another kind having a side of 6 inches (outer size of 149×122 and a frame width of 2 mm).
The frame on which the mask-adhering layer was formed as described above was stuck to the mask in a horizontal state with a sticking load of 30 kg for 3 minutes.
The mask in a stuck state was preserved for a month to measure the deformation of the mask-adhering layer and flatness of the mask (Tables 1 and 2).
The frame was then peeled off the mask to measure the peeling property and flatness of the mask after peeling (Tables 1 and 2).
Upon forming the mask-adhering layer on the frame as described above, the flatness of the mask could be maintained after being stuck, and the mask-adhering layer was not deformed. The frame could be easily peeled off since it was mounted on the mask via the hard resin layer, and the flatness could be maintained even after the peeling.
Comparative Example 1
The frame on which the mask-adhering layer was formed under the conditions lying outside the scope of Example 1 was measured in the same manner as in Example 1 [Table 1 (1, 3, 7, 11) and Table 2 (1, 3, 7, 11)]. As a result, problems occurred as shown in Tables 1 and 2.
Example 2
A mask-adhering layer 1 was formed on an aluminum frame to constitute the layer structure as shown in FIG. 1 in a manner that the soft resin layer 5 possessed a hardness of from 40 to 100 gf and a thickness of from 75 to 95% and that the hard resin layers 3 a and 3 b possessed hardnesses of from 170 to 240 gf and thicknesses of from 5 to 25%. There were used two kinds of aluminum frames, the frames of the one kind having a side of 5 inches (outer size of 120×98 and a frame width of 2 mm) and the frames of another kind having a side of 6 inches (outer size of 149×122 and a frame width of 2 mm).
The frame on which the mask-adhering layer was formed as described above was stuck to the mask in a horizontal state with a sticking load of 30 kg for 3 minutes.
The mask in a stuck state was preserved for a month to measure the deformation of the mask-adhering layer and flatness of the mask (Tables 3 and 4). The frame was then peeled off the mask to measure the peeling property and flatness of the mask after peeling (Tables 3 and 4).
Upon forming the mask-adhering layer on the frame as described above, the flatness of the mask could be maintained after being stuck, and the mask-adhering layer was not deformed. The frame could be easily peeled off since it was mounted on the mask via the mask-adhering layer of a combination of the hard resin layer and the soft resin layer, and the flatness could be maintained even after the peeling.
Comparative Example 2
The frame on which the mask-adhering layer was formed under the conditions lying outside the scope of Example 2 was measured in the same manner as in Example 2 [Table 3 (1, 3, 7, 11) and Table 4 (1, 3, 7, 11)]. As a result, problems occurred as shown in Tables 3 and 4.
Example 3
A mask-adhering layer was formed on an aluminum frame to constitute the layer structure as shown in FIG. 3 in a manner that the soft resin layer 5 possessed a hardness of from 40 to 100 gf and a thickness of from 70 to 90% and that the hard resin layer 3 possessed a hardness of from 170 to 240 gf and a thickness of from 10 to 30%.
There were used two kinds of aluminum frames, the frames of the one kind having a side of 5 inches (outer size of 120×98 and a frame width of 2 mm) and the frames of another kind having a side of 6 inches (outer size of 149×122 and a frame width of 2 mm).
The frame on which the mask-adhering layer was formed as described above was stuck to the mask in a vertical state with a sticking load of 30 kg for 3 minutes.
The mask in a stuck state was preserved for a month to measure the deformation of the mask-adhering layer and flatness of the mask (Tables 5 and 6).
The frame was then peeled off the mask to measure the peeling property and flatness of the mask after peeling (Tables 5 and 6).
Upon forming the mask-adhering layer on the frame as described above, the flatness of the mask could be maintained after being stuck, and the mask-adhering layer was not deformed. The frame could be easily peeled off since it was mounted on the mask via the mask-adhering layer of a combination of the hard resin layer and the soft resin layer, and the flatness could be maintained even after the peeling.
Comparative Example 3
The frame on which the mask-adhering layer was formed under the conditions lying outside the scope of Example 3 was measured in the same manner as in Example 3 [Table 5 (1, 3, 7, 11) and Table 6 (1, 3, 7, 11)]. As a result, problems occurred as shown in Tables 5 and 6.
Example 4
A mask-adhering layer was formed on an aluminum frame to constitute the layer structure as shown in FIG. 4 in a manner that the soft resin layer 5 possessed a hardness of from 40 to 100 gf and a thickness of from 70 to 90% and that the hard resin layers 3 a and 3 b possessed hardnesses of from 170 to 240 gf and thicknesses of from 10 to 30%. There were used two kinds of aluminum frames, the frames of the one kind having a side of 5 inches (outer size of 120×98 and a frame width of 2 mm) and the frames of another kind having a side of 6 inches (outer size of 149 ×122 and a frame width of 2 mm).
The frame on which the mask-adhering layer was formed as described above was stuck to the mask in a vertical state with a sticking load of 30 kg for 3 minutes.
The mask in a stuck state was preserved for a month to measure the deformation of the mask-adhering layer and flatness of the mask (Tables 7 and 8). The frame was then peeled off the mask to measure the peeling property and flatness of the mask after peeling (Tables 7 and 8).
Upon forming the mask-adhering layer on the frame as described above, the flatness of the mask could be maintained after being stuck, and the mask-adhering layer was not deformed. The frame could be easily peeled off since it was mounted on the mask via the mask-adhering layer of a combination of the hard resin layer and the soft resin layer, and the flatness could be maintained even after the peeling.
Comparative Example 4
The frame on which the mask-adhering layer was formed under the conditions lying outside the scope of Example 4 was measured in the same manner as in Example 4 [Table 7 (1, 3, 7, 11) and Table 8 (1, 3, 7, 11)]. As a result, problems occurred as shown in Tables 7 and 8.
TABLE 1
(Frame having a side of 5 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
16
60
84
2.2
yes
X
{circle around (2)}
170
14
↓
86
1.2
no
◯
{circle around (3)}
220
31
↓
69
2.4
no
X
{circle around (4)}
↓
23
↓
77
1.4
no
◯
{circle around (5)}
↓
15
↓
85
0.8
no
◯
{circle around (6)}
↓
6
↓
94
1.3
no
◯
{circle around (7)}
↓
3
↓
97
2.3
yes
X
{circle around (8)}
240
16
↓
84
1.5
no
◯
{circle around (9)}
220
15
40
85
1.3
no
◯
{circle around (10)}
↓
↓
100
↓
1.4
no
◯
{circle around (11)}
↓
17
120
83
2.1
no
X
*: Adhesive layer is 500 μm thick
TABLE 2
(Frame having a side of 6 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
15
60
85
4.8
yes
X
{circle around (2)}
170
14
↓
86
4.2
no
◯
{circle around (3)}
220
33
↓
67
6.2
no
X
{circle around (4)}
↓
24
↓
76
4.0
no
◯
{circle around (5)}
↓
14
↓
86
3.2
no
◯
{circle around (6)}
↓
5
↓
95
3.9
no
◯
{circle around (7)}
↓
3
↓
97
5.8
yes
X
{circle around (8)}
240
15
↓
85
3.6
no
◯
{circle around (9)}
220
14
40
86
3.8
no
◯
{circle around (10)}
↓
17
100
83
4.4
no
◯
{circle around (11)}
↓
16
120
84
6.1
no
X
*: Adhesive layer is 500 μm thick
TABLE 3
(Frame having a side of 5 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
14
60
86
1.9
yes
X
{circle around (2)}
170
13
↓
87
0.9
no
◯
{circle around (3)}
220
31
↓
69
2.2
no
X
{circle around (4)}
↓
24
↓
76
1.1
no
◯
{circle around (5)}
↓
17
↓
83
0.6
no
◯
{circle around (6)}
↓
6
↓
94
1.0
no
◯
{circle around (7)}
↓
4
↓
96
2.1
yes
X
{circle around (8)}
240
15
↓
85
1.4
no
◯
{circle around (9)}
220
18
40
82
1.3
no
◯
{circle around (10)}
↓
16
100
84
1.3
no
◯
{circle around (11)}
↓
15
120
85
2.2
no
X
*: Adhesive layer is 500 μm thick
TABLE 4
(Frame having a side of 6 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
14
60
86
5.1
yes
X
{circle around (2)}
170
12
↓
88
4.2
no
◯
{circle around (3)}
220
34
↓
66
6.2
no
X
{circle around (4)}
↓
23
↓
77
4.0
no
◯
{circle around (5)}
↓
15
↓
85
3.2
no
◯
{circle around (6)}
↓
6
↓
94
3.9
no
◯
{circle around (7)}
↓
2
↓
98
5.8
yes
X
{circle around (8)}
240
17
↓
83
3.6
no
◯
{circle around (9)}
220
15
40
85
3.8
no
◯
{circle around (10)}
↓
14
100
86
4.4
no
◯
{circle around (11)}
↓
13
120
87
6.1
no
X
*: Adhesive layer is 500 μm thick
TABLE 5
(Frame having a side of 5 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (Gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
21
60
79
2.1
yes
X
{circle around (2)}
170
20
↓
80
1.2
no
◯
{circle around (3)}
220
43
↓
57
2.6
no
X
{circle around (4)}
↓
29
↓
71
1.3
no
◯
{circle around (5)}
↓
18
↓
72
0.8
no
◯
{circle around (6)}
↓
12
↓
88
1.2
no
◯
{circle around (7)}
↓
4
↓
96
2.7
yes
X
{circle around (8)}
240
20
↓
80
1.4
no
◯
{circle around (9)}
220
22
40
78
1.3
no
◯
{circle around (10)}
↓
21
100
79
1.5
no
◯
{circle around (11)}
↓
19
120
81
2.6
no
X
*: Adhesive layer is 1600 μm wide
TABLE 6
(Frame having a side of 6 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (Gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
18
60
82
4.9
yes
X
{circle around (2)}
170
21
↓
79
4.4
no
◯
{circle around (3)}
220
43
↓
57
6.8
no
X
{circle around (4)}
↓
28
↓
72
4.2
no
◯
{circle around (5)}
↓
21
↓
79
3.5
no
◯
{circle around (6)}
↓
9
↓
91
4.1
no
◯
{circle around (7)}
↓
3
↓
97
5.6
yes
X
{circle around (8)}
240
20
↓
80
4.0
no
◯
{circle around (9)}
220
21
40
79
3.9
no
◯
{circle around (10)}
↓
19
100
81
4.5
no
◯
{circle around (11)}
↓
18
120
82
6.5
no
X
*: Adhesive layer is 1600 μm wide
TABLE 7
(Frame having a side of 5 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (Gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
20
60
80
1.9
yes
X
{circle around (2)}
170
21
↓
79
1.5
no
◯
{circle around (3)}
220
42
↓
58
2.9
no
X
{circle around (4)}
↓
28
↓
72
1.4
no
◯
{circle around (5)}
↓
23
↓
77
0.9
no
◯
{circle around (6)}
↓
12
↓
88
1.6
no
◯
{circle around (7)}
↓
4
↓
96
3.0
yes
X
{circle around (8)}
240
23
↓
77
1.7
no
◯
{circle around (9)}
220
20
40
80
1.5
no
◯
{circle around (10)}
↓
19
100
81
1.6
no
◯
{circle around (11)}
↓
19
120
81
2.9
no
X
*: Adhesive layer is 1600 μm wide
TABLE 8
(Frame having a side of 6 inches.)
Hard adhesive layer
Soft adhesive layer
One month after stuck
Overall
Condition
Hardness (gf)
Thickness (%)
Hardness (Gf)
Thickness (%)
Flatness (μm)
Deformation of adhesive
evaluation
{circle around (1)}
150
19
60
81
5.1
yes
X
{circle around (2)}
170
20
↓
80
4.6
no
◯
{circle around (3)}
220
43
↓
57
7.8
no
X
{circle around (4)}
↓
28
↓
72
4.4
no
◯
{circle around (5)}
↓
20
↓
80
3.7
no
◯
{circle around (6)}
↓
13
↓
87
4.3
no
◯
{circle around (7)}
↓
5
↓
95
6.1
yes
X
{circle around (8)}
240
20
↓
80
4.1
no
◯
{circle around (9)}
220
21
40
79
4.3
no
◯
{circle around (10)}
↓
23
100
77
4.4
no
◯
{circle around (11)}
↓
21
120
79
6.5
no
X
*: Adhesive layer is 1600 μm wide
In the pellicle of the present invention, the mask-adhering layer for mounting the pellicle on the mask is formed of a combination of a hard resin layer and a soft resin layer, the hard resin having a hardness of not smaller than 170 gf and the soft resin having a hardness of not larger than 100 gf. In mounting the pellicle on the mask or in peeling the pellicle off the mask, therefore, the mask is not damaged and the adhesive does not remain on the mask. Besides, the mask maintains flatness even when the surfaces of the mask and of the pellicle film are held not only in the horizontal direction but also in the vertical direction. | A pellicle comprising a pellicle film, a pellicle frame supporting the pellicle film, and an adhesive resin layer provided on the surface of the pellicle frame on the side opposite to the surface supporting the pellicle film, wherein the adhesive resin layer is formed of a combination of a hard resin layer and a soft resin layer. The pellicle can be mounted on the mask and can be removed from the mask without giving damage to the mask, and does not spoil the flatness of the mask irrespective of when the mask surface is maintained in either the horizontal direction or the vertical direction. | 8 |
BACKGROUND OF THE INVENTION
[0001] Many mechanical assemblies such as internal combustion or steam engines and cutting or stamping machines convert a relating motion into a reciprocating motion or a reciprocating motion into a rotating motion. Although cranks and crankshafts are ideal in these large assemblies they become cumbersome and inconvenient when applied to any small hand-held devices especially a mascara applicator. Therefore, there is a need for a compact, lightweight mechanism to achieve the converting a rotating motion into a reciprocating motion for use in small hand-held devices.
FIELD OF THE INVENTION
[0002] The present invention relates to a device tor converting a rotating motion into a reciprocating motion tor use, for example, in a mascara applicator assembly and in an electric toothbrush assembly having such a device. However, the present invention is not limited to minute devices.
SUMMARY OF THE INVENTION
[0003] The present invention proposes a device for converting a rotating motion into a reciprocating motion.
[0004] According to a first aspect of the present invention these is provided a device for converting a rotating motion into a reciprocating motion comprising:
a rotatable shaft carrying a first cylindrical element having a embedded cam groove therein; a second rod element constrained to move back and forth; and a cam follower carried on the second rod element for engagement in the embedded cam groove of the first cylindrical element so that as the rotatable shaft rotates, the cam follower transmits the movement dictated by the embedded cam groove profile thereby causing the second rod element to move back and forth.
[0008] According the second aspect of the present invention there is provided an mascara applicator assembly comprising the said device defined above.
[0009] According the third aspect of the present invention there is provided an first electric toothbrush assembly comprising the said device defined above.
[0010] According the fourth aspect of the present invention there is provided an second electric toothbrush assembly comprising the said device defined above
[0011] An advantage of one or more of the embodiments of the present invention is that the conversion of the rotating motion into a reciprocating motion is in its simplest form. Thereby, the mechanism is simple to construct and may be used in small device such as said above assemblies.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] For the sake of illustration the preferred features of the invention will now be described with reference to the following figures in which:
[0013] FIG. 1 is a cross-sectional view of the mascara applicator assembly including a reciprocating drive mechanism according to an embodiment of the invention.
[0014] FIG. 2 is a cross-sectional view of the mascara applicator assembly including a reciprocating drive mechanism according to an embodiment of the invention showing a different battery type.
[0015] FIG. 3 is a cross-sectional view of the mascara applicator assembly including a reciprocating drive mechanism according to an embodiment of the invention showing a tube to constrain a second rod element.
[0016] FIG. 4 is a first progressive view of a reciprocating drive mechanism of the mascara applicator assembly in operation.
[0017] FIG. 5 is a second progressive view of a reciprocating drive mechanism of the mascara applicator assembly in operation.
[0018] FIG. 6 is a third progressive view of a reciprocating drive mechanism of the mascara applicator assembly in operation.
[0019] FIG. 7 is a fourth progressive view of a reciprocating drive mechanism of a mascara applicator assembly in operation.
[0020] FIG. 8 is a fifth progressive view of a reciprocating drive mechanism of a mascara applicator assembly in operation.
[0021] FIG 9 is a partial cross-sectional top view of the electric toothbrush assembly including a reciprocating drive mechanism according to an embodiment of the invention.
[0022] FIG. 10 is a first progressive view of a reciprocating drive mechanism of the electric toothbrush assembly in operation.
[0023] FIG. 11 is a second progressive view of a reciprocating drive mechanism of the electric toothbrush assembly in operation.
[0024] FIG. 12 is a third progressive view of a reciprocating drive mechanism of the electric toothbrush assembly in operation.
[0025] FIG. 13 is a fourth progressive view of a reciprocating drive mechanism of the electric toothbrush assembly in operation.
[0026] FIG. 14 is a fifth progressive view of a reciprocating drive mechanism of the electric toothbrush assembly in operation.
[0027] FIG. 15 is a upper partial cross-sectional top view of the electric toothbrush assembly.
[0028] FIG. 16 is a upper partial cross-sectional right side view of the electric toothbrush assembly.
[0029] FIG. 17 is a upper partial cross-sectional left side view of the electric toothbrush assembly.
[0030] FIG. 18 is a top view of the upper electric toothbrush assembly.
[0031] FIG. 19 is a top partial cross-sectional view of the upper electric toothbrush assembly.
[0032] FIG. 20 is a cross-sectional top view of the electric toothbrush assembly having a detachable head where said detachable head is detached and further includes a reciprocating drive mechanism according to an embodiment of the invention.
[0033] FIG. 21 is a cross-sectional top view of the electric toothbrush assembly having a detachable head where said detachable bead is attached and further includes a reciprocating drive mechanism according to an embodiment of the invention.
[0034] FIG. 22 is a first progressive view of the reciprocating drive mechanism of the electric toothbrush assembly having a detachable head in operation.
[0035] FIG 23 is a second progressive view of a reciprocating drive mechanism of the electric toothbrush assembly having a detachable head in operation.
[0036] FIG. 24 is a third progressive view of a reciprocating drive mechanics of the electric toothbrush assembly having a detachable bead in operation.
[0037] FIG. 25 is a fourth progressive view of a reciprocating drive mechanism of the electric toothbrush assembly having a detachable head in operation.
[0038] FIG. 26 is a fifth progressive view of a reciprocating drive mechanism of the electric toothbrush assembly having a detachable head in operation.
[0039] FIG. 27 is an upper partial cross-sectional top view of the electric toothbrush having a detachable head assembly.
[0040] FIG. 28 is an upper partial cross-sectional right side view of the electric toothbrush having a detachable head assembly.
[0041] FIG. 29 is an upper partial cross-sectional left side view of the electric toothbrush having a detachable head assembly.
[0042] FIG. 30 is a top view of the upper electric toothbrush having a detachable head assembly.
[0043] FIG. 31 is a top partial cross-sectional view of the upper electric toothbrush having a detachable bead assembly.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0044] FIG. 1 shows an electric mascara applicator assembly 1 which comprises a motor 2 encased in a motor housing 3 . Motor housing 3 is embedded in housing 4 . The motor 2 includes motor shaft 5 on which cylindrical wheel 6 is attached. The cylindrical wheel 6 has a embedded cam groove track 7 in which a cam follower pin 8 is loosely seated, as shown in FIG. 4 . The cam follower pin 8 is attached to a reciprocating push-pull rod 9 , as shown in FIG. 4 . Brush bead 10 , as shown in FIG. 1 , is attached to the other end of reciprocating push-pull rod 9 . A cordon of the reciprocating push-pull rob 9 is constrained by a portion of housing 4 thereby constraining the movement of the entire reciprocating push-pull rod 9 . A flat circular stop limiter 11 is attached to the reciprocating push-pull rod 9 . The bellows expansion seal seat 12 is attached to the outer bottom housing 13 . The bellows expansion seal seat 14 is attached to the reciprocating push-pull rod 9 . The bellows expansion seal 15 is seated in bellows expansion seal seat 12 and bellows expansion seal seat 14 . Air vent 16 is embedded in housing 4 , as shown in FIG. 1 .
[0045] The reciprocating push-pull rod 9 may be constrained by a tube 17 retained within the housing 4 , as shown in FIG. 3 . At the other end of the motor shaft 5 to that carrying the cylindrical wheel 6 , an optional weight 18 , as shown in FIG. 2 , may be attached. As shown in FIG. 1 , batteries 19 rest within battery compartment 20 which is embedded in housing 4 . Removable negative battery contact 21 is held firmly in place by end cap 22 . As shown in FIG. 2 , batteries 23 rest within battery compartment 24 which is embedded in housing 4 . Removable positive and negative battery contact 25 is held firmly in place by end cap 22 . Mascara applicator assembly 1 further composes detachable cosmetic tank 26 which is designed to distribute mascara evenly upon brush 10 when brush 10 is removed from cosmetic tank 26 by brush 10 heavy pulled through trimmer 27 .
[0046] The motor 2 is driven by one or more batteries 19 , as shown in FIG. 1 or another type of primary batteries 23 , as shown in FIG. 2 . The motor 2 is driven by one or more batteries 19 , as shown in FIG. 1 or another type of primary batteries 23 , as shown in FIG. 2 . Motor 2 may be powered by a battery pack, which may be of the lithium-ion type for ready charging via a secondary voltage cod and an integral male socket portion within housing 4 , not shown. Said male socket portion is detachably received in a corresponding female socket portion provided in a charger base assembly having a primary charging coil, also not shown. The electrical circuit would be defined with one side of the secondary coil attached to a negative battery terminal connector and the other side of the secondary coil coupled through a diode to the positive battery terminal. The diode rectifies voltage out-puts from the coil, also no shown. Other prior art charging circuitry may be used. Motor 2 is controlled by an on-off switch 28 .
[0047] In operation, the user starts the motor 2 by moving the on-off switch 28 to the on position. As the cylindrical wheel 6 that is mounted on motor shaft 5 is rotated by the motor 2 , the cam follower pin 8 follows the groove of the embedded cam groove track 7 to produce the desired back and forth motion of the reciprocating push-pull rod 9 . The shape of the embedded cam groove track 7 defines the distance that the reciprocating push-pull rod 9 and the attached brush head 10 move back and forth. As the reciprocating push-pull rod 9 moves forth the bellows expansion seal 15 expands, as shown in FIG. 1 , and as the reciprocating push-pull rod 9 moves back the bellows expansion seal 15 contracts, as shown in FIG. 2 The bellows expansion seal 15 maintains the seal of the opening between the reciprocating push-pull rod 9 and the opening of that portion of housing 4 that constrains the reciprocating push-pull nod 9 . Air vent 16 provides a means for air to flow freely during the expansion and contraction of the bellows expansion seal 15 .
[0048] A partial progressive sequence of events illustrating one complete cycle of the reciprocating drive mechanism for a electric mascara applicator assembly 1 of the type shown in FIG. 1 is shown in FIGS. 4 , 5 , 6 , 7 and 8 . In FIGS. 4 , 5 , 6 , 7 and 8 motor 2 is rotating motor shaft 5 counterclockwise. In FIG. 4 the embedded cam groove track 7 is at its closest point to casing surface of motor 2 . As the motor shaft 5 rotates counterclockwise the cam follower pin 8 follows the groove of the embedded cam groove track 7 and causes the reciprocating push-pull rod 9 and brush head 10 to move forth, as shown in FIG. 5 until it reaches the furthest forward plotted distance of the reciprocating push-poll rod 9 , as shown in FIG. 6 . As the motor shaft 5 continues to rotate the direction of the reciprocating push-pull rod 9 is changed to the opposite or back direction, as shown in FIG. 7 , until it reaches that point where once again the embedded cam groove track 7 is at its closest point to casing surface of motor 2 , as shown in FIG. 8 . This cycle is continually repeated until t he on-off switch 28 is moved by the user to the off position. The short back and forth movement of brush head 10 aids the uses in the application of mascara to the desired eyelash, not shown. Optional weight 18 , as shown in FIG. 2 . produces an off-centered rotation when motor shaft 5 rotates causing a vibration to occur that in some instance may aid the user in the application of mascara.
[0049] FIG. 9 shows an first electric toothbrush assembly 30 which comprises a mobs 31 encased in a motor housing 32 . Motor housing 32 is embedded in housing 33 . The motor 31 includes motor shaft 34 or which cylindrical wheel 35 is attached. The cylindrical wheel 35 has an embedded cam groove track 36 in which a cam follower pin 37 is loosely seated, as shown in FIG. 10 . The cam follower pin 37 is attached to a reciprocating push-pull rod 38 , as shown in FIG. 10 . A portion of the reciprocating push-pull rod 38 is constrained by a portion of housing 33 thereby constraining the movement of the entire reciprocating push-pull rod 38 , as shown in FIG. 9 . A flat circular stop limiter 39 is attached to the reciprocating push-pull rod 38 . Guide cod 40 is attached at the other end of reciprocating push-pull rod 38 to that to which the cam follower pin 37 is attached, as shown m FIG. 15 . Guide rod 40 comprises a geared shaft 41 which simultaneously engages first semi gear wheel 42 and second semi gear wheel 43 . First semi gear wheel 42 and second semi gear wheel 43 is attached to first shaft 44 and second shaft 45 respectively, as shown in FIG. 15 . Shaft 44 extends in opposite directions from its attachment to first semi gear wheel 42 , as shown in FIG. 16 . First rotating anchor end 46 of shaft 44 test in extended housing base 47 . Opposite end 48 of shad 44 passes through the second shaft housing 73 of housing 33 , brush plate seal 49 and is attached to first semi brush plate 50 . First semi brush plate 50 is directly attached to first semi brush head 51 . Shaft 45 extends in opposite directions from its attachment to Second semi gear wheel 43 , as shown in FIG. 17 . The second rotating anchor end 52 , of shaft 45 , rest in extended housing base 53 , as shown in FIG, 17 . Opposite end 54 of shaft 45 passes through the first shaft housing 72 of housing 33 , brush plate seal 49 and is attached to second send brash plate 55 . Second send brush plate 55 is directly attached to second semi brush head 56 .
[0050] Guide rod 40 further comprises a second posh-pub rod 77 . Second posh-pull rod 77 is attached to the first free end of geared shaft 41 . Second push-pull rod 77 comprises a vertical passage housing 57 , as shown in FIG. 15 . In FIG. 17 vertical passage housing 57 is shown receiving one end of male guide rod 58 and is secured by first retaining end 59 and second retaining end 60 respectively while the opposite end 61 of male guide rod 58 passes through shaft housing 74 of housing 33 , bellows expansion seal 62 and is attached to brush plate 63 . Brush plate 63 is directly attached to brush bead 64 . Second push-pull rod 77 further comprises genie rod end 65 . Guide rod end 65 , as shown in FIG. 15 rest within guide rod end housing 66 which includes internal air vent 67 and internal, air vent 68 respectively, as shoo a in FIG. 15 .
[0051] An first electric toothbrush assembly 36 further comprises upper outer shell 69 , as shown in FIG. 18 . Upper outer shell 69 provides and first embedded platform 70 and second embedded platform 71 . First embedded platform 76 is shaped well enough to allow brush plate seal 49 , not shown, to snugly rest within its boundaries while establishing a border for first semi brush bead 51 and 56 , not shown. First embedded platform 70 further comprises first shaft housing 72 and second shaft housing 73 . Second embedded platform 71 in the shape of a rectangle is allows the bellows expansion seal 62 , not shown, to snugly rest within its boundaries while establishing a border for brush head 64 , not shown. Second embedded platform 71 further comprises a shaft housing 74 designed to permit male guide rod 58 to move about freely. In FIG. 19 the directional arrows depict, the movement of the reciprocating push-pull rod 38 , first semi brush head 51 , second semi brush head 56 and brush head 64 when in operation.
[0052] The motor 31 is driven by one or more batteries 75 , as shown in FIG. 9 . Motor 31 may be powered by a battery pack, which may be of the lithium-ion type for ready charging via a secondary voltage coil and an integral male socket portion within housing 33 , not shown. Said male socket portion is detachably received in a corresponding female socket portion provided in a charger base assembly having a primary charging coil, also not shown. The electrical circuit would be defined with one side of the secondary coil attached to a negative battery terminal connector and the other side of the secondary coil coupled through a diode to the positive battery terminal. The diode rectifies voltage outputs from the coil, also not shown. Other prior art charging circuitry may be used. First electric toothbrush assembly 30 further comprises an end cap 78 , as shown in FIG. 9 . End cap 78 enables easy replacement of one or more batteries 75 . Motor 31 is controlled by an on-off switch 76 .
[0053] In operation, the riser starts the motor 31 by moving the on-off switch 76 to the on position. As the cylindrical wheel 35 that is monitored on motor shaft 34 is rotated by the motor 31 , the cam follower pin 37 follows the groove of the embedded cam groove track 36 to produce the desired back and forth motion of the reciprocating push-pull rod 38 . The shape of the embedded cam groove track 36 defines the distance that the reciprocating push-pull rod 38 and the attached guide rod 40 move back and forth.
[0054] A partial progressive sequence of events illustrating one complete cycle of the reciprocating drive mechanism for a electric toothbrush assembly 30 of the type shows in FIG. 9 is shown so FIGS. 10 , 11 , 12 , 13 and 14 . In FIGS, 10 , 11 , 12 , 13 and 14 motor 31 is rotating motor shaft 34 counterclockwise. In FIG. 10 the embedded cam groove track 36 is at its closest point to casing surface of motor 31 . As the motor shaft 34 rotates counterclockwise the earn follower pin 37 follows the groove of the embedded cam groove track 36 and causes the reciprocating push-pull rod 38 and the attached guide rod 40 to move forth, as shown in FIG. 11 until it reaches the furthest forward plotted distance of the reciprocating push-pull rod 38 and the attached guide rod 40 , as shown in FIG. 12 . As the motor shaft 34 continues to rotate the direction of the reciprocating push-pull rod 38 and the attached guide rod 40 is changed to the opposite or back direction, as shown in FIG. 13 , until it reaches that point where once again the embedded cam groove track 36 is at its closest point to casing surface of motor 31 , as shown in FIG. 14 . This cycle is continually repeated until the on-off switch 76 is moved by the user to the off position. The short back and forth movement of guide rod 40 engages first semi gear wheel 42 and 43 causing the movement of the first semi brush head 51 , second semi brush head 56 in the direction shown in FIG. 19 while simultaneously pushing and pulling male guide rod 58 which ultimately moves brush head 64 in the direction shown in FIG. 19 .
[0055] In FIG. 20 the second electric toothbrush assembly 80 comprises housing 81 . Housing 81 comprises handle portion 82 . Handle portion 82 comprises motor 83 encased in a motor housing 84 . Motor housing 84 is embedded in housing 85 . The motor 83 includes motor shaft 86 on which cylindrical wheel 87 is attached. The cylindrical wheel 87 has an embedded cam groove track 88 in which a cam follower pin 89 is loosely seated, as shown in FIG. 22 The cam follower pin 89 is attached to a reciprocating push-pull rod 90 , as shown in FIG. 22 . A portion of the reciprocating push-pull rod 90 is constrained by a portion of housing 85 thereby constraining the movement of the entire reciprocating push-pull rod 90 , as shown in FIG. 20 . A flat circular stop limiter 91 is attached to the reciprocating push-pull rod 90 . Tapered male end 92 is attached at the other end of reciprocating push-pull rod 90 to that to which the cam follower pin 89 is attached, as shown in FIG. 20 .
[0056] Housing 81 further comprises a detachable brush head 93 , as shown in FIGS. 20 , 21 and 27 . Detachable brush head 93 comprises rod 94 having female end 95 , as shown in FIG. 27 . At female end 95 of rod 94 is attached rod limber 96 . Rod limiter 96 and a portion of rod 94 are constrained by housing 97 thereby constraining the entire rod 94 . Guide rod 98 is attached at the other end of rod 94 to that to which the female end 95 is attached, as shown in FIG. 27 . Guide rod 98 comprises a geared shaft 99 which simultaneously engages first semi gear wheel 100 and second semi gearwheel 101 . First semi gear wheel 100 and 101 is attached to first shaft 102 and second shaft 103 respectively, as shown in FIG. 27 . First shaft 102 extends in opposite directions from its attachment to first semi gear wheel 100 , as shown in FIG. 28 . First rotating anchor end 104 of first shaft 102 rest in extended housing base 105 . Opposite end 100 of first shaft 102 passes through the second shaft housing 133 of housing 97 , brush plate seat 107 and is attached to first semi brush plate 108 . First semi brush plate 108 is directly attached to first semi brush head 109 . Second shaft 103 extends in opposite directions from its attachment to Second semi gear wheel 101 , as shown in FIG. 29 . The second rotating anchor end 110 , of second shaft 103 , rests in extended housing base 111 , as shown in FIG. 29 . Opposite end 112 of second shaft 103 passes through the first shaft housing 132 of housing 97 , brush plate seal 107 and is attached to second semi brush plate 113 . Second semi brush plate 113 is directly attached to second semi brush head 114 . Guide rod 98 further comprises a second push-pull rod 141 . Second push-pull rod 141 is attached to the last free end of geared shaft 99 . Second push-pull rod 41 comprises a vertical passage housing 115 , as shown in FIG. 27 . In FIG. 29 vertical passage housing 115 is shown receiving one end of male guide rod 116 and is secured by first retaining end 117 and second retaining end 118 respectively while the opposite end 119 of male guide rod 119 passes through shaft housing 134 of housing 97 , bellows expansion seal 120 and is attached to brush plate 121 . Brush plate 121 is directly attached to brush bead 122 . Second push-pull rod 141 further comprises guide rod end 123 . Guide rod end 123 , as shown in FIG. 27 rest within guide rod end housing 124 which includes internal air vent 125 and internal air vent 126 respectively, as shown in FIG. 27 . Guide rod end 123 is in continual contact with one side of movable plate 127 at all times due to the pressure exerted by spring 128 on the opposite side of movable plate 127 . Movable plate is retained within guide reel end housing 124 , as shown in FIG. 27 .
[0057] A detachable brush head 95 further comprises upper carter shell 129 , as shown in FIG. 30 . Upper outer shell 129 provides and first embedded platform 130 and second embedded platform 131 first embedded platform 130 is shaped well enough to allow brush plate seal 107 , not shown, to snugly rest within its boundaries while establishing a border for first semi brush head 169 and see end send brush head 114 , not shown. First embedded platform 130 further comprises first shaft housing 132 and second shaft housing 133 . Second embedded platform 131 in the shape of a rectangle is allows the bellows expansion seal 120 , not shown, to snugly rest within its boundaries while establishing a border for brush head 122 , not shown. Second embedded platform 131 further comprises a shaft housing 134 designed to permit male guide rod 116 to move about freely. In FIG. 31 the directional arrows depict the movement of the reciprocating push-pull rod 90 , rod 94 , first semi brush head 109 , second semi brush head 114 and brush head 122 when in operation. The detachable brush head 93 is held in place by retaining clip end 135 and 136 are engaged with retaining clip anchor 137 and 138 respectively as shown in FIGS. 21 and 31 .
[0058] The motor 83 is driven by one or more batteries 139 , as shown in FIG. 20 . Motor 83 may be powered by a battery pack, which may he of the lithium-ion type for ready charging via a secondary voltage coil and an integral male socket portion within housing 35 , not shown. Said male socket portion is detachably received in a corresponding female socket portion provided in a charger base assembly having a primary charging coil, also not shown. The electrical circuit would be defined with one side of the secondary coil attached to a negative battery terminal connector and the other side of the secondary coil coupled through a diode to the positive battery terminal. The diode rectifies voltage outputs from the coil, also not shown. Other prior art charging circuitry may be used. Second electric toothbrush assembly 80 further comprises an end cap 142 , as shown in FIG. 21 . End cap 142 enables easy replacement of one or more batteries 139 . Motor 83 is controlled by an on-off switch 140 .
[0059] In operation, the user starts the motor 83 by moving the on-off switch 140 to the on position. As the cylindrical wheel 37 that is mounted on motor shaft 86 is rotated by the motor 83 , the cam follower pin 89 follows the groove of the embedded cam groove track 83 to produce the desired back and forth motion of the reciprocating push-pull rod 90 . The shape of the embedded cam groove track 88 defines the distance that the reciprocating push-pull rod 90 moves back and forth. The tapered male oval 92 of reciprocating push-pull rod 40 is firmly pressed against female end 95 of rod 94 and as the reciprocating push-pull rod 90 moves back and forth so does rod 94 and the attached guide rod 98 . Guide rod end 123 pushes movable plate 127 forth compressing spring 128 . Compressed spring 128 continually pushes movable plate 127 against guide rod end 123 and eliminates any backlash.
[0060] A partial progressive sequence of events illustrating one complete cycle of the reciprocating drive mechanism for a second electric toothbrush assembly 80 of the type shown in FIG. 20 is shown in FIGS. 22 , 23 , 24 , 25 and 26 . In FIGS. 22 , 23 , 24 , 25 and 26 motor 83 is rotating motor shaft 86 counterclockwise. In FIG. 22 the embedded cam groove track 88 is at its closest point to casing surface of motor 83 . As the motor shaft 86 rotates counterclockwise the cam follower pin 89 follows the groove of the embedded cam groove track 88 and causes the reciprocating push-pull rod 90 and the attached guide rod 98 to move forth, as shown in FIG. 23 until it reaches the furthest forward plotted distance of the reciprocating push-pull rod 90 and the attached guide rod 98 , as shown in FIG. 24 As the motor shaft 86 continues to rotate the direction of the reciprocating push-poll rod 90 and the attached guide rod 98 is changed to the opposite or back direction, as shown in FIG. 25 , until it reaches that point where once again the embedded cam groove track 88 is at its closest point to casing surface of motor 83 , as shown in FIG. 26 . This cycle is continually repeated until the on-off switch 140 is moved by the user to the off position. The short back and forth movement of guide rod 98 engages first semi gear wheel 100 and 101 causing the movement of the first semi brush head 109 , second semi brush head 114 in the direction shown in FIG. 31 while simultaneously pushing and pulling male guide rod 110 which ultimately moves brush head 122 in the direction shown in FIG. 31 .
[0061] While the present invention has been described and illustrated above in the content of an electric mascara applicator assembly and a reciprocating drive mechanism: and in the contest of an first electric toothbrush assembly and a reciprocating drive mechanism, and in the contest of an second electric toothbrush assembly and a reciprocating drive mechanism it is not to be considered limited to either of these assemblies. It is to be understood that other embodiments maybe used or modifications and additions may be made to the described embodiments for performing the same function of the present invention without deviating therefrom. Therefore, the present invention should be construed in breadth and scope in accordance with the recitation of the appended claims.
Mascara Applicator Assembly Numbering Chart
[0000]
mascara applicator assembly 1
motor 2
motor housing 3
housing 4
motor shaft 5
cylindrical wheel 6
embedded cam groove track 7
cam follower pin 8
reciprocating push-pull rod 9
Brush head 10
circular stop limiter 11
bellows expansion seal seat 12
outer bottom housing 13
bellows expansion seal seat 14
bellows expansion seal 15
Air vent 16
tube 17
optional weight 18
Batteries 19
battery compartment 20
Removable negative battery contact 21
end cap 22
Batteries 23
battery compartment 24
Removable positive and negative battery contact 25
cosmetic tank 26
trimmer 27
on-off switch 26
First Electric Toothbrush Assembly Numering Chart
[0000]
first electric toothbrush assembly 30
motor 31
motor housing 32
housing 33
motor shaft 34
cylindrical wheel 35
embedded cam groove track 36
cam follower pin 37
reciprocating push-pull rod 38
flat circular stop limiter 39
Guide rod 40
geared shaft 41
first semi gear wheel 42
second semi gear wheel 43
first shaft 44 and second shaft 45
First rotating anchor end 46
extended housing base 47
Opposite end 48
brush plate seal 49
first semi brush plate 50
first semi brush head 51
Second rotating anchor end 52
extended housing base 53
Opposite end 54
second semi brush plate 55
second semi brush head 56
vertical passage housing 57
male guide rod 58
first retaining cam 59 second retaining end 60
opposite end 61
bellows expansion seal 62
brush plate 63
brush head 64
Guide rod end 65
guide rod end housing 66
internal air vent 67 and internal air vent 63
upper outer shell 67
first embedded platform 70 and second embedded platform 71
first shaft housing 72 and second shaft housing 73
shaft housing 74
batteries 75
on-off switch 76
second push-pull rod 77
end cap 78
Second Electric Toothbrush Assembly Numbering Chart
[0000]
second electric toothbrush assembly 80
housing 81
comprises handle portion 82
motor 83
motor housing 84
housing 85
motor shaft 86
cylindrical wheel 87
embedded cam groove track 88
cam follower pin 89
reciprocating push-pull rod 90
flat circular stop limiter 91
tapered male end 92
detachable brush head 93
rod 94
female end 95
rod limiter 96
housing 97
Guide rod 98
geared shaft 99
first semi gear wheel 100
second semi gear wheel 101
first shaft 102 and second shaft 103
First rotating anchor end 104
extended housing base 105
Opposite end 106
brush plate seal 107
first semi brush plate 108
first semi brush head 109
Second rotating anchor end 110
extended housing base 111
Opposite end 112
Second semi brush plate 113
second semi brush head 114
vertical passage housing 115
male guide rod 116
first retaining end 117 and second retaining end 118
Opposite end 119
bellows expansion seal 120
brush plate 121
brush head 122
Guide rod end 123
guide rod end housing 124
internal air vent 123 and internal air vent 126
movable plate 127
spring 128
upper outer shell 129
first embedded platform 130 and second embedded platform 131
first shaft housing 132 and second shaft housing 133
shaft housing 134
retaining clip end 135 and 136
retaining clip anchor 137 and 138
batteries 139
on-off switch 140
second push-pull rod 141
end cap 142 | A device for converting a rotating mod on into a reciprocating notion comprises a rotatable shaft carrying a first cylindrical element, an embedded cam groove of the first cylindrical element, a second rod element constrained to move back and forth and forth, and a cam follower carried on the second rod element. The cam follower may be engaged in the embedded cam groove of the first cylindrical element so that as the rotatable shaft rotates, the cam follower transmits the movement dictated by the embedded cam groove profile thereby causing the second rod element to move back and forth transmits power. There is also disclosed an mascara applicator assembly; an first electric toothbrush assembly comprising such a device, and an second electric toothbrush assembly comprising such a device. | 8 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to a method of manufacturing high performance semiconductor devices utilizing selective electroless plating processing and more specifically, this invention relates to a method of manufacturing high performance semiconductor devices utilizing a method of defining copper seed layers for selective electroless plating processing.
2. Discussion of the Related Art
As the performance of semiconductor devices have progressed to higher speeds, the use of aluminum as an interconnect material is causing a speed bottleneck Alternate materials such as gold (Au), silver (Ag), nickel (Ni), palladium (Pd), copper (Cu), and platinum (Pt) have all been explored. Of these, copper has become the preferred alternate replacement due to its low resistance and low cost. However, unlike aluminum, copper is not easily etched into wires or via plugs. An alternative method for manufacturing integrated circuits using multilevel copper interconnects has been developed that utilizes single damascene mask methodology.
As the price of semiconductor devices continues to decrease, there is pressure on the semiconductor manufacturing industry to minimize total cost. One of the major requirements to minimize total cost is to minimize the number of process steps. One method to minimize the number of processing steps is to combine the filling of conductive layers of metallization, for example, into both a trench and a via in a single step. Because current and future devices may have five or more layers of metallization (wire and via equal to one layer), combining the two will have a significant impact upon the total cost of the semiconductor device. Furthermore, the use of copper reduces contact resistance since this will eliminate every other barrier, glue, and seal layers between the current layer's via and wire, as shown in FIG. 1 .
FIG. 1 shows a semiconductor device 100 in which vias and wire interconnects have been formed by standard damascene methods. The semiconductor device 100 includes a layer 102 that could be a semiconductor substrate on and in which active devices (not shown) have been formed. The next layer 104 is a layer of interlayer dielectric in which metal structures, such as a wire 106 is formed. As is known in the semiconductor manufacturing art, a wire is used to connect one portion of a semiconductor device to another portion of the semiconductor device on the same layer. The wire 106 is typically formed in a trench formed in the layer of interlayer dielectric 104 . The walls of the trench are covered with a barrier layer 108 . The barrier layer 108 is typically formed from a metallic nitride material such as TiN or TaN. The trench is then filled with a conductive material. Conductive materials that can be used to fill the trench include tungsten, aluminum and copper. If copper is to be the conductive material to fill the trench, a seed layer 109 is formed on the barrier layer 108 . The seed layer is typically a thin layer of copper that may be sputtered onto the barrier layer 108 . A seal layer or hard mask layer 110 is formed on the surface of the layer 104 of interlayer dielectric. The layer 110 is a seal layer if the conductive material is to be copper. A seal layer prevents copper ions from diffusing into the surrounding material. A typical seal layer is made up of a material such as Si z N y or SiO z N y . A layer 112 of interlayer dielectric is formed on the layer 110 and metal structures such as via 114 are formed in the layer 112 of interlayer dielectric. The walls of via 114 are covered with a barrier layer 116 similar to barrier layer 108 . If via 114 is to be filled with copper, a seed layer 117 is formed on the barrier layer 116 . Via 114 is then filled with a conductive material. A seal layer or hard mask layer 118 is formed on the surface of the layer 112 of interlayer dielectric. The layer 118 is a seal layer if the via 114 is to be filled with copper. A layer 120 of interlayer dielectric is formed on the layer 118 . Trenches shown at 122 and 124 are formed in the layer 120 of interlayer dielectric. Barrier layers 126 and 128 are formed on the walls of the trenches 122 and 124 respectively and the trenches 122 and 124 are filled with conductive material. If the trenches 122 and 124 are to be filled with copper, seed layers 123 and 125 are formed on the barrier layers 126 and 128 . As is known in the semiconductor manufacturing art, trenches and vias are etched into a layer of interlayer dielectric material and a blanket layer of conductive material is then typically formed on the surface of the wafer and a polishing process, such as a chemical mechanical polishing process, is conducted to remove unwanted conductive material. As can be appreciated, the above process of forming individual-metal structures requires numerous steps.
FIGS. 2A-2C show a method of eliminating several steps from the process of forming a semiconductor device as described above in conjunction with FIG. 1 . Like numerical designations denote like structures in the figures. FIG. 2A shows a partially completed semiconductor device 200 . The partially completed semiconductor device 200 shows layer 102 with metal structure 106 formed in layer 104 of interlayer dielectric. The metal structure 106 is formed by forming a via or trench in the layer 104 , forming a barrier layer 108 on the walls of the via or trench in the layer 104 , and forming a seed layer 109 on the barrier layer 108 if the via or trench in the layer 104 is to be filled with copper. The seal layer or hard mask layer 110 , the layer 112 of interlayer dielectric, the seal layer or hardmask layer 118 and the layer 120 of interlayer dielectric are formed on the layer 104 . The layer 110 is a seal layer if the subsequently formed vias and trenches are to be filled with copper. A series of masking and etching processes are then conducted to form vias, such as the via 114 and trenches, such as the trenches 122 and 124 , in the layers 104 , 110 , 112 , 118 , and 120 . A barrier layer 202 is formed on the walls of the vias and trenches. A seed layer 204 of copper is formed on the barrier layer 202 if via 114 and trenches 122 and 124 are to be filled with copper. There are several methods to deposit copper, however, only two of the methods can successfully form copper into the small geometries required for modern semiconductor technology. These two methods are chemical vapor deposition (CVD) and electroplating. Of the two, CVD is too expensive because of the gases used to supply the copper ions. Electroplating is the preferred method because electroplating can be done in batches, unlike a CVD process, which can only be done on one wafer at a time. When an electroplating process is utilized, the seed layer 204 of copper is formed on the barrier layer 202 . In this instance, a global deposition or sputtering of the conductive seed layer 204 is formed on the entire surface of the wafer. If the conductive material to be used is copper, the seed layer formation process consists of depositing or sputtering a thin layer of copper onto the entire wafer, which includes the sidewalls and bottom of the trenches and vias that have been formed in the semiconductor device 200 . The entire wafer is then submerged into a bath of ionic solution containing copper ions and an electroplating process causes a layer 206 of copper to be formed on the surface of the wafer. It is noted that the thickness of the layer 206 must be thick enough so that via 114 and trench 122 can be completely filled. Because some materials such as copper are difficult to polish, the process of planarizing the copper layer 206 is very difficult.
FIG. 2B shows the partially completed semiconductor device 200 as shown in FIG. 2A after a polishing process to remove undesired portions of the layer 206 of copper and of the seed layer 204 . However, as known in the semiconductor manufacturing art, the polishing of copper is a difficult process and it is therefore desirable to keep the thickness of the layer 206 of copper to a minimum.
FIG. 2C shows the partially completed semiconductor device 200 as shown in FIG. 2B after a polishing process to remove undesired portions of the barrier layer 202 from the top surfaces of the partially completed semiconductor device 200 . As can be appreciated, the via 114 and trench 122 are filled with a conductive material during the same process thus saving one or more process steps when compared to the process necessary to form the structure as shown in FIG. 1 . As will be noted, the semiconductor device 100 in FIG. 1 is the same as the semiconductor device 200 shown in the FIGS. 2A-2C.
The semiconductor device shown in FIG. 1 requires multiple steps to form the individual metal structures using the damascene method of forming metal filled vias and trenches. The semiconductor device shown in FIGS. 2A-2C requires extensive chemical mechanical polishing to remove excess copper that has been electroplated on the entire surface of the partially completed semiconductor device.
Therefore, what is needed is a method of manufacturing semiconductor devices that form multiple layers of metal filled vias and trenches in the minimum number of processes and that does not require extensive polishing processes.
SUMMARY OF THE INVENTION
According to the present invention, the foregoing and other objects and advantages are attained by a method of manufacturing a semiconductor device that utilizes an electroless plating process that has low cost, is conducted at a low temperature and that yields high purity copper film.
In accordance with an aspect of the invention, a partially completed semiconductor wafer having trenches and vias formed in a layer of interlayer dielectric has a barrier layer globally formed on the surface of the partially completed semiconductor wafer. A seed layer is globally formed on the surface of the barrier layer. The barrier and seed layers are removed from portions of the surface of the partially completed semiconductor wafer on which plating is not to occur. The partially completed semiconductor wafer is then subjected to an electroless plating process and conductive material is plated on those portions of the seed layer that remains on the partially completed semiconductor wafer.
In accordance with another aspect of the invention, the seed layer and barrier layer are removed from portions of the surface of the interlayer dielectric by a polishing process.
In accordance with still another aspect of the invention, the seed layer and barrier layer are removed from portions of the surface of the interlayer dielectric by self aligning masking portions of the surface of the interlayer dielectric and etching the seed layer and barrier layers from the surface of the interlayer dielectric.
The described method thus provides a method of manufacturing semiconductor wafers that utilizes the advantages of electroless plating of copper that has low cost, can be conducted at low temperature and that yields high purity copper film.
The present invention is better understood upon consideration of the detailed description below, in conjunction with the accompanying drawings. As will become readily apparent to those skilled in the art from the following description, there is shown and described embodiments of this invention simply by way of illustration of the best mode to carry out the invention. As will be realized, the invention is capable of other embodiments and its several details are capable of modifications in various obvious aspects, all without departing from the scope of the invention. Accordingly, the drawings and detailed description will be regarded as illustrative in nature and not as restrictive.
BRIEF DESCRIPTION OF THE DRAWINGS
The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself, however, as well as a preferred mode of use, and further objects and advantages thereof, will best be understood by reference to the following detailed description of an illustrative embodiments when read in conjunction with the accompanying drawings, wherein:
FIG. 1 shows a semiconductor device in which vias and wire interconnects have been formed by standard damascene methods;
FIGS. 2A-2C show a prior art method of manufacturing semiconductor devices by global deposition or sputtering a conductive seed layer on the entire surface of the wafer and submerging the wafer into a bath of ionic solution containing copper ions that results in a thick layer of copper on the entire surface of the semiconductor wafer;
FIG. 2A shows a portion of a partially completed semiconductor wafer showing a thick layer of copper formed on the surface of the wafer,
FIG. 2B shows the portion of the partially completed semiconductor wafer as shown in FIG. 2A after a polishing process to polish the thick layer of copper, including the seed layer, formed on the surface of the wafer down to the barrier layer;
FIG. 2C shows the portion of the partially completed semiconductor wafer as shown in FIG. 2B after a polishing process to polish the barrier layer down to the surface of the semiconductor wafer;
FIGS. 3A-3D show a method of manufacturing semiconductor devices in accordance with the present invention, wherein;
FIG. 3A shows a portion of a partially completed semiconductor wafer by forming a seed layer on the surface of the partially completed semiconductor wafer;
FIG. 3B shows the portion of the partially completed semiconductor wafer after a polishing process to remove portions of the seed layer and barrier layer from surfaces on which the metal layer is not to be formed;
FIG. 3C shows the portion of the partially completed semiconductor wafer after trenches and vias in the partially completed semiconductor wafer have been filled with conductive material;
FIG. 3D shows the portion of the partially completed semiconductor wafer after excessive conductive material in the trenches have been polished;
FIGS. 4A-4F show an alternative method of manufacturing semiconductor devices in accordance with the present invention, wherein portions of a seed layer formed on the surface of the semiconductor wafer on which copper is to be formed are masked and portions of the seed layer on which copper is not to be formed are removed, wherein;
FIG. 4A shows a portion of a partially completed semiconductor wafer showing a seed layer formed on the surface of a the partially completed semiconductor wafer;
FIG. 4B shows the portion of the partially completed semiconductor wafer with a layer of photoresist formed on the surface of the partially completed semiconductor wafer;
FIG. 4C shows the portion of the partially completed semiconductor wafer after the layer of photoresist has been removed from portions of the seed layer on which copper is not to be formed;
FIG. 4D shows the portion of the partially completed semiconductor wafer after the seed layer and the underlying barrier layer have been removed from those portions of the semiconductor wafer that are not protected by photoresist;
FIG. 4E shows the portion of the partially completed semiconductor wafer after the remaining photoresist has been removed; and
FIG. 4F shows the portion of the partially completed semiconductor wafer after the trenches and vias in the wafer have been filled with conductive material.
DETAILED DESCRIPTION
Reference is now made in detail to specific embodiments of the present invention that illustrate the best mode presently contemplated by the inventors for practicing the invention.
FIGS. 3A-3D show a method of manufacturing semiconductor devices in accordance with the present invention in which portions of the seed layer and barrier layer are removed from portions of the semiconductor wafer on which copper is not to be formed, wherein;
FIG. 3A shows a portion of a partially completed semiconductor wafer 300 . The partially completed semiconductor device 300 shows a layer 302 with a metal structure 306 formed in a layer 304 of interlayer dielectric. The metal structure 306 is formed by forming a via or trench in the layer 304 , forming a barrier layer 308 on the walls of the via or trench in the layer 304 , and forming a seed layer 309 on the barrier layer 308 if the via or trench in the layer 304 is to be filled with copper. The via or trench is then filled with the appropriate conductive material to form the metal structure 306 . The seal layer or hard mask layer 310 , the layer 312 of interlayer dielectric, the seal layer or hard mask layer 318 and the layer 312 are formed on the layer 304 . The layer 310 is a seal layer if the subsequent vias and trenches are to be filled with copper. A series of masking and etching processes are then conducted to form vias, such as the via 314 and trenches, such as the trenches 322 and 324 , in the layers 304 , 310 , 312 , 318 , and 320 . A barrier layer 326 is formed on the surface of the partially completed semiconductor wafer 300 , including the walls of the vias and trenches. A seed layer 328 is formed on the barrier layer 326 of the partially completed semiconductor device 300 . Typically, the seed layer 328 is typically a material such as copper. As discussed above, there are several methods to deposit copper, however, only two can successfully form copper into the small geometries required for modern semiconductor technology. These are chemical vapor deposition (CVD) and electroplating. Of the two, CVD is too expensive because of the gases used to supply the copper ions. Electroplating is preferred because an electroplating can be done in batches, unlike a CVD process, which can only be done on one wafer at a time. When an electroplating process is utilized, a seed layer 328 is formed on the barrier layer 326 as described above. The present invention selectively deposits conductive material by means of electroless plating. Since electroless plating does not require a continuous sheet of seed layer as does electrolytic plating, the seed layer can be selectively placed where wires and vias are to be formed. The present invention will be discussed in relation to the use of copper electroless plating and a single damascene mask process. However, it is to be understood that the present invention is not limited to only copper and a single damascene process.
FIG. 3B shows the partially completed semiconductor wafer 300 as shown in FIG. 3A after a polishing or buffing process to remove portions of the seed layer 328 and barrier layer 326 from surfaces of the semiconductor wafer 300 on which copper is not to be formed. As can be seen, the via or trench is recessed and will not be affected by the polishing and buffing process.
FIG. 3C shows the partially completed semiconductor wafer 300 as shown in FIG. 3B after an electroless plating process has been conducted to plate copper onto surfaces that have a seed layer, such as the via 314 and trenches 322 and 324 .
FIG. 3D shows the partially completed semiconductor wafer 300 as shown in FIG. 3C after a polishing process to planarize the surface of the semiconductor wafer 300 .
FIGS. 4A-4F show an alternate method of manufacturing semiconductor devices in accordance with the present invention, wherein portions of a seed layer formed on the surface of the semiconductor wafer on which copper is be formed are self aligned, masked and portions of the seed layer on which copper is not to be formed are removed.
FIG. 4A shows a portion of a partially completed semiconductor wafer 400 . The partially completed semiconductor device 400 shows the layer 402 with the metal structure 406 formed in the layer 404 of interlayer dielectric. The metal structure 406 is formed by forming a via or trench in the layer 404 , forming a barrier layer 408 on the walls of the via or trench in the layer 404 , and forming a seed layer 409 on the barrier layer 408 if the via or trench in the layer 404 is to be filled with copper. The via or trench is then filled with the appropriate conductive material to form the metal structure 406 . The seal layer or hard mask layer 410 , the layer 412 of interlayer dielectric, the seal layer or hard mask layer 418 and the layer 412 are formed on the layer 404 . The layer 410 is a seal layer if subsequent vias and trenches to be formed will be filled with copper. A series of masking and etching processes are then conducted to form vias, such as the via 414 and trenches, such as the trenches 422 and 424 , in the layers 404 , 410 , 412 , 418 , and 420 . A barrier layer 426 is formed on the surface of the partially completed semiconductor wafer 400 , including the walls of the vias and trenches. A seed layer 428 is formed on the barrier layer 426 of the partially completed semiconductor device 400 . Typically, the seed layer 428 is typically a material such as copper. As discussed above, there are several methods to deposit copper, however, only two can successfully form copper into the small geometries required for modern semiconductor technology. These are chemical vapor deposition (CVD) and electroplating. Of the two, CVD is too expensive because of the gases used to supply the copper ions. Electroplating is preferred because an electroplating can be done in batches, unlike a CVD process, which can only be done on one wafer at a time. When an electroplating process is utilized, a seed layer 428 is formed on the barrier layer 426 as described above.
FIG. 4B shows the partially completed semiconductor wafer 400 as shown in FIG. 4A after a layer 430 of a photo-sensitive or non-photo sensitive resist is formed on the surface of the partially completed semiconductor wafer 400 .
FIG. 4C shows the partially completed semiconductor wafer 400 as shown in FIG. 4B after the resist has been stripped from surfaces of the wafer 400 on which copper plating is not to be formed. Because of the thickness differences between the via/trench cavities and the surface, photoresist in the non-cavity regions are removed by anisotropic stripping method. The exposed seed and barrier layers are etched away.
FIG. 4D shows the partially completed semiconductor wafer 400 as shown in FIG. 4C after an etch process to remove the seed layer 428 and the barrier layer 426 from the portions of the wafer 400 not protected by the layer 430 of resist.
FIG. 4E shows the partially completed semiconductor wafer 400 as shown in FIG. 4D with the remaining portions of the layer 430 of resist removed.
FIG. 4F shows the partially completed semiconductor wafer 400 as shown in FIG. 4F after the via 414 and the trenches 422 and 424 have been filled with a conductive material, such as copper.
The advantages of conductive material deposition, such as copper, by electroless plating are as follows:
1. conformal deposition,
2. low temperature,
3. high copper purity,
4. planar surfaces, and
5. low cost.
The basic mechanism for copper deposition by electroless plating is a two step reaction and is as follows:
1) Anodic oxidation of reducing agents on catalytic metal surface:
HCHO+2OH − =HCOO − +2H 2 +½H 2 +e −
2) Cathodic reduction of copper ions on catalytic metal surface:
Cu 2+ +2e − =Cu
The chemical components utilized are as follows:
Chemicals
Function
copper sulfate
supplies Cu ions
TMAH
supplies OH − ions
EDTH (ethylene
complexing agent
diamine tetra acetic
acid)
Formaldehyde
reducing agent
Ammonium cyanide
complexing agent
Surfactant
reduce surface tension and allow solution
to reach small features
The requirements for the seed material are as follows:
1. must be catalytically active for nucleation
2. must be conductive, and
3. must be non-oxidized, non-contaminated, and have a clean surface.
Suitable seed layer materials are as follows:
Palladium, Platinum, Nickel, Gold, Silver, Cobalt, Tungsten (ok/poor adhesion). The commonly used materials; Ti, TiN, Ta, and Al are not suitable as the seed layer. Tungsten is not catalytic, but galvanic displacement results in monolayer copper formation, thus initiating deposition. Therefore, if tungsten is used as a seed layer, it is essential that the surface is ultraclean.
The deposition conditions for the electroless plating of copper are as follows:
Temperature 40-80° C.
(70° C. typical)
Deposition Rate: 150-300 Å/min
(200 Å/min typical)
pH value: must >12
(12.5 typical)
Resistivity:
2.0 micro ohms cm
Microstructure:
epitaxial growth on Cu, grain size -
0.1 μm.
In summary, the results and advantages of the method of the present invention can now be more fully realized. The described method provides a method of manufacturing a semiconductor device that utilizes the advantages of electroless plating of copper that has low cost, can be conducted at low temperature and that yields high purity copper film.
The foregoing description of the embodiments of the invention has been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed. Obvious modifications or variations are possible in light of the above teachings. The embodiments were chosen and described to provide the best illustration of the principles of the invention and its practical application to thereby enable one of ordinary skill in the art to utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated. All such modifications and variations are within the scope of the invention as determined by the appended claims when interpreted in accordance with the breadth to which they are fairly, legally, and equitably entitled. | A method of manufacturing semiconductor wafers using electroless plating processing. A partially completed semiconductor wafer having trenches and vias formed in a layer of interlayer dielectric has a barrier layer globally formed on the surface of the partially completed semiconductor wafer. A seed layer is globally formed on the surface of the barrier layer. The barrier and seed layers are removed from portions of the surface of the partially completed semiconductor wafer on which plating is not to occur. The partially completed semiconductor wafer is then subjected to an electroless plating process and conductive material is plated on those portions of the seed layer that remains on the partially completed semiconductor wafer. | 7 |
TECHNICAL FIELD
Applicants' invention relates to microprocessor based devices and, more particularly, to a system for processing alarm notifications.
RELATED APPLICATIONS
This application is related to commonly assigned co-pending application Ser. No. 07/497,451, "An Equivalent Network Interface Module for Connecting a Programmable Logic Controller to a High Speed Communications Network"; Ser. No. 07/497461 "A System for Sharing Data Between Microprocessor Based Devices"; Ser. No. 07/497,465, "Apparatus for Networking Programmable Logic Controllers to Host Computers"; and Ser. No. 07/497,455, "Emulation of a Programmable Logic Controller by a Host Computer".
BACKGROUND ART
As industrial automation advances, interconnectivity between various microprocessor based plant floor devices, such as programmable logic controllers ("PLCs"), and plant computers, becomes more and more desirable. For example, the extensive math and register commands of a PLC can perform data pre-processing on raw data right at the raw data's point of origin, as opposed to uploading all of the raw data to the host computer, thereby permitting use of a smaller host computer.
Various schemes have been developed to interconnect PLCs and host computers, but their applications have been limited. For example, if one wanted to communicatively couple three PLCs in the absence of a network, each PLC would typically require a separate serial, or point to point, connection with each of the other two PLCs. However, the speed of serial communication is limited. Further, as the number of interconnected PLCs grows linearly, the number of serial connections grows geometrically.
In a co-pending, commonly assigned patent application Ser. No. 180,093, "now abandoned" a peer-to peer system is disclosed for interconnecting a plurality of PLCs. However this system requires a dedicated communication network.
Allen-Bradley Company, Inc., in conjunction with Digital Equipment Corporation ("DEC") has developed a system marketed under the trade name "Pyramid Integrator" for interconnecting devices over the relatively standardized Ethernet network via DEC's VAX® computer. However according to this system, only a maximum of four PLCs can be coupled to an Ethernet network per VAX computer, and each of the PLCs must be plugged into the backplane of the VAX computer. If five PLCs are required on the Ethernet, two VAX computers are required. This greatly adds to the expense of automation.
In addition, a host computer can concurrently perform a plurality of applications programs, or user tasks. When a PLC is connected to such a host computer, it is often important for the host computer to obtain data from the PLC. Typically this is accomplished by having the host computer poll the PLC. However, this polling either requires the host computer to interrupt the PLC's processing of its ladder program, or it requires the host computer to wait for the PLC to complete a scan of its ladder program. Further it is often important for the PLC to send unsolicited information to the host computer.
Messages typically are transmitted between microprocessor based devices on an Ethernet network in the form of data packets. The data packets generally include a preamble portion comprising routing information and protocol type, a user defined portion comprising the message itself, and an error detection portion. As the speed of communication between microprocessor based devices increases, error detection operations become ever more critical. Typically the error detection operation views the entire data packet to determine existence of an error. This often does not quickly enough detect errors in the user data portion. Further, the protocol often cannot accurately respond to lost messages.
Finally as automated systems control ever larger operations, handling and prioritizing of event notifications or alarms, such as faults, alerts and warnings, by the host computer becomes even more important. While certain host computers have been able to receive alarms, they have been received on a global basis, rather than individually on a user task basis.
Applicants' invention is provided to solve these and other problems.
SUMMARY OF THE INVENTION
It is an object of the invention to provide an apparatus for interconnecting PLCs and other microprocessor based devices over a high speed communications network, such as Ethernet.
It is a further object of the invention to provide a system wherein a host computer can immediately obtain data from a PLC without interrupting execution of the PLC's ladder program and wherein the host computer can receive unsolicited information from the PLC.
It is a still further object of the invention to provide a communication protocol including high speed error detection of the user data portion of a data packet.
It is yet another object of the invention to provide a communication protocol which can accurately respond to lost messages.
Finally, it is an object of the invention to provide a system which prioritizes alarms, such as faults, alerts and warnings, while also allowing for an essentially unlimited number of alarms per queue.
Other features and advantages of the invention will be apparent from the following specification taken in conjunction with the following drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a plurality of microprocessor based devices coupled to a high-speed communications network;
FIG. 2 is a more detailed block diagram illustrating software architecture of a host computer and a PLC, each coupled to the high-speed data communications network;
FIG. 3 is a software data flow diagram illustrating important elements in the communications architecture of the system; and
FIG. 4 is a graphic illustration of the communication buffer of FIG. 3.
DETAILED DESCRIPTION
While this invention is susceptible of embodiments in many different forms, there is shown in the drawings and will herein be described in detail, a preferred embodiment of the invention with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention and is not intended to limit the broad aspects of the invention to the particular embodiment illustrated.
A first programmable logic controller ("PLC") 21 coupled to a high-speed data communications network 23 is illustrated in FIG. 1. Other microprocessor based devices such as a host computer 25 or other microprocessor based devices 27, 29 can also be coupled to the communications network 23. The host computer 25 can be a VAX® computer, sold by the Digital Equipment Corporation, and the PLC 21 can be a SY/MAX® Model 650 programmable controller, sold by Square D Company, assignee of this patent application
The communications network 23 comprises a Thin Wire Ethernet (Type 10BASE2) 10 Mbaud network. The host computer 25 can couple directly to the Thin Wire Ethernet network with an appropriate Thin Wire Ethernet interface (not shown), or it can attach to a standard Ethernet (Type 10BASE5) network which is then connected through a repeater (not shown) to the Thin Wire Ethernet network.
Up to 100 microprocessor based devices can be connected to the communications network 23. A standard Thin Wire Ethernet network may have up to 30 devices attached. If a multi-port Thin Wire repeater is used, however, each of the repeater ports can have a 29-device network attached. All the Thin Wire and standard Ethernet networks connected through the repeater are logically part of the same network, therefore drop numbers (discussed below) used must be unique across the whole network. This is how up to 100 microprocessor based devices can be connected to the one communications network 23.
One such repeater is a DEC model DEMPR-AA multi-port repeater which has one 15-pin transceiver cable connector and eight Thin Wire connectors. Another repeater is a DEC model DESPR-AA single-port repeater, which has one 15-pin transceiver cable connector and one Thin Wire connector. The 15-pin transceiver cable is used to connect the repeaters to a standard thick-wire Ethernet. The DEMPR-AA and DESPR-AA count as one Thin Wire network drop on each network to which they are attached, so up to 29 microprocessor based devices can be attached to each port. The repeaters do not require drop numbers.
The first PLC 21 includes a control processor 31 (Motorola 68010), an image table 32 and a scan processor 33 (AMD 29116). Traditionally PLCs have required a separate network interface module (or "NIM") in order to communicate on a high-speed communications network such as Ethernet. In accordance with one aspect of the invention, the first PLC 21 includes an equivalent network interface module (ENIM) 35. The ENIM 35 comprises a communications processor 37 (Motorola 68010) and random access memory operable as an ENIM mailbox register 39. As discussed below, the ENIM 35 is coupled to the communications network 23 via a first port 35a.
A two-port RAM 41 has first and second ports 43, 45, respectively. The first port 43 is coupled to the ENIM 35. The second port 45 is coupled to a data bus 47. The data bus 47 is also coupled to the control processor 31, the image table 32 and the scan processor 33. The control processor 31 accesses the two-port RAM 41 via the data bus 47. The control processor 31 transfers data from the two-port RAM 41 to the image table 32, which is accessed by the scan processor 33. Thus, the ENIM 35 and the control processor 31 exchange data via the two-port RAM 41.
The mailbox register 39 provides random access registers to permit the first PLC 21 to receive unsolicited messages from other devices coupled to the communication network 23 without affecting operation of the scan processor 33. Unsolicited messages can also be received directly in the image table 32, but this requires interruption of the scan processor 33. Typically messages are first placed directly into the ENIM mailbox register 39 and then are moved into the image table 32 at predetermined times by the scan processor 33. Only critical unsolicited messages, such as a stop bit to stop the scan processor 33, are placed directly into the image table 32.
Software architecture of the host computer 25 as viewed by a user is illustrated in FIG. 2.
As indicated above, traditionally a PLC required a network interface module (NIM) to communicate over a high-speed data communications network. Such a NIM typically had only a single high-speed port, adaptable to communicatively couple to the network, and a serial port. Thus, in order to communicate between two networks, two separate NIMs were required so that each of the two high-speed ports could be coupled to a respective one of the networks. The two NIMs would then be jointly coupled by their serial ports. According to the invention, the host computer 25 is provided with software architecture including a network to network (net-to-net) software bridge which permits PLCs and other similar devices coupled to the communications network 23 to communicate directly with user tasks within the host computer 25 as though the user tasks were simply other PLC's on the communications network 23. Accordingly, such other PLC's are able to request data from the user tasks while the user tasks are running.
As discussed above, host computers have been able to poll specific PLCs coupled thereto for information, though such polling has required either interruption of the PLC's scan cycle, or waiting for completion of the PLC's scan cycle. However, these traditional host computers have been unable to obtain unsolicited messages from a PLC. Further, a host computer typically concurrently runs a plurality of user tasks. Sometimes it is desirable for unsolicited information from a PLC to be available for all of these concurrently running user tasks. At other times, it is desirable that the unsolicited information be available for only one, or a limited number, of these concurrently running user tasks.
Accordingly, the host computer 25 illustrated in FIG. 2 operatively includes software architecture comprising a dispatcher (or software bridge) 52, a system task 53, system task operating memory 53a, a global mailbox register 54, and first, second and third user tasks 55, 57 and 59, respectively. Three user tasks 55, 57 and 59 are disclosed herein for illustrative purposes; however, it is to be understood that any number of such user tasks could be used without departing from the spirit and scope of the invention. The dispatcher 52 accepts and routes data transfers between the user tasks 55, 57 and 59, the system task 53 and other devices on the communications network 23. The dispatcher 52 thus acts as an intermediary between the system and user tasks 53, 55, 57, 59, and the physical communication channel operating as the communications network 23 in a manner transparent to the system and user tasks 53, 55, 57, 59.
The host computer 25 further includes a global alarm queue 60. Specifics of the software architecture are discussed below with respect to FIG. 3.
As viewed in FIG. 2, each of the first, second and third user tasks, 55, 57 and 59 includes respective first, second and third user task operating memory 55a, 57a, 59a, wherein operating data is stored, as is well known. Each of the first, second and third user tasks, 55, 57 and 59 further includes respective first, second and third user task mailbox registers 61, 62, 63, and a respective first, second, and third alarm queue 64, 65, 66. Each of the first, second and third user tasks 55, 57, 59 is communicatively coupled to the dispatcher 52 by a software bus 67. The dispatcher 52 is a server program and includes first and second network modules 69, 71 and a host configuration table 72. The first and second network modules 69, 71 cooperate as an ENIM between the communications network 23 and the software bus 67. Specifically, the first network module 69 and second network module 71 emulate two back-to-back hardware NIMs which traditionally, as described above, had been used to interconnect two networks. The first and second modules 69, 71, permit the PLCs on the network 23 to communicate with selected ones of the user tasks 55, 57, 59 as though they were just other PLCs.
Devices on the communications network 23 are operatively located at "drops". In order to route a message from one device to another, a routing address is added to the message indicating where the message is from (originating drop number), where the message is going (destination drop number) and the path for the message to get there (routing drop number). For example, the first PLC 21 is located on the communications network 23 at a drop "5", and the host computer 25 is located on the communications network 23 at a drop "7". The first user task 55 is located at a drop "6", the second user task 57 is located at a drop "8", and the third user task 59 is located at a drop "9". The global mailbox register 54 and the global alarm queue 60 are assigned a drop number of 100 plus the drop number of the computer 25, in this case being "107". The global mailbox register 54 and the global alarm queue 60 have the same drop number. Data to be sent to the global mailbox register 39 is distinguished from data to be sent to the global alarm queue 60 by the particular register address.
The task mailbox registers 61, 62, 63, and their respective alarm queues 64, 65, 66, are assigned the drop number of their respective device. For example, the first user task mailbox register 61 is located at drop number "6". Therefore, the first user task mailbox register 61 and the first user alarm queue, have the drop number "6". As with the global mailbox register 54 and the global alarm queue 60, the user task mailbox registers 61, 62, 63 have the same drop numbers as their respective user alarm queues 64, 65, 66. Data to be sent to one of the user task mailbox registers 61, 62, 63 is distinguished from data to be sent to one of their respective user alarm queues 64, 65, 66, by the particular register address.
Two locations in the first PLC 21 are able to receive and store data, that being the mailbox register 39 and the image table 32. In order to route information from the two-port RAM 41 to the global mailbox register 54, one uses the routing address (5, 107). The number "5" of the routing address (5, 107) represents the location of the origination of the data, in this case being the device coupled to drop number "5". The number "107" of the routing address (5, 107) is the address of the global mailbox register 54.
The ENIM mailbox registers of the individual PLCs on the communications network 23, such as the mailbox register 39 of the first PLC 21, are assigned an address number "200". When routing data to a particular ENIM mailbox register, such as the mailbox register 39, the number "200" precedes the drop number of its respective drop location. For example, if data is to be transferred from the first user task 55, to the mailbox register 39, the routing would be (6, 7, 200, 5). The number "6" of the routing address (6, 7, 200, 5) indicates the location of the origination of the message, in this case being the drop number of the first user task 55. The number "7" of the routing address (6, 7, 200, 5) represents the exit from the software bus 67. The number "200" of the routing address (6, 7, 200, 5) indicates that the data is going to a PLC mailbox register, and the number "5" of the routing address (6, 7, 200, 5) indicates that it is the PLC mailbox register of the PLC coupled to drop number "5".
If unsolicited register data is to be available for each of the user tasks 55, 57, 59, the message is routed to, and stored in, the global mailbox register 54. However, if the unsolicited register data is only for one of the user tasks, such as the first user task 55, the message is directed to the first user task mailbox register 61. Similarly, if the message is for a selected, limited number, though not all, of the user tasks, the unsolicited register data would be sent to the mailbox registers of the selected, limited number of the user tasks. Similarly, the first PLC 21 or other similar devices on the communications network 23 can also obtain data from the individual user task mailbox registers 61, 63, 65, or the global mailbox register 54. Software resident in the host computer 25 supports the user task mailbox registers 61, 62, 63 and the global mailbox register 54.
The user task mailbox registers 61, 62, 63, are requested and specified when the respective user task first connects to the dispatcher 52. The host configuration table 72 is a block of 1000 registers coupled to the second network module 71. As indicated above, the first network module 69 and second network module 71 emulate two back-to-back hardware NIMs. Therefore, as with the ENIM 35, the host configuration table 72 has an address of "200" followed by the drop number of its respective drop location, which in this case would be (200,7). The host configuration table 72 specifies protocol data, such as response time-outs, retries and the like.
Measures such as slave response timeouts, reply timeouts and message retries are utilized to limit the inherently non-deterministic nature of the Ethernet network. These measures allow a user to specify a maximum time to wait for a message to be delivered, or a reply to be received, without error, effectively providing deterministic behavior on the network.
Each of the user tasks 55, 57, 59 can have up to 8192 user task registers numbered in the range 0001-8192. Three of the registers from each of the user tasks 55, 57, 59, form the respective alarm queues 64, 65, 66, and the remainder of these user task registers from each of the user tasks 55, 57, 59, form the respective user task mailbox registers 61, 62, 63. The particular mailbox register numbers are specified by its respective user task. Start and end register numbers of start and end registers can be anywhere in the range, if fewer than 8192 registers are needed. For example, 1000 mailbox registers could be numbered 1234-2233, if desired.
Each of the user tasks 55, 57, 59 can access its own respective mailbox register 61, 62, 63 in either of two ways, specifically by (1) indexing into an array or (2) with read/write register commands.
Indexing into an array is the most efficient way, as it is the user task's own mailbox register which is being read. Accordingly, the particular one of the user tasks 55, 57, or 59 specifies memory blocks in random access memory (RAM) of the host computer 25. These specified memory blocks are used as mailbox registers, and the particular user task can access the specified memory blocks as an array of 16-bit register values. In the example above (mailbox registers 1234-2233), the user task reads its mailbox register 1235 by reading the second word of the register array (memory block).
The second way of accessing a user task's own mailbox register is similar to reading any other mailbox register in that a read/write register command (a command by a user task to read or write to a particular register) is utilized. This is less efficient than the first way of a user task accessing its own mailbox register, discussed immediately above, as read or write subroutines must first be called. With read/write register commands, an empty route field of a register command (the terminator is the first entry) indicates that reads and writes will refer to the user task's own mailbox registers.
A 2-drop route field in a register command is used to read and write to other task's local mailboxes. A 3-drop route field is used to read the global mailbox 54; the middle number of the 3-drop route field being the drop number of the host computer 25 and the last number of the 3-drop route field being the number "100" plus the drop number of the host computer 25.
The actual software architecture is illustrated in the data flow chart of FIG. 3. The system task 53 architecturally appears simply as another one of the user tasks, thus the following discussion with respect to the first user task 55 applies as well to the system task 53. Reference numbers common to FIG. 2 have been maintained.
Messages from one of the user tasks 55, 57, or 59 to another of the user tasks 55, 57, or 59, or from the communications network 23 or the system task 53 are routed through the dispatcher 52, as follows.
Each of the tasks, user tasks as well as system task, includes a respective per-process mailbox, such as the first per-process mailbox 80 associated with the first user task 55. The per-process mailbox 80 is used as a signaling mechanism to inform the respective tasks that a message is available. Messages sent via the per-process mailbox 80 are simply a prompt; only a few bytes of pertinent data are actually transferred via the per-process mailbox 80. The actual message is placed into and temporarily stored in a communication buffer 82.
The communication buffer 82 performs the function of the software bus 67 (FIG. 2) and is illustrated in FIG. 4. The communication buffer 82 is part of the virtual memory RAM of the host computer 25, which is allocated by the software of the host computer 25 under control of the dispatcher 52. The communication buffer 82 includes reply input queue pointers and command input queue pointers for each of the tasks, user as well as system, such as the first reply input queue pointers 84 and the first command input queue pointers 86 which are associated with the first user task 55. The command input queue pointer 86 stores memory addresses of command messages directed toward the user task 55, and the reply input queue pointer 84 stores memory addresses of reply messages directed toward the user task 55. The respective reply input queue pointers and command input queue pointers operate similarly for their respective tasks. Reply messages have a higher priority than command messages, therefore the communications buffer 82 distinguishes reply messages from command messages so that reply messages can be processed first.
The communications buffer 82 further includes dispatcher queues, specifically dispatcher input queue pointers 88 and free list queue pointers 94. Additionally, the communication buffer 82 includes message buffers 96.
The message buffers 96 are memory locations for storing messages. The dispatcher input queue pointers 88 identify locations in the message buffer 96 for messages received from the various ones of the tasks, user as well as system. The free list queue pointers 94 identify unused (ie, available) locations in the message buffer 96. Messages received from the communications network 23 are given a higher priority than messages from the tasks to lessen the chance of missing a message from the communications network 23.
Referring again to FIG. 3, the per-process mailbox 80 is simply a VMS (VAX software) mechanism for sending a prompt, indicating that a message is waiting. Data in one of the per-process mailbox interrupts the particular one of the tasks associated with the one of the per-process mailboxes, causing the particular one of the tasks to read the message, command or reply, located at the address stored in its respective reply and/or command input queue pointers in the communications buffer 82.
Messages are similarly transferred from a task to the dispatcher 52. However because the dispatcher 52 does not distinguish between reply and command messages, only one queue is required.
To send a command message from one of the user tasks, the particular user task obtains an available message buffer from the free list queue pointers 94.
To send a reply message from one of the user tasks, the particular user task uses the same buffer which the command message was delivered in. In this way there will never be the situation where there are no free buffers to accept the reply message.
The particular one of the user tasks then writes the message data into the message buffer, and queues the message on the dispatcher input queue pointer 88. If the dispatcher input queue pointer was empty, a prompt is sent to a dispatcher prompt mailbox 98 to indicate a presence of a new message. The dispatcher 52 will process the messages identified in the dispatcher input queue pointer until none are left.
For messages to be transferred from the dispatcher 52 to the communications network 23 (ie. outbound Ethernet messages), the dispatcher 52 passes the address of the message to an Ethernet driver 97. The dispatcher 52 includes a pending outbound message pointer 52a and an inbound message queue pointer 52b. The pending outbound messages queue pointer 52a identifies message buffer locations for messages to be transmitted on the communications network 23. The inbound message queue pointer 52b identifies message buffer locations for messages to be transferred from the dispatcher 52 to one of the tasks, user as well as system.
The host computer 25 must be able to reliably deliver messages. Messages may not be dropped except for extraordinary circumstances.
When a command message must be delivered to the first user task 55, the dispatcher 52 will queue the command message to the command input queue pointer 86. If the command input queue pointer 86 is empty, a message prompt will be sent to the first user task's 55 per-process mailbox 80. If the first user task's command input queue pointer 86 is not full, the message is queued, and no prompt is sent.
If the particular task specified by the routing address is not connected to the dispatcher 52, an error reply is generated. The error reply is sent to the source of the command message.
One does not want to overwhelm a particular task with commands such that the particular task cannot respond to commands as quickly as they are received, as this conceivably could result in filling all of the available communication buffers, which could then also back-up other ones of the tasks. Although this has not been found to be a problem in practice, it is contemplated that an error command could be generated if such did occur.
Unsolicited messages can be accepted by the tasks, user as well as system. These messages can read and write data to the local mailboxes and write alarms to the local alarm queues.
Mailbox registers and alarm queues (both local and global) can also be used to implement data sharing between application programs. However, tasks will only respond to alarms, and read/write of the task mailbox registers. Other functions will result in error replies being returned to the sender.
The present invention also provides for prioritization and response to alarms by the host computer 25, both on a global level as well as on a user task level. Alarms on the global level are accessible by any one of the user tasks 55, 57, 59, while alarms on the user task level are only accessible by that particular one of the user tasks 55, 57, 59.
As discussed above, the dispatcher 52 is provided with a global alarm queue 60. The global alarm queue 60 has three levels of alarm sub-queues, specifically a global fault alarm queue 60a for storing global fault alarms, a global alert alarm queue 60b for storing global alert alarms and a global warning alarm queue 60c for storing global warning alarms.
In addition, each of the first, second and third user alarm queues 64, 65, 66 includes three similar user level alarm sub-queues, 64 a,b,c, 65 a,b,c and 66 a,b,c, respectively. Each of the user level alarm sub-queues can receive an alarm of up to 128 16-bit registers.
An alarm queue entry, whether global or user-level, contains the following information:
1. a reference number
2. a time-stamp indicating the time the alarm was received by the host computer 25;
3. a routing address (the route from originator to destination);
4. level of alarm (ie. fault alarms, alert alarms and warning alarms);
5. a user specified alarm code; and
6. user specified data.
The allowed number of alarms per queue and the number of user data registers is determined by the user, depending upon an anticipated number of alarms as well as available memory. Each of the user tasks 55, 57, 59 can perform the following functions in response to alarms in their own alarm queues as well as the global alarm queue:
1. Read first alarm -- get alarm data for 1st (ie., oldest) alarm in a queue;
2. Read specific alarm -- get alarm data for an alarm, specified by the reference number of a particular alarm;
3. Read next alarm -- get alarm data for the alarm with a reference number greater than (i.e., newer than) a reference number specified;
4. Clear alarm -- delete an alarm from a queue;
5. Clear and acknowledge alarm -- acknowledge and delete an alarm from a queue;
6. Clear all alarms -- delete all alarms from a queue;
7. Clear and acknowledge all alarms -- acknowledge and delete all alarms from a queue;
8. Set alarm notify -- set up for task notification on addition/deletion of an alarm to/from a queue; and
9. Read alarm queue information -- get information about an alarm queue.
As previously indicated, there are three types (levels) of alarm sub-queues: fault queues; alert queues; and warning queues. In general, the severity of an alarm condition dictates which alarm sub-queue the alarm is posted to, with fault alarms being the most severe and warning alarms being the least severe.
An alarm is written to an alarm queue, by another device, by issuing a write-register command to the particular register, based on the queue to be written. In the present embodiment, these "pointer" registers are:
1. register number "8101" for a fault alarm;
2. register number "8102" for an alert alarm; and
3. register number "8103" for a warning alarm.
Thus, a fault alarm to be sent by the PLC 21 at drop number "5" to the first user task alarm queue 64 would have the routing address (5, 7, 6) and would be written to register number 8101.
Generally, an alarm acknowledgement is sent back to the same register, in the device issuing the alarm, as the queue to which the alarm was written, though this can be overridden if the user desires to send an acknowledgement to a different register.
The first register value in the data field of an alarm write-register is an alarm code to be posted, and the remaining register values are support data for the alarm. The amount of support data for a particular alarm is controlled by the user's application and needs and can range from 0 to a user-specified number of registers, up to a maximum of 127 registers. A complete alarm write-register command, such as from the PLC 21, would contain:
1. a routing address from the device sending the alarm to the alarm queue location;
2. an alarm "opcode" indicating an alarm operation to be performed;
3. the sending device's status register address, which does not effect the alarm writing process;
4. the alarm queue register address (8101, 8102, or 8103) as the destination of the write register;
5. the alarm code for the particular alarm; and
6. any support data particularly desired by the user (0 or more user specified registers).
The dispatcher 52 further includes a configuration file 52c comprising a disk file that the dispatcher 52 reads when it starts running to determine a number of operating parameters, such as the drop number of the host computer 25. As indicated above, the drop number of the global alarm queues is the drop number of the host computer 25 plus 100. Therefore, the route of an alarm write operation would have the drop number of the host r computer 25 plus 100 as the last route number.
Each alarm queue entry is time-stamped with the current time of the host computer 25 when it is written to an alarm queue. Additionally, each alarm queue entry is given a unique reference number for identification. If an attempt is made to write an alarm to an alarm queue that is already full, a standard error code, such as "alarm buffer full", is returned in a priority-write reply message.
The three global alarm queues 60a, 60b, 60c are specified when the system task 53 is initially started up, usually upon system boot. The length (number of entries) and width (maximum number of support data registers) of these alarm queues are specified in the configuration file 52c and can be modified only by shutting down the dispatcher 52, modifying the configuration file 52c, and restarting the dispatcher 52, such as by re-booting the system. If the length of the global alarm queues is specified as 0, no global alarm queues are created.
Any external device or internal task can write to the global alarm queues, and any internal task can view, clear, and acknowledge alarms from the global alarm queues.
Each of the user tasks 55, 57, 59 has an option of setting up three alarm queues for itself This is done when the particular one of the user tasks first "connects" to the dispatcher 52. These local alarm queues can only be read by the particular one of the user tasks; however alarms can be sent to the local alarm queues from anywhere on the system. The user task's drop number, which is also specified when the user task connects to the system task 53, is used as the last route number in the route field address of an alarm write operation. The second-last route number is the drop number of the host computer 25.
Any external device or internal task can write to a user task's local alarm queues, but only that particular user task can view, clear, and acknowledge such an alarm.
Any particular one of the user tasks 55, 57, 59 has an option of being "interrupted" when an alarm is added or removed from each of its three alarm queues. Alarm notification can be turned on or off for each of the alarm queues (fault, alert, and warning) and operation type (addition and removal). Global and user task alarm queues are accessed independently.
Alarm addition notifications occur when an alarm is added to a specified queue. Similarly, alarm removal notifications occur when an alarm is removed from a specified queue. This includes when a user task clears an alarm from one of its own queues if it has alarm removal notifications set on that queue.
The user tasks cannot be interrupted while their interrupt routines are executing. Alarm notifications will be stacked, and each call to the interrupt routine will consist of only one notification event.
The "interrupt" takes the form of a user-provided subroutine that is called when any of the desired alarm queue operations takes place. When a user task connects to the dispatcher 52, the particular user task specifies which alarms to interrupt on, plus the interrupt routine address. A default is provided which causes no interrupts to be generated.
The user task can also change the interrupt routine while running, so that changes to the interrupt routine address can be made `on the fly`. All alarm notification interrupts for a particular one of the user tasks must use the same interrupt routine.
Data passed to the interrupt routine includes:
1. queue location -- global or local;
2. queue type -- fault, alert, or warning;
3. queue operation -- alarm added or alarm removed; and
4. reference number of the alarm.
The reference number of an alarm is useful even if the interrupt is an alarm removal. For example, this would allow an alarm display to remove cleared alarms from a video display screen (not shown) without having to re-read the entire alarm queue contents.
The system task 53 maintains a table of interrupt notification settings for any of the user tasks that require notification of global alarms. The table will accommodate notification information for up to 100 tasks. There can be no more than 100 tasks connected to the system task 53 at any time.
To assure accurate data transmission over the communications network 23, a high performance, positive acknowledgment retransmission communication protocol has been provided. This communication protocol is used by any of the processor based devices on the communications network 23, including the host computer 25, that wish to exchange information.
For each message correctly received by a receiving device, a positive acknowledgment, or "ACK", is returned to a sending device on the communications network 23 sending the message. If the receiving device receives an incorrect message, the receiving device will attempt to send a negative acknowledgment, or "NAK", back over the communications network 23. Both ACKs and NAKs contain a transmission number of the last message successfully received by the receiving device.
To guarantee that a message or its corresponding acknowledgment does not get lost, a timer is provided. The timer determines if the sending device waited long enough for an acknowledgment (ACK) to be returned. The length of time that the sending device waits is user determinable.
The protocol has the following features:
1. A route address Each device on the communications network 23 that is to communicate with this protocol must have an unique route address. The route address of the PLC 21 is set by using a four-bit rotary switch and four DIP switches located on the PLC 21. For other devices on the communications network 23, the route address can be set by the software of the particular device. The route addresses can range from 00 to 99.
2. A transmission number. Each device that is to communicate with this protocol must keep track of the next transmission number it will send to each of the other devices on the communications network 23. The transmission numbers help insure error-free data transfer. The numbering of the transmission numbers is cyclic, from 0 to 254. The transmission number is initialized at the number 255.
3. Pipelining. Each device that is to communicate with this protocol allows additional messages to be sent while awaiting an acknowledgment of each of the messages previously transmitted. Accordingly, a positive acknowledgement not only confirms that the specified message had been received correctly, it also specifies that all previous unacknowledged messages to the particular device were also received error-free.
4. An "ACK" implied in a "NAK". All acknowledgements contain the transmission number of the last message successfully received from a particular device, thus allowing a negative acknowledgement (NAK) to also provide positive acknowledgments of earlier messages.
Each device on the communications network 23 maintains an address table of known active route addresses as well as Ethernet addresses. The address table is used to correspond the route address of each device with its corresponding Ethernet address.
Ethernet addresses have a length of 48 bits. As specified in IEEE Std. 802.3, the first bit transmitted specifies if the message is for a single device (bit=0) or if the message has a multicast address (bit=1). A multicast address can be received by a plurality of devices on the communications network 23. The second bit transmitted in the Ethernet address is used to distinguish between locally (bit=1) or globally (bit=0) administered addresses. A globally administered address indicates that the following 22 bits have been assigned by the above IEEE standard. All communications with this protocol use globally administered addresses.
The PLC 21 can generate its own Ethernet address, consisting of an assigned block of addresses and a value generated from the rotary and DIP switches. However, the Ethernet addresses of other devices (i.e., host computers or other PLCs unable to generate an Ethernet address) are not automatically known.
There are two methods to obtain the Ethernet addresses that are required to establish communication on the communications network 23. According to the first method, a single multicast (i.e., a message containing a multicast address) CONNECT message is sent over the communications network 23 after start-up. This CONNECT message allows all of the devices that are currently on the communications network 23 to place the Ethernet address of the new device in their respective Address tables
The devices on the communications network 23 that receive the CONNECT message do not return a response. After they place the source's Ethernet and route address in their Address table, they discard the CONNECT message. The source of the CONNECT message, after sending the CONNECT message, is then able to transmit and receive other messages over the communications network 23.
All devices physically must be connected to the communications network 23 before their Ethernet Driver is installed. If the user fails to follow this procedure, the devices on the communications network 23 will not receive the CONNECT message of a new device. Any device that wishes to communicate with the new device will then need to get the new device's Ethernet address by using a GET ADDRESS command, described below.
With the CONNECT message, only the devices that are currently listening on the communications network 23 will know the Ethernet address of any new device. Consequently, a second method of establishing Ethernet addresses is provided to communicate with this protocol. This second method uses a GET ADDRESS request, a multicast message that is actually a superset of the CONNECT message.
The GET ADDRESS REQUEST is transmitted whenever a first device, already established on the communications network 23, needs to transmit a message to a new device having a route address that has not been established in the Address table of the first device. The GET ADDRESS REQUEST is also received by all devices that are communicating with this protocol. Though each device on the communications network 23 will receive the message, the message will indicate which particular one of the devices should return a response. The remainder of the devices on the communications network 23 store the Ethernet address and route address of the new device in each of their Address tables and discard the message.
The GET ADDRESS REQUEST is only used to establish the addresses of the devices on the communications network 23. The GET ADDRESS REQUEST does not contain any data destined for an end device or task. Once the addresses of the devices on the communications network 23 are established, data can be sent to the end devices or tasks.
The device that responds to the GET ADDRESS REQUEST (the responding device) stores the route address and Ethernet address of the source device issuing the GET ADDRESS REQUEST in its Address table. The responding device then sends a multicast GET ADDRESS RESPONSE. This GET ADDRESS RESPONSE allows all other devices on the communications network 23 to update their Address table with the addresses specified in the GET ADDRESS RESPONSE. The GET ADDRESS REQUEST and GET ADDRESS RESPONSE, as well as all other multicast messages, will not be acknowledged. If a GET ADDRESS RESPONSE is incorrectly received, a timeout will occur and a GET ADDRESS REQUEST will be retried.
In the event the GET ADDRESS RESPONSE is not returned within a timeout period (defined to be the greater of 5 seconds, or 4 times the time that a device should wait for an acknowledgement), the GET ADDRESS REQUEST will be sent again. If, after 8 retries of the GET ADDRESS REQUEST, a GET ADDRESS RESPONSE is still not received, all messages for this route address will be eliminated and, for commands, error responses will be returned to the originating device or task.
When a message that is destined for a device that exists in the Address table needs to be transmitted, the Ethernet address of that device will be used. By using the Ethernet address, only the specified device will receive the message. The first data containing message that will be sent will have a 255 as its transmission number.
Each of the devices on the communications network 23 has a Transmit Queue, a Receive Buffer, and an Unacknowledge Queue dedicated to its Ethernet port. Also, variables for the amount of time a device should wait for an acknowledgement, the next transmission number to be sent, the next transmission number to be accepted, and the number of times a message should be retried must be kept for every route address
If there is a new message in the Ethernet transmit queue and the device for which the message is destined is defined in the Address table, the following steps should be used
1. For each new message, a variable for the next transmission number to be sent for the particular route address is placed in the data field of the message. The transmission variable is then incremented and stored back in the device's memory.
2. The retry count is initialized to 0 and is stored in the message.
3. After a message is to be transmitted, a timeout value is calculated from using the current time and the timeout time for the route address the message is intended for. This timeout value is stored along with the message in an unacknowledged message queue.
4. After a message is sent, the Ethernet transmit queue is reexamined to see if there are any other messages for this device. If other messages exist, the transmitter will perform steps 1-3 on new messages (without waiting for an acknowledgment of the original message). The only exception to this step is if there are 254 outstanding messages to a particular device. For this case, the transmitter will be required to hold any new message until an acknowledgement is received to a previous message.
5. After transmitting a message(s), the device needs to examine if a timeout has occurred. This examination continues until either an acknowledgment for the message(s) is received or a timeout error occurs.
6. If a timeout error occurs, or if a NAK is received that is not due to a lack of buffer space, the retry count for this message is examined. If the device has sent the number of retries specified for the destination route address, an error handler is invoked. If the device is to re-send the message, a retry count (located in the message) is incremented and the message is sent again. A timeout error will cause a single message to be retried, provided the retry limit has not been met. A NAK, however, can cause multiple messages to be retried, depending on the transmission number that is sent with the NAK.
When an Ethernet packet is received, it must be examined to determine if it is a new message or an acknowledgment. If the packet is an acknowledgment, the following steps should be used, assuming that the corresponding addresses have been previously placed in the Address table:
1. Examine the transmission number returned in the acknowledgment. For the specific route address, if there is any message in the unacknowledge message queue with an transmission number earlier or the same to what was returned, eliminate the message. The messages that are eliminated have been positively acknowledged by the corresponding device.
2. Examine if the acknowledgment is an ACK or a NAK. If an ACK, processing is complete. If a NAK, determine which message caused the error (returned in the NAK packet). Assuming the retry count has not reached its limit, perform the following:
a. Retry all messages that are in the unacknowledge queue and were transmitted before the message that caused the NAK.
b. Retry the message that caused the NAK if it is still in the unacknowledge queue.
c. If the message that caused the NAK is to be retried, retry messages that are in the unacknowledge queue and were transmitted after the message that caused the NAK. For all NAKs, the reason for the failure is included in the message packet. If the NAK was due to insufficient room in the responding device's buffers, the device which sent the message should not increment its retry count.
If the packet is a message, the following steps are followed. Note that these steps cause an acknowledgement to occur. When any device has both acknowledgements and messages in its Ethernet transmit queue, the acknowledgements are transmitted first. This allows the device that sent the message to either purge the message from its unacknowledge queue (if an ACK was received) or retry the message (if a NAK was received).
1. Check if any errors were generated while the message was received. If an error occurred that indicates unreliable data in the message, purge the message from the buffer.
2. If the message was received without any noted errors, get the route address and the transmission number from the message and compare the next transmission number to be accepted for this route address to the transmission number from the message. If the two values are not the same, return a NAK with the value of the last transmission number accepted and purge the message from the buffer.
3. If the message was received without any errors being noted and the transmission number from the message is the value that was expected (after comparing it against the next transmission number to be accepted for this route address):
a. return an ACK with the transmission number from the message;
b. update the next transmission number to be accepted; and
c. process the message.
In order to permit pipelining (the ability to send more than one message without waiting for ACKs to each successive message), discussed above, the description in the above step 3 must be expanded. For pipelining to occur, an ACK must not only confirm that the specified message has been received correctly, but that all previous messages with numbers between the one acknowledged in the last ACK and the one acknowledged by the current ACK have been received correctly. This is accomplished by examining the transmit queue after each new message is received. If an ACK is in the transmit queue for the same device, update the transmission number that is to be sent with the ACK.
It will be understood that the invention may be embodied in other specific forms without departing from the spirit or central characteristics thereof. The present examples and embodiments, therefore, are to be considered in all respects as illustrative and not restrictive, and the invention is not to be limited to the details given herein. | A control system contains a communications network, a host computer and a programmable logic controller (PLC). The host computer includes prioritized alarm queues for receiving prioritized alarms from the programmable logic controller. Alarms fall into either a local or a global category, and each category supports three types of alarms: warnings, alerts or faults. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims the benefit of Provisional Patent Application Ser. No. 61/991,963 filed May 12, 2014, which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to submarine cables and more particularly to a system and method of suspending submarine cables with anchored buoys.
BACKGROUND OF THE INVENTION
[0003] It is recognized that communication, electrical, and other cables must necessarily cross bodies of water. In such cases, the cable is generally submerged to avoid any collisions with vessels and the like and to remove obstructions from the surface of a body of water. For simplicity the submarine cables that will be discussed herein will be referred to in the context of cables found in the ocean, or the sea, but it is understood by those of skill in the art that the cable system described herein is equally suited for fresh water applications.
[0004] Underwater, or submarine, cables are typically installed with large cable laying vessels that drop a line of cable along the bottom of a body of water, which by necessity requires additional lengths of cable for areas of increased depths and/or to accommodate various topologies along the seafloor. In some cases, underwater, or submarine, cables are installed by using cable burial plows, or the like, to place the cable a certain distance under the seafloor especially in more shallow areas. See, for example, U.S. Pat. No. 2,067,717 and U.K. Pat. No. GB 0524831. Depending on the region or the particular body of water, there may be benefits or drawbacks to burying the cable. Regardless, the amount of cable required to trace the topology of the seafloor in current systems is necessarily larger, and as such more costly, than would be required for the system of the present invention.
SUMMARY OF THE INVENTION
[0005] One aspect of the present invention is a submarine cable system for suspending a submersible cable above a seafloor comprising a submersible cable having a length, a first end, and a second end; a plurality of buoys configured to attach to the submersible cable; a plurality of tethers, each having a length, a first end and a second end, wherein the first end of each tether is in contact with a buoy; and a plurality of anchors, wherein each anchor is in contact with the second end of a tether thereby suspending the submersible cable above the seafloor when the submersible cable is submerged.
[0006] One embodiment of the submarine cable system is wherein the plurality of buoys is spaced along the length of the submersible cable.
[0007] One embodiment of the submarine cable system is wherein each of the plurality of tethers is adjustable in length.
[0008] One embodiment of the submarine cable system is wherein adjusting the length of each tether is done remotely.
[0009] One embodiment of the submarine cable system is wherein the first end of the submersible cable is attached to a vessel.
[0010] One embodiment of the submarine cable system is wherein the first end of the submersible cable is attached to a generator.
[0011] One embodiment of the submarine cable system is wherein the first end of the submersible cable is attached to land.
[0012] Another aspect of the present invention is a buoy system for suspending a submersible cable above a seafloor comprising a buoy configured to attach to a submersible cable; a tether, having a length, a first end and a second end, wherein the first end of the tether is connected to the buoy; and an anchor, wherein the anchor is connected to the second end of the tether.
[0013] One embodiment of the buoy system for suspending a submersible cable above a seafloor wherein the length of the tether is adjustable.
[0014] One embodiment of the buoy system for suspending a submersible cable above a seafloor wherein adjusting the length of the tether is done remotely.
[0015] Another aspect of the present invention is a method for suspending a submersible cable above a seafloor comprising providing a submersible cable having a length, a first end, and a second end; providing a plurality of buoys configured to attach to the submersible cable; providing a plurality of tethers, wherein each tether has a length, a first end and a second end, and wherein the first end of each tether is in contact with one of the plurality of buoys; providing a plurality of anchors, wherein each anchor is in contact with the second end of one of the plurality of tethers; and adjusting the length of each of the plurality of tethers to suspend the submersible cable above the surface of the seafloor when the cable is submerged.
[0016] One embodiment of the method for suspending a submersible cable above a seafloor is wherein adjusting the length of a tether is done remotely.
[0017] One embodiment of the method for suspending a submersible cable above a seafloor is wherein the first end of the submersible cable is attached to a vessel.
[0018] One embodiment of the method for suspending a submersible cable above a seafloor is wherein the first end of the submersible cable is attached to a generator.
[0019] One embodiment of the method for suspending a submersible cable above a seafloor is wherein the second end of the submersible cable is attached to land.
[0020] These aspects of the invention are not meant to be exclusive and other features, aspects, and advantages of the present invention will be readily apparent to those of ordinary skill in the art when read in conjunction with the following description, appended claims, and accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The foregoing and other objects, features, and advantages of the invention will be apparent from the following description of particular embodiments of the invention, as illustrated in the accompanying drawings in which like reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention.
[0022] FIG. 1 shows one embodiment of the submarine cable system of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] It is recognized that communication, electrical, and other cables must necessarily cross bodies of water. These cables are submerged and are typically draped along the seafloor or are buried in sections of the seafloor. In some cases, the cable contains a series of buoys, which are used to aid in the installation of the cable. See, for example, U.S. Pat. No. 4,659,253, where evenly spaced buoys are fixed along the cable such that they do not move during installation so that the cable tension can be controlled during installation and so that the cable does not result in a runaway situation. Runaway situations can be very dangerous and costly. Upon installation of the cable, these buoys are suspended above the cable that has been installed along the seafloor. Similarly, in other systems, such as is described in U.S. Pat. No. 4,048,686, buoys are used during the installation of the cable to reduce tension on the cable system beyond its maximum tolerances. The weight of cables varies considerably depending on whether the cable is a power cable, a communication cable, or some other type of cable. In U.S. Pat. No. 4,048,686, the buoys detach at a particular depth to release the cable to its final resting position along the seafloor.
[0024] In contrast, the submarine cable system of the present invention retains the buoys on the submersible cable and the buoys do not extend above the submersible cable when it is installed on the seafloor. Rather, the buoys are used to elevate the submersible cable from the seafloor. In certain embodiments, the buoys are tethered to anchors. The system of the present invention provides for reduced cable cost by minimizing the length of submersible cable required to traverse a body of water by using anchored buoys with tethers of varying lengths to accommodate a variety of seafloor topologies. Additionally, when the submersible cable needs to be repaired, without some form of buoying system such as described herein, the weight of the submersible cable would be prohibitively heavy and would make repairs difficult. The system of the present invention provides for a mechanism for a repair vessel to more easily grab the submersible cable and to hoist it into to position for repairs.
[0025] Referring to FIG. 1 , one embodiment of the submarine cable system of the present invention is shown. More particularly, a submersible cable 1 shown in the ocean 2 suspended some distance off the seafloor 3 . In certain embodiments of the present invention, a plurality of buoys 4 is used to suspend the submersible cable some distance off the seafloor to minimize the length of submersible cable needed to traverse a body of water. In certain embodiments of the present invention, the plurality of buoys 4 is anchored to the seafloor by a plurality of anchors 5 . The plurality of anchors 5 is tethered to the plurality of buoys 4 via tethers 6 of various lengths so that the submersible cable may be suspended in a nearly horizontal fashion regardless of the topology of the seafloor. In certain embodiments of the system of the present invention, the lengths of the tethers 6 are adjustable to facilitate installation in various underwater environments (e.g., a variety of depths, contours, and the like.). In certain embodiments, the length of the tethers 6 is configured to be adjusted remotely.
[0026] In certain embodiments of the present invention, the submersible cable 1 has a first end 10 and second end 11 . In certain embodiments, the first end 10 of the cable 1 is attached to an electrical generator. In certain embodiments, the electrical generator (not shown) can be a windmill, a flywheel, a power generator using solar, gas, diesel, wind, water or the like, or other forms of electrical or power generators known to those of skill in the art.
[0027] In certain embodiments of the present invention, the first end 10 of the cable 1 is attached to a vessel. In certain embodiments of the present invention, the first end of the cable is attached to a generator present on a vessel or platform configured to generate electrical energy. In certain embodiments of the present invention, the first end 10 of the cable 1 is attached to land. In certain embodiments, the connection to land comprises a connection to an electrical or power grid, an electrical or power storage facility or device, an electrical or power generator, or the like.
[0028] While the principles of the invention have been described herein, it is to be understood by those skilled in the art that this description is made only by way of example and not as a limitation as to the scope of the invention. Other embodiments are contemplated within the scope of the present invention in addition to the exemplary embodiments shown and described herein. Modifications and substitutions by one of ordinary skill in the art are considered to be within the scope of the present invention. | A system and method of utilizing a submarine cable system. The cable system comprises a plurality of buoys tethered to anchors. The tethers are adjustable in length to allow for suspending a submersible cable above the seafloor when installed. The system allows for cost savings, by minimizing the length of submersible cable needed to traverse a body of water. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a nonprovisional utility application of the provisional patent application, Ser. No. 61/869,207 filed in the United States Patent Office on Aug. 23, 2013 and claims the priority thereof and is expressly incorporated herein by reference in its entirety.
TECHNICAL FIELD
The present disclosure relates generally to a platform support and a method of installing said support. More particularly, the present disclosure relates to a below main cable work platform support for hanging a work platform below a main cable of a suspension bridge and a method of installation.
BACKGROUND
A suspension bridge is a type of bridge in which the load-bearing portion called the deck is hung below main suspension cables on vertical hangers or suspender cables. The main cables are suspended between towers and form a parabola, the suspenders transferring the load to the cables and the cables transferring the load to the towers.
The main cables are generally braided steel wire and are over-wrapped to form a circular cross section. At specific points along the main cable, bands are installed to carry the steel wire suspenders.
Like any steel that is constantly exposed to the elements, the steel of cables requires periodic maintenance. Generally, maintenance projects require that the bridge be shut down completely or reduced to a minimum number of lanes. Since most bridges carry a significant amount of traffic during most of the day and night, maintenance usually is limited to off-peak traffic times if possible, which extends the duration of the project.
When maintenance is performed on the main cables, workers generally must walk on top of the main cable, using a hand rope parallel above the cable to maintain balance. For safety reasons when the workers are working on the main cable, it is generally necessary to shut down several if not all lanes on the bridge to traffic which is not only inconvenient but also has economic consequences.
In the present disclosure, where a document, act or item of knowledge is referred to or discussed, this reference or discussion is not an admission that the document, act or item of knowledge or any combination thereof was at the priority date, publicly available, known to the public, part of common general knowledge or otherwise constitutes prior art under the applicable statutory provisions; or is known to be relevant to an attempt to solve any problem with which the present disclosure is concerned.
While certain aspects of conventional technologies have been discussed to facilitate the present disclosure, no technical aspects are disclaimed and it is contemplated that the claims may encompass one or more of the conventional technical aspects discussed herein.
BRIEF SUMMARY
An aspect of an example embodiment in the present disclosure is to provide a support for a work platform that permits a worker to safely traverse a main cable of a suspension bridge. Accordingly, the present disclosure provides a support for a below main cable work platform that permits a worker to traverse a main cable of a suspension bridge by walking on a flat surface platform situated below the main cable.
Another aspect of an example embodiment in the present disclosure is to provide a support for a work platform that allows bridge maintenance to be performed without disrupting traffic. Accordingly, the present disclosure provides a support for a below main cable work platform that allows bridge maintenance to be performed by workers standing on a flat platform, minimizing safety risks while working above traffic, allowing traffic to flow without disruption while maintenance work is performed.
A further aspect of an example embodiment in the present disclosure is to provide a work support that fastens to a band on the main bridge cable without disrupting the distribution of a deck load. Accordingly, the present disclosure provides a support that couples to a band on a cable by attaching a plate to the band and coupling a work platform support to the band, further coupling the work platform support to the band with a temporary strap, maintaining tension and load on the cable with the temporary strap.
Accordingly, the present disclosure describes a below main cable work platform support for hanging a work platform below a main cable of a suspension bridge and a method of installation thereof. A plurality of supports attach to a plurality of bands on a main cable. Each support has a pair of struts bolted to the band, the top of each strut on each side of the band, the struts extending downward, connecting to the ends of a horizontal bar that sits between a pair of suspender cables hanging from each band. A work platform is suspended from the horizontal bar and tie down cables extend downward from the bar attaching below to stabilize the platform against wind and uplift. The method includes the step of screwing a single bolt into a cable band for supporting a structure therebelow.
The present disclosure addresses at least one of the foregoing disadvantages. However, it is contemplated that the present disclosure may prove useful in addressing other problems and deficiencies in a number of technical areas. Therefore, the claims should not necessarily be construed as limited to addressing any of the particular problems or deficiencies discussed hereinabove. To the accomplishment of the above, this disclosure may be embodied in the form illustrated in the accompanying drawings. Attention is called to the fact, however, that the drawings are illustrative only. Variations are contemplated as being part of the disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings, like elements are depicted by like reference numerals. The drawings are briefly described as follows.
FIG. 1A is a dynamic perspective view of an example embodiment of a below main cable work platform support in place on a bridge main cable.
FIG. 1B is a side elevational view in cross section of an example embodiment of the below main cable work platform support in place on a bridge main cable.
FIG. 2 is a dynamic perspective view of an example embodiment of the below main cable work platform support in place on a bridge main cable, maintaining the work platform below the cable.
FIG. 3 is a dynamic perspective view of a plurality of the below main cable work platform supports in place on the main cable prior to installing the work platform below the cable.
FIG. 4 is a perspective view from below of the work platform installed on the example embodiment of the below main cable work platform supports.
FIG. 5 is a side elevational view of a strut of the support bolted to a band on the bridge main cable.
FIG. 6 is a dynamic perspective view of the platform in place on the example embodiment of the below main cable work platform support with an overlay portion connecting a pair of sections of the deck and covering a horizontal bar of the below main cable work platform support.
FIG. 7A is a dynamic perspective view of a further example embodiment of a below main cable work platform support in place on a bridge main cable, the support having a pair of horizontal bars.
FIG. 7B is a side elevational view in cross section of another example embodiment of the below main cable work platform support in place on a pair of twin bridge main cables.
The present disclosure now will be described more fully hereinafter with reference to the accompanying drawings, which show various example embodiments. However, the present disclosure may be embodied in many different forms and should not be construed as limited to the example embodiments set forth herein. Rather, these example embodiments are provided so that the present disclosure is thorough, complete and fully conveys the scope of the present disclosure to those skilled in the art.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1A illustrates a below main cable work platform support 10 , hereafter referred to as a platform support, in place on a bridge main cable 100 . The bridge main cable is one of several suspension main cables suspended between a plurality of towers. A plurality of vertical suspender cables hang off the main cables, the main cables and suspender cables bearing the load-bearing portion of the bridge called the deck. The below main cable work platform support supports a below main cable work platform when the platform is in a position for performing maintenance work on the main cable of the suspension bridge. The below main cable work platform allows maintenance work on the main cable to occur without shutting a portion of the bridge deck to traffic.
In this disclosure, a method of attaching and supporting a particular style of work platform will be discussed. However, it is understood that the method and the support can be applied to many types of platforms and scaffolding for use on a suspension bridge main cable and it not limited to the particular structure or use shown in the illustrations.
The support has a pair of struts 14 and a horizontal bar 12 connecting the struts. Each strut has a top end 14 T and a bottom end 14 B. The horizontal bar 12 has a top and a pair of opposing end portions 12 E. The bottom end 14 B of each strut attaches to the horizontal bar 12 substantially towards an opposing end portion 12 E of the bar, a strut coupled to each end forming an isosceles triangle with the main cable at the apex of the triangle. In one embodiment, as shown in FIG. 1B , the triangle formed by extending imaginary lines from the tops of the struts is an equilateral triangle.
The horizontal bar 12 is further stabilized by a pair of tie-downs 22 , the tie downs attaching to the ends of the bar 12 E and extending downward, attaching to the bridge structure below 118 . The tie-downs 22 and bar 12 form a second isosceles triangle.
Referring again to FIG. 1A , the top 14 T of each strut attaches to a plate 16 that fits snugly against the a band on the main cable. The band has a pair of opposing sides, one plate fastening to each opposing side of the band. The strut and plate fasten to the band by a single bolt.
The horizontal bar 12 hangs between a pair of suspender cables 102 . A temporary strap 20 straddling the band and attaching to the horizontal bar is in place to stabilize the support during installation. The temporary strap temporarily distributes the decking section load without disrupting the main cable load. Disruption of the load on a suspension bridge can have catastrophic results. The temporary strap helps to prevent the disruption during the installation of the work platform supports and work platform.
In the illustration, a plurality of cord guides 18 are on the top of the horizontal bar 12 for placing a plurality of cords of the work platform prior to clamping and installing the work platform. The cord guides 18 govern a plurality of cords 116 . A plurality of clamps 122 fastened to the cord guides, one clamp on each cord guide after one cord of the decking section is placed through the cord guide, the cords operative for hanging a decking section of a below main cable work platform. In one example embodiment, the clamp is a U-clamp. It is understood that substituting other types of fastening systems are possible with this support 10 operative for hanging other structures, scaffolding and platforms from the main cable.
As illustrated in FIG. 3 , a plurality of work platform supports 10 are installed on the bands 104 before a plurality of decking sections are installed, the horizontal bar 12 between each pair of suspender cables 102 .
The system for maintaining a main cable on a suspension bridge without shutting a portion of the suspension bridge to traffic is illustrated in FIG. 3 . A plurality of supports 10 are fastened to a plurality of bands 104 on the main cable, each band having at least one support, the horizontal bar 12 of each support between each pair of suspender cables 102 on each band.
Each support has a pair of plates fastened to the each band as explained hereinabove as shown in FIG. 1A .
As shown in FIG. 4 , a plurality of decking sections 114 hang from cords 116 in the cord guides of the horizontal bars, each decking section having an opposing edge 114 E abutting the opposing edge of an adjacent decking section, forming a continuous platform 120 below the entirety of the main cable.
The system has clamps 122 fastened to the cord guides 18 , as shown in FIG. 1A , one clamp on each cord guide after one cord 116 of the decking section is placed through the cord guide. Note the drawing shows the cords in a slack state for purposes of illustration, but generally are in a taut state resulting from the weight of the decking section.
As shown in FIG. 6 , an overlay decking portion 112 covers each horizontal bar 12 , providing an uninterrupted surface on the continuous platform 120 below the main cable. The overlay decking portion also covers the cord guides and secures the clamped cords of the platform decking sections.
FIG. 7A demonstrates another example embodiment of the work platform support 10 . A pair of supports 10 is fastened to each band 104 through one pair of plates 16 . The support has two pairs of struts 14 , each coupled to one horizontal bar 12 of a pair of horizontal bars 12 , the horizontal bars on the outside of the suspender cables 102 .
As shown in FIG. 7B , in one example embodiment, the bridge has a pair of twin main cables 100 in parallel on each side of the bridge. The below main cable work platform support 10 has the plates 16 and struts 14 coupled to bands 104 on each main cable, the struts 14 on the two cables coupled to one horizontal bar 12 . The below main cable work platform 120 is supported on the work platform support 10 as described hereinabove.
The method of attaching the support is described in detail hereinbelow. FIG. 5 shows a novel step of the method. On each band 104 on the main cable, are a pair of side bolts 106 , one on each side. Coupled to the side bolts are hand rope supports 110 that extending vertically above. Each bolt is temporarily removed and the plate 16 is coupled to the bolt 106 and hand rope support 110 when the bolt is replaced. The top of the strut 14 T is coupled to the plate 16 below the bolt 106 . A temporary strap 20 is placed over the band 104 to stabilize the support during installation. Balancing the load throughout the bridge structure at all times is critical and the method requires temporary stabilization until installation is complete.
FIG. 2 shows a hand rope 108 and the hand rope supports 110 extending above each band on the main cable. The hand rope and hand rope supports are pre-existing structures that are present prior to the installation of the below main cable work platform supports 10 and a below main cable work platform 120 . Without the below main cable work platform, workers walk on top of the cable, using the hand rope for support. Without the below main cable work platform, cable maintenance can only be performed when traffic on the deck below is prohibited, either causing tie-ups or having the work performed on off-peak hours.
Referring to FIG. 1 A, the method of installing the below main cable work platform support 10 in place on a bridge main cable comprises removing the bolt 106 coupling the hand rope support 110 to the main cable band 104 and reattaching the bolt with the hand rope and the plate 16 as described hereinabove. The top of a first strut 14 T on the support 10 is coupled to one plate 16 and the top of a second strut us coupled to one plate on an opposing side. In one embodiment, the horizontal bar 12 is coupled to the bottoms 14 B of the first and second strut 14 prior to coupling the struts to the plates 16 and in another embodiment, the bar 12 is coupled to the struts 14 after the struts are in place on the plates on the band.
The support 10 is stabilized by at least one temporary strap 20 . Decking portions are coupled to the fastening means on the horizontal bar. In FIG. 1A , as a non-limiting example, cord guides 18 are on the horizontal bar and cords are placed in the guides and clamped in place. Gaps in the decking are covered by overlay portions 112 as shown in FIG. 6 . As shown in FIG. 1B , the horizontal bar 12 is further stabilized by a pair of tie-downs 22 , the tie downs attaching to the ends of the bar 12 E and extending downward, attaching to the bridge structure below 118 . Once the decking section 112 and tie-downs are installed, the temporary strap can be removed.
Once the supports 10 are coupled to the each band 104 on the main cable 110 , as shown in FIG. 3 , the platform deck or other structures can be installed. FIG. 4 shows a plurality of decking sections 112 having a plurality of planks connected by a plurality of cords 116 . In this embodiment, the cords of the deck 120 are placed in the cord guides 18 and clamped in place. As explained hereinabove, other configurations of decking and scaffolding structures with different fastening means are possible within the inventive concept.
FIG. 6 shows an overlay decking portion 112 covering the horizontal bar 12 of the support, to cover a gap for safety reasons and to protect the cords in the cord guides.
It is understood that when an element is referred hereinabove as being “on” another element, it can be directly on the other element or intervening elements may be present therebetween. In contrast, when an element is referred to as being “directly on” another element, there are no intervening elements present.
Moreover, any components or materials can be formed from a same, structurally continuous piece or separately fabricated and connected.
It is further understood that, although ordinal terms, such as, “first,” “second,” “third,” are used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms are only used to distinguish one element, component, region, layer or section from another element, component, region, layer or section. Thus, “a first element,” “component,” “region,” “layer” or “section” discussed below could be termed a second element, component, region, layer or section without departing from the teachings herein.
Spatially relative terms, such as “beneath,” “below,” “lower,” “above,” “upper” and the like, are used herein for ease of description to describe one element or feature's relationship to another element(s) or feature(s) as illustrated in the figures. It is understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as “below” or “beneath” other elements or features would then be oriented “above” the other elements or features. Thus, the example term “below” can encompass both an orientation of above and below. The device can be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Example embodiments are described herein with reference to cross section illustrations that are schematic illustrations of idealized embodiments. As such, variations from the shapes of the illustrations as a result, for example, of manufacturing techniques and/or tolerances, are to be expected. Thus, example embodiments described herein should not be construed as limited to the particular shapes of regions as illustrated herein, but are to include deviations in shapes that result, for example, from manufacturing. For example, a region illustrated or described as flat may, typically, have rough and/or nonlinear features. Moreover, sharp angles that are illustrated may be rounded. Thus, the regions illustrated in the figures are schematic in nature and their shapes are not intended to illustrate the precise shape of a region and are not intended to limit the scope of the present claims.
In conclusion, herein is presented a below main cable work platform support. The disclosure is illustrated by example in the drawing figures, and throughout the written description. It should be understood that numerous variations are possible, while adhering to the inventive concept. Such variations are contemplated as being a part of the present disclosure. | A below main cable work platform support for hanging a work platform below a main cable of a suspension bridge and a method of installation thereof. A plurality of supports attach to each band on a main cable. Each support has a pair of struts bolted to the band, the top of each strut on each side of the band, the struts extending downward, connecting to the ends of a horizontal bar that sits between a pair of suspender cables hanging from each band. A work platform is suspended from the horizontal bar and tie down cables extend downward from the bar attaching below to stabilize the platform against wind and uplift. The method includes the step of screwing a single bolt into each side of a cable band for supporting the support therebelow. | 4 |
FIELD OF THE INVENTION
[0001] This invention relates to a novel process of preparing certain hydrolyzable silylated polymers, particularly alpha-substituted alkyl alkoxy silyl-terminated polymers, by reacting a certain silylorganohalide, particularly an alpha-substituted haloalkylalkoxysilane, with a salt of cyanate in the presence of active hydrogen-functional polymers.
BACKGROUND OF THE INVENTION
[0002] Hydrolyzable silylated polymers are useful to make room temperature and moisture curable compositions, such as coatings, adhesives, gaskets, sealants and the like. Inherently fast moisture cure characteristics of alpha-substituted alkyl hydrolyzable silyl-terminated polyurethane polymers, in comparison to their gamma-substituted counterparts, make them desirable, as they potentially allow the use of lesser amounts of environmentally hazardous tin catalysts and offer Hazardous Air Pollutants (HAPs) free curing compositions.
[0003] The preparation of hydrolyzable silylated polymers is generally known in the art. A commonly used commercial method for making hydrolyzable silylated polymers generally involves two steps. The first step comprises the synthesis of isocyanato-substituted hydrolyzable silane by heating the corresponding carbamato-functional hydrolyzable silane at elevated temperatures and under reduced pressures. This step requires the inefficient and costly cracking of the carbamato-functional silane in specialized reactors that allow for the parallel and efficient separation of thereby formed isocyanato-functional silane from its reactants and byproducts, and subsequent purification. Due to high reactivity of the isocyanato-substituted silanes, special care is required to prevent the polymerization of the isocyanato group and hydrolysis of the silyl group during storage of these materials, prior to use. In the second step, the isocyanato-functional silane is reacted with active hydrogen containing polymers, such as polyols, in a differently configured reactor.
[0004] Inventively, it has now been discovered that, one can make hydrolyzable silylated polymers in one-step, without the need to first make, purify and store the isocyanato-functional silanes and subsequently to react them with corresponding active hydrogen-functionalized polymers.
SUMMARY OF THE INVENTION
[0005] The present invention provides a process for making moisture curable and hydrolyzable silylated polymer which comprises reacting under substantially anhydrous conditions (a) at least one hydrolyzable halohydrocarbylsilane, (b) at least one salt of a cyanate, and (c) at least one active hydrogen containing polymer, and, optionally, at least one catalyst and/or inert solvent, and, optionally, at elevated temperatures.
[0006] The hydrolyzable silylated polymers of the present invention make them suitable for coatings, adhesives and sealants in the applications of construction, automotive, marine, aerospace, consumer and industry.
DETAILED DESCRIPTION OF THE INVENTION
[0007] The present invention is directed to a new one-step process of making hydrolyzable silylated polymers. In this inventive process, “in-situ” generated isocyanatohydrocarbylsilane which is obtained by the reaction of halohydrocarbylsilane containing at least one hydrolyzable group with a salt of cyanate, reacts with an active hydrogen polymer, optionally in an organic solvent and/or in the presence of catalysts and optionally at elevated temperatures, to obtain a hydrolyzable silylated polymer.
[0008] The one-step process of making hydrolyzable silylated polymers involves in-situ trapping of the isocyanatohydrocarbylsilane, generated by the reaction of halohydrocarbylsilane with a salt of cyanate optionally in an organic solvent, by the hydrogen active polymers and more specifically hydroxyl-functional polymers.
[0009] As such, the present process can utilize different types of active hydrogen containing polymers. In one embodiment, these active hydrogen containing polymers include hydroxyl-functional polymers such as the non-limiting examples of polyethylene glycol of various molecular weights; polypropylene glycols of various molecular weights; polyols based upon alpha-substituted glycols, such as polybutylene glycol, polyhexylene glycol, and the like; polyurethanes formed by reacting polypropylene glycols, polyethylene glycols, copolymers of polyethylene glycol and polypropylene glycol and the like; copolymers of polyethylene glycol and polypropylene glycol; polyester polyols; polycarbonate polyols; polybutadiene diols; polycaprolactone diols; silanol; aliphatic diols with siloxane backbone; triols and higher functionality polyols, such as tetraols and pentaols; any other active hydrogen containing compounds such as primary and secondary amines, e.g., Jeffamine (amine terminated polypropylene glycol); and carboxylic acids and the like, can be used in this reaction.
[0010] In another embodiment, suitable polyols include polyether polyol, polyetherester polyols, polyesterether polyols, polybutadiene polyols, acrylic component-added polyols, acrylic component-dispersed polyols, styrene-added polyols, styrene-dispersed polyols, vinyl-added polyols, vinyl-dispersed polyols, urea-dispersed polyols, and polycarbonate polyols, polyoxypropylene polyether polyol, mixed poly (oxyethylene/oxypropylene) polyether polyol, polybutadienediols, polyoxyalkylene diols, polyoxyalkylene triols, polytetramethylene glycols, polycaprolactone diols and triols, and mixtures of polyols of varying active hydrogen content, such as monols, diols, triols and higher functionality polyols.
[0011] In still another embodiment, specific non-limiting examples of polyether polyols are polyoxyalkylene polyol, particularly linear and branched poly (oxyethylene) glycol, poly (oxypropylene) glycol, copolymers of the same and combinations thereof. Graft or modified polyether polyols, typically called polymer polyols, are those polyether polyols having at least one polymer of ethylenically unsaturated monomers dispersed therein. Non-limiting representative modified polyether polyols include polyoxypropylene polyether polyol into which is dispersed poly (styrene acrylonitrile) or polyurea, and poly (oxyethylene/oxypropylene) polyether polyols into which is dispersed poly (styrene acrylonitrile) or polyurea. Graft or modified polyether polyols comprise dispersed polymeric solids. Suitable polyesters of the present invention, include but are not limited to aromatic polyester polyols such as those made with phthalic anhydride (PA), dimethylterephthalate (DMT) polyethyleneteraphthalate (PET) and aliphatic polyesters, and the like. In one embodiment of the present invention, the polyether polyol is selected from the group consisting of ARCOL® polyol U-1000, Hyperlite® E-848 from Bayer AG, ACCLAIM® 8200 and 12200 from Bayer AG, Voranol® Dow BASF, Stepanpol® from Stepan, Terate® from Invista and combinations thereof.
[0012] Similarly, hydroxyl group terminated polyurethanes obtained by reacting different polyols as listed herein above, with different diisocyanates and/or polyisocyanates, such as the non-limiting examples of diisocyanates such as 2,4-toluene diisocyanate (TDI), 2,6-toluene diisocyanate, 4,4′-diphenyl-methanediisocyanate (MDI), 2,4′-diphenyl-methanediisocyanate, isophorone diisocyanate (“IPDI”), 4,4′-dicyclohexylmethane-diisocyanate isomers, hexamethylene diisocyanate (HDI), Desmodur N and the like, and mixtures thereof.
[0013] The molecular weight of the polyols or hydroxyl-terminated polyurethanes is specifically in the range between 300 and 25,000 grams per mole, more specifically between 1,000 and 16,000 grams per mole, even more specifically between 5,000 and 14,000 grams per mole and most specifically between 8,000 and 12,000 grams mole, as measured by gel permeation chromatography, against polystyrene standards.
[0014] To prepare active hydroxyl-terminated polyurethanes useful in this invention, at least a slight molar excess of the hydroxyl equivalents (—OH groups) with respect to the isocyanato equivalents (—NCO groups) is employed to terminate the polymer chains with hydroxyl groups. The specific molar ratio of the NCO to OH is from about 0.2 to 0.95, and more specifically between 0.5 and 0.85, depending on the polyol in use.
[0015] In one embodiment herein, the reactant employed in the practice of this present invention to prepare the hydroylsable silylated polymer is one or more hydrolyzable halo-substituted hydrocarbylsilane according to Formula (1):
[0000] YG 1 SiX 1 X 2 X 3 (1)
[0000] wherein:
[0016] each occurrence of Y is independently selected from the group consisting of chloro, bromo and iodo;
[0017] each occurrence of G 1 is independently a divalent hydrocarbylene group, optionally containing heteroatom-substituted with one or more oxygen atoms, and selected from the group comprising alkylene, alkenylene and aralkylene containing from 1 to 20 carbon atoms;
[0018] each occurrence of X 1 is independently a hydrolyzable group selected from the group consisting of R 1 O—, R 1 C(═O)O—, R 1 R 2 C═NO—, and R 1 R 2 NO—, wherein each occurrence of R 1 , R 2 and R 3 is independently a monovalent hydrocarbyl selected from the group consisting of hydrogen, and alkyl, alkenyl, aryl, and aralkyl containing from 1 to 10 carbon atoms;
[0019] each occurrence of X 2 is independently selected from the group consisting of R 1 O—, R 1 C(═O)O—, R 1 R 2 C═NO—, R 1 R 2 NO— and R 3 —, wherein each occurrence of R 1 , R 2 and R 3 is independently a monovalent hydrocarbyl selected from the group consisting of hydrogen, and alkyl, alkenyl, aryl, and aralkyl containing from 1 to 10 carbon atoms; and
[0020] each occurrence of X 3 is independently selected from the group consisting of R 1 O—, R 1 C(═O)O—, R 1 R 2 C═NO—, R 1 R 2 NO— and R 3 —, wherein each occurrence of R 1 , R 2 and R 3 is independently a monovalent hydrocarbyl selected from the group consisting of hydrogen, and alkyl, alkenyl, aryl, and aralkyl containing from 1 to 10 carbon atoms.
[0021] In one embodiment, specific non-limiting examples of Y are Cl—, Br— and I—, more specifically Br— and Cl—, and most specifically Cl—.
[0022] In another embodiment, the G 1 is specifically a hydrocarbylene group in which the carbon atom that is substituted with the Y group is a primary carbon atom. In still another embodiment, when the G 1 groups contains at least two carbon atoms, the carbon atom adjacent to the carbon containing the Y group contains at least one hydrogen and more specifically two hydrogen atoms. In yet another embodiment, specific non-limiting examples of G 1 include alkylene, such as methylene, ethylene, propylene, butylenes, 3-methyl pentylene, bis-(ethylene)cyclohexane; alkenylene such as —CH 2 CH═CH—, —CH 2 CH═CHCH 2 —, —CH 2 CH 2 CH(CH 3 )═CH 2 CH 2 —; aralkylene, such as —CH 2 CH 2 C 6 H 4 CH 2 CH 2 —, —CH 2 CH 2 OC 6 H 4 OCH 2 CH 2 —, wherein C 6 H 4 represents a phenylene group, and the like.
[0023] In another embodiment, X 1 is R 1 O— including the specific non-limiting examples of methoxy, ethoxy, isopropoxy, propoxy, butoxy and more specifically methoxy and ethoxy.
[0024] In yet another embodiment, X 2 and X 3 are selected from the group consisting of R 1 O—, including the specific non-limiting examples of methoxy, ethoxy, isopropoxy, propoxy, butoxy and more specifically methoxy and ethoxy; and R 3 —, including the specific non-limiting examples of methyl, ethyl, propyl, phenyl, 2-phenylethyl and more specifically methyl and ethyl.
[0025] In one embodiment of the present invention the hydrolyzable alpha-chloromethylsilanes suitable to use is at least one selected from the group consisting of chloromethyltriethoxysilane, chloromethyltrimethoxysilane, chloromethyltripropoxysilane, chloromethyldiethoxymethylsilane, chloromethyldimethoxymethylsilane, chloromethyldipropyloxymethylsilane, chloromethylethoxydimethylsilane, chloromethylmethoxydimethylsilane and mixtures thereof.
[0026] In another embodiment of the present invention, the hydrolyzable halohydrocarbylsilane suitable to use is at least one selected from the group consisting of 2-chloroethyltriethoxysilane, 3-chloropropyltrimethoxysilane, 6-chlorohexyltripropoxysilane, 2-chloroethyldiethoxymethylsilane, 3-chloropropyldimethoxymethylsilane, 4-(2-chloroethyl)phenyldipropyloxymethylsilane, 2-chloroethylethoxydimethylsilane, 3-chloropropylmethoxydimethylsilane and mixtures thereof.
[0027] The time necessary to cure the hydrolyzable silylated polymers is dependent in part upon the structure of the G 1 group. The hydrolyzable silylated polymers that contain only a single carbon atom between the silicon atom and the nitrogen atom of the carbamate functional group hydrolyze much more rapidly than when two or more carbon or oxygen atoms separate the silicon atom and nitrogen atom. Divalent hydrocarbylene G 1 groups that are cyclic or branch further slow down the curing rate. In an embodiment, mixtures of hydrolyzable halohydrocarbylsilanes can be used in the method for preparing hydrolyzable silylated polymers to achieve desirable curing rates. Specific non-limiting examples of the reactants include mixtures of chloromethyltrimethoxysilane and 3-chloropropyltrimethoxysilane, chloromethyltrimethoxysilane and 5-chloro-3-methylpentyltrimethoxysilane, chloromethyltrimethoxysilane and 2-chloroethylyltrimethoxysilane and the like. The molar ratios of haloalkylsilanes in which G 1 is one carbon to haloalkylsilanes in which G 1 is 2 to 30 carbon atoms is from about 95 to 5, more specifically from about 80 to 20 and most specifically from about 80 to 60. In another embodiment, hydrolyzable silylated polymers containing different G 1 groups can be mixed together.
[0028] According to another embodiment of the process of this invention, another reactant of the process of the present invention is a salt of cyanate, which is reacted with the hydrolyzable halohydrocarbylsilane in the presence of an active hydrogen containing polymer to produce a hydrolyzable silylated polymer. The cyanates which may be employed in the practice of this invention are metal cyanates, for example, but not limited thereto, lithium, sodium, potassium, rubidium, barium, strontium, silver, lead, mercury, calcium cyanates, and the like, and ammonium cyanate and phosphonium cyanate. According to one specific embodiment of the process of the invention, the cyanate is potassium cyanate.
[0029] In another embodiment of this invention, the novel process is employed to produce an hydrolyzable silylated polymer by reacting a salt of cyanate, with a hydrolyzable halohydrocarbylsilane and an active hydrogen containing polymer, such as the non-limiting example of a hydroxyl-functional polymer, in the presence of a phase-transfer catalyst at elevated temperatures and either at a controlled rate of reaction or controlled reaction conditions such as reaction temperature and catalyst amount.
[0030] Examples of phase transfer catalysts include quaternary phosphonium salts such as tetra-n-butylphosphonium bromide, tetra-n-butylphosphonium chloride, methyltri-n-butylphosphonium chloride, methyltri-n-butylphosphonium bromide, n-butyltriphenylphosphonium bromide, n-butyltriphenylphosphonium chloride, methyltriphenylphosphonium chloride and methyltriphenylphosphonium bromide, with particular preference being given to methyltriphenylphosphonium chloride, n-butyltriphenylphosphonium bromide and tetra-n-butylphosphonium bromide.
[0031] According to another embodiment of the invention, the novel process to produce a hydrolyzable silylated polymer can be carried out in the presence or absence of an organic solvent, but use of an organic solvent, in particular a polar aprotic solvent, is preferred. When an organic solvent is used, the amount is preferably from 100 to 1000 percent by weight, more preferably from 20 to 800 percent by weight, and most preferably from 400 to 600 percent by weight, in each case based on the amount of hydrolyzable halocarbylsilane compound supplied.
[0032] Examples of organic, polar aprotic solvents include those which aid the reaction, for instance acetone, N,N-dimethylformamide, dimethyl sulfoxide, N-methyl-2-pyrrolidone, gamma-butyrolactone, diethylene glycol dimethyl ether and diethylene glycol diethyl ether, with preference being given to acetone, N,N-dimethylformamide and N-methyl-2-pyrrolidone, most preferably N,N-dimethylformamide.
[0033] According to one specific embodiment of the invention, the solvent is dimethylformamide.
[0034] According to an embodiment of the invention, the novel process to produce a hydrolyzable silylated polymer is carried out either at room temperature or at elevated temperatures from about 80 to about 140° C. In another embodiment of the invention, the process is carried out at a temperature from about 90 to about 120° C. In yet another embodiment of the invention, the process is carried out at a temperature from about 100 to about 110° C.
[0035] Additional catalyst can be employed in the process of the present invention. Suitable additional catalysts include organoamine and organotin compounds for this purpose. Other metal catalysts can be used in place of, or in addition to, organotin compound. Suitable non-limiting examples of additional catalysts include tertiary amines such as bis(2,2′-dimethylamino)ethyl ether, trimethylamine, triethylenediamine, 1,8-diazabicyclo[5.4.0]undec-7-ene, triethylamine, N-methylmorpholine, N,N-ethylmorpholine, N,N-dimethylbenzylamine, N,N-dimethylethanolamine, N,N,N′,N′-tetramethyl-1,3-butanediamine, pentamethyldipropylenetriamine, triethanolamine, triethylenediamine, 2-{[2-(2-dimethylaminoethoxy)ethyl]methylamino}ethanol, pyridine oxide, and the like; strong bases such as alkali and alkaline earth metal hydroxides, alkoxides, phenoxides, and the like; acidic metal salts of strong acids such as ferric chloride, stannous chloride, antimony trichloride, bismuth nitrate and chloride, and the like; chelates of various metals such as those which can be obtained from acetylacetone, benzoylacetone, trifluoroacetylacetone, ethyl acetoacetate, salicylaldehyde, cyclopentanone-2-carboxylate, acetylacetoneimine, bis-acetylaceone-alkylenediimines, salicylaldehydeimine, and the like, with various metals such as Be, Mg, Zn, Cd, Pb, Ti, Zr, Sn, As, Bi, Cr, Mo, Mn, Fe, Co, Ni, or such ions as MoO 2 ++, UO 2 ++, and the like; alcoholates and phenolates of various metals such as Ti(OR) 4 , Sn(OR) 4 , Sn(OR) 2 , Al(OR) 3 , and the like, wherein R is alkyl or aryl of from 1 to about 12 carbon atoms, and reaction products of alcoholates with carboxylic acids, beta-diketones, and 2-(N,N-dialkylamino)alkanols, such as well known chelates of titanium obtained by this or equivalent procedures; salts of organic acids with a variety of metals such as alkali metals, alkaline earth metals, Al, Sn, Pb, Mn, Co, Bi, and Cu, including, for example, sodium acetate, potassium laurate, calcium hexanoate, stannous acetate, stannous octoate, stannous oleate, lead octoate, metallic driers such as manganese and cobalt naphthenate, and the like; organometallic derivatives of tetravalent tin, trivalent and pentavalent As, Sb, and Bi, and metal carbonyls of iron and cobalt; and combinations thereof. In one specific embodiment organotin compounds that are dialkyltin salts of carboxylic acids, can include the non-limiting examples of dibutyltin diacetate, dibutyltin dilaureate, dibutyltin maleate, dilauryltin diacetate, dioctyltin diacetate, dibutyltin-bis(4-methylaminobenzoate), dibuytyltindilaurylmercaptide, dibutyltin-bis(6-methylaminocaproate), and the like, and combinations thereof. Similarly, in another specific embodiment there may be used trialkyltin hydroxide, dialkyltin oxide, dialkyltin dialkoxide, or dialkyltin dichloride and combinations thereof. Non-limiting examples of these compounds include trimethyltin hydroxide, tributyltin hydroxide, trioctyltin hydroxide, dibutyltin oxide, dioctyltin oxide, dilauryltin oxide, dibutyltin-bis(isopropoxide) dibutyltin-bis(2-dimethylaminopentylate), dibutyltin dichloride, dioctyltin dichloride, and the like, and combinations thereof.
[0036] In accordance with one embodiment of the present invention, one and two-part sealant, adhesive or coating formulations incorporating the above hydrolsable silylated polymer can be prepared by mixing together the silylated polymer and any of the customary functional additives known to those skilled in the art, such as one or more fillers, plasticizers, thixotropes, antioxidants, U.V. stabilizers, surfactants, defoamers, adhesion promoter(s) and/or cure catalyst.
[0037] Commercial incorporation of the moisture-curable polymer of the present invention include various forms of construction, automotive applications, consumer applications, industrial application, industrial assembly, polyurethane foams, e.g., as used for the insulation for roofs, tanks and pipes, transportation applications, e.g., RV's, subway cars, trailers and the like.
[0038] The components used in the inventive process can mixed with one another in any order. After the reaction has reached the desired degree of completion, the resulting hydrolyzable silylated polymer can be isolated and purified by methods known per se, i.e. by filtration, concentration by distillation, dilution with co-solvents, filtration and distillation.
[0039] In the following examples, all parts and percentages are, by weight, unless indicated otherwise, and are carried out at the pressure of the surrounding atmosphere, i.e. at about 1,000 hPa, and at a temperature usually performed in the range of 90-120° C. for a time period of 10-24 hrs. All viscosities reported in the examples are as measured at a temperature of 25° C. All reactions described in the examples were carried out under an inert gas atmosphere comprising nitrogen.
EXAMPLE 1
Synthesis of Alpha-Substituted Silyl-Terminated Polypropylene Glycol
[0040] A solution/dispersion of 5.0 g chloromethyltrimethoxysilane, 2.9 g of potassium cyanate and 6.25 g of polypropylene glycol (Mn˜425, available from Aldrich) in dry dimethylformamide (25 ml) was heated gradually from 90 to 120° C. and allowed to reflux for 24 hours. The reaction is performed with addition of 50 ppm tin catalyst, dibutyltin dilaurate (DBTDL), after 6 hrs from the start of the reaction. Subsequently, the mixture was cooled to room temperature, filtered and concentrated. To this concentrated solution, toluene (100 ml) was added and the precipitated salt was filtered. The solvent was subsequently removed under vacuum to get alpha silyl terminated polypropylene glycol. The composition of the product was confirmed by FT-IR and FT-NMR analyses.
EXAMPLE 2
Synthesis of Alpha-Substituted Silyl Terminated Polypropylene Glycol
[0041] The procedure described in Example-1 was performed with chloromethyltriethoxysilane, in place of chloromethyltrimethoxysilane.
EXAMPLE 3
Synthesis of Alpha-Substituted Silyl-Terminated Polypropylene Glycol
[0042] The procedure described in Example-1 was performed with chloromethylmethyldimethoxysilane, in place of chloromethyltrimethoxysilane.
EXAMPLE 4
Synthesis of Alpha-Substituted Silyl-Terminated Polypropylene Glycol
[0043] The procedure described in Example-1 was performed with chloromethylmethyldiethoxysilane, in place of chloromethyltrimethoxysilane.
EXAMPLE 5
Synthesis of Gamma-Substituted Silyl-Terminated Polypropylene Glycol
[0044] (Method-1) A solution/dispersion of 5.8 g chloropropyltrimethoxysilane, 2.8 g of potassium cyanate and 6.2 g of polypropylene glycol (Mn˜425, procured from Aldrich) in dry dimethylformamide (25 ml) was heated gradually from 90-120° C. and allowed to reflux for 24 hours. The reaction is performed with addition of 50 ppm tin catalyst (dibutyltin dilaurate (DBTDL) after 6 hrs from the start of the reaction. Subsequently, the mixture was cooled to room temperature, filtered and concentrated. To this concentrated solution, toluene (100 ml) was added and the precipitated salt was filtered. The solvent was subsequently removed under vacuum to get gamma silyl terminated polypropylene glycol. The composition of the product was confirmed by FT-IR and FT-NMR analysis.
COMPARATIVE EXAMPLE 1
Synthesis of Gamma-Substituted Silyl-Terminated Polypropylene Glycol
[0045] (Method-2) A mixture of 10.0 g of polypropylene glycol (available from Aldrich, Mn˜425), 9.64 g of isocyanatopropyltrimethoxysilane (available from GE-Silicones, Trade name: A link-35) and 50 ppm of tin catalyst (dibutyltin dilaurate (DBTDL) taken in a RB flask fitted with a condenser and a magnetic stirrer was stirred under nitrogen atmosphere at 80 to 85° C. for 5 hr to get the desired product. The composition of the product was confirmed by FT-IR and FT-NMR analysis.
EXAMPLE 6
Synthesis of Alpha-Substituted Silyl-Terminated Polypropylene Glycol
[0046] The procedure described in Example-1 was performed with required mole equivalent of polypropylene glycol (Mn˜2700, available from Aldrich), instead of polypropylene glycol (Mn˜425).
COMPARATIVE EXAMPLE 2
Synthesis of Gamma-Substituted Silyl-Terminated Polypropylene Glycol
[0047] The procedure described in Comparative Example-1 was performed with required mole equivalent of polypropylene glycol (Mn˜2700, available from Aldrich), instead of polypropylene glycol (Mn˜425).
EXAMPLE 7
Synthesis of Alpha-Substituted Silyl-Terminated Polyurethane
[0048] The procedure described in Example-1 was performed with required mole equivalent of hydroxyl group terminated polyurethane obtained by reacting mole excess of polypropylene glycol (Mn˜425, available from Aldrich) with isoprone diisocyante (available from Aldrich), instead of polypropylene glycol.
EXAMPLE 8
Synthesis of Alpha-Substituted Silyl-Terminated Polyurethane
[0049] The procedure described in Example-7 was performed with required mole equivalent of chloromethyltriethoxysilane, instead of chloromethyltrimethoxysilane.
EXAMPLE 9
Synthesis of Alpha-Substituted Silyl-Terminated Polyurethane
[0050] The procedure described in Example-1 was performed with required mole equivalent of hydroxyl group terminated polyurethane obtained by reacting mole excess of polypropylene glycol (Mn˜2700, available from Aldrich) with isoprone diisocyante (available from Aldrich), instead of polypropylene glycol.
EXAMPLE 10
Synthesis of Gamma-Substituted Silyl-Terminated Polyurethane
[0051] The procedure described in Example-5 (Method-1) was performed with required mole equivalent of hydroxyl group terminated polyurethane obtained by reacting mole excess of polypropylene glycol (Mn˜425, available from Aldrich) with isoprone diisocyante (available from Aldrich), instead of polypropylene glycol.
COMPARATIVE EXAMPLE 3
Synthesis of Gamma-Substituted Silyl-Terminated Polyurethane
[0052] The procedure described in Comparative Example-1 (Method-2) was performed with required mole equivalent of hydroxyl group terminated polyurethane obtained by reacting mole excess of polypropylene glycol (Mn˜425, available from Aldrich) with isoprone diisocyante (available from Aldrich), instead of polypropylene glycol.
COMPARATIVE EXAMPLE 4
Synthesis of Gamma-Substituted Silyl-Terminated Polyurethane
[0053] The procedure described in Comparative Example-1 (Method-2) was performed with required mole equivalent of hydroxyl group terminated polyurethane obtained by reacting mole excess of polypropylene glycol (Mn˜2700, available from Aldrich) with isoprone diisocyante (available from Aldrich), instead of polypropylene glycol
EXAMPLES 11-18, COMPARATIVE EXAMPLES 5-8
[0054] The utility of the hydrolyzable silylated polymers was demonstrated by measuring the tack-free times. The procedure involved casting a film using a film applicator that was 2.5 mm (0.1 inch) thick and recording the time under ambient temperature and humidity, about 25° C. and 50 percent relative humidity, when the film was no longer tacky to the touch using an index finger. The results are presented in Table 1.
[0055] Table 1: Tack-free times for the silylated polymers of the present invention.
[0000]
TABLE 1
Catalysts
Tack-free
Silylated Polymer
concentration, ppm
time,
Example No.
from Example No.
(dibutyltin dilaurate)
minutes
EXAMPLE 11
EXAMPLE 1
50
5
EXAMPLE 12
EXAMPLE 2
50
78
EXAMPLE 13
EXAMPLE 6
50
2,880
EXAMPLE 14
EXAMPLE 7
50
30
EXAMPLE 15
EXAMPLE 8
50
1,440
EXAMPLE 16
EXAMPLE 9
50
1,080
EXAMPLE 17
EXAMPLE 5
50
7,200
COMPARATIVE
COMPARATIVE
50
7,200
EXAMPLE 5
EXAMPLE 1
COMPARATIVE
COMPARATIVE
50
31,700
EXAMPLE 6
EXAMPLE 2
EXAMPLE 18
EXAMPLE 10
1000
5,760
COMPARATIVE
COMPARATIVE
1000
5,760
EXAMPLE 7
EXAMPLE 3
COMPARATIVE
COMPARATIVE
1000
7,200
EXAMPLE 8
EXAMPLE 4
[0056] While the process of the invention has been described with reference to certain embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out the process of the invention but that the invention will include all embodiments falling within the scope of the appended claims. | An improved process for preparing hydrolyzable polymers, the process includes, inter alia, reacting certain silylorganohalide compounds with a salt of a cyanate in the presence of active hydrogen containing polymers. | 2 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a cleaning method and a polishing apparatus employing such cleaning method, and more particularly to a cleaning method suitable for cleaning substrates that require a high degree of cleanliness, such as semiconductor wafers, glass substrates, or liquid crystal displays, and to a polishing apparatus employing such cleaning method.
[0003] 2. Description of the Related Art
[0004] As semiconductor devices have become more highly integrated in recently years, circuit interconnections on semiconductor substrates become finer and the distances between those circuit interconnections have become smaller. One of the processes available for forming such circuit interconnections is photolithography. In the case where circuit interconnections are formed by the photolithography or the like, it requires that surfaces on which patterns images are to be focused by a stepper be as flat as possible because the depth of focus of the optical system is relatively small.
[0005] It is therefore necessary to make the surfaces of semiconductor substrates flat for photolithography. One customary way of flattening the surfaces of the semiconductor substrates is to polish them with a polishing apparatus. As shown in FIG. 8, a conventional polishing apparatus 76 comprises a turntable 72 having a polishing cloth 70 thereon, and a top ring 74 for holding a semiconductor substrate W and pressing the semiconductor substrate W against the turntable 72 . In the polishing apparatus, a chemical mechanical polishing (CMP) of the substrate is performed by a combination of chemical polishing with an abrasive liquid and mechanical polishing with abrasive particles contained in the abrasive liquid. An abrasive liquid supply nozzle 78 is provided above the turntable 72 to supply the abrasive liquid Q to the polishing cloth 70 . Further, a dressing device 80 is provided to regenerate, i.e. dress the polishing cloth 70 .
[0006] [0006]FIG. 9 shows a CMP unit which is constructed as an integral unit having the polishing apparatus 76 shown in FIG. 8 and various devices associated with the polishing apparatus 76 . The CMP unit has a substantially rectangular shape in plan, and the polishing apparatus 76 is disposed at one side of the CMP unit, and load and unload units 84 a , 84 b for placing wafer cassettes which accommodate semiconductor substrates to be polished are disposed at the other side of the CMP unit. Transfer robots 86 a , 86 b are movably provided between the polishing apparatus 76 and the load and unload units 84 a , 84 b so that the transfer robots 86 a , 86 b are movable along a transfer line C. Reversing devices 88 a , 88 b for reversing a semiconductor substrate are disposed at one side of the transfer line C, and cleaning apparatuses 90 a , 90 b , 90 c for cleaning the semiconductor substrate are disposed at the other side of the transfer line C. A pusher 10 is disposed adjacent to the turntable 72 to transfer the semiconductor substrate between the top ring 74 and the pusher 10 by vertical movement thereof.
[0007] In the polishing apparatus 76 having the above structure, the semiconductor substrate W is held by the lower surface of the top ring 74 and pressed against the polishing cloth 70 on the turntable 72 . The abrasive liquid Q is supplied from the abrasive liquid supply nozzle 78 onto the polishing cloth 70 and retained on the polishing cloth 70 . During operation, the top ring 74 exerts a certain pressure on the turntable 72 , and the surface of the semiconductor substrate held against the polishing cloth 70 is therefore polished in the presence of the abrasive liquid Q between the surface of the semiconductor substrate W and the polishing cloth 70 by a combination of chemical polishing and mechanical polishing while the top ring and the turntable are rotated. The abrasive liquid Q contains various abrasive particles, and the pH of the abrasive liquid Q is adjusted in accordance with the kind of semiconductor substrates to be polished.
[0008] As described above, as semiconductor devices have become more highly integrated, circuit interconnections on semiconductor substrates become finer and the distances between those circuit interconnections have become smaller. Therefore, in the above polishing process, if a particle greater than the distance between interconnections adheres to a semiconductor substrate and thus such particle remains on the product, i.e. semiconductor device, then the particle will short-circuit interconnections on the semiconductor device. Therefore, any undesirable particles on the semiconductor substrate have to be sufficiently smaller than the distance between interconnections on the semiconductor substrate. Such a problem and a requirement hold true for the processing of other substrates including a glass substrate to be used as a mask, a liquid crystal panel, and so on.
[0009] In the above-mentioned CMP process, the semiconductor substrate which has been polished is transferred to the cleaning apparatuses 90 a , 90 b and 90 c . In the cleaning apparatuses 90 a , 90 b and 90 c , for example, a scrubbing cleaning process in which a cleaning member such as a brush or a sponge is used to scrub a surface of the semiconductor substrate while supplying a cleaning liquid such as pure water, and a spinning dry process subsequent to the scrubbing cleaning process are performed, and the abrasive particles or the ground-off particles attached to the semiconductor substrate during the polishing process are removed from the semiconductor substrate.
[0010] When pure water (deionized water) is supplied to the semiconductor substrate which has been polished, the pH of the abrasive liquid remaining on the semiconductor substrate changes greatly. Therefore, in some cases, abrasive particles which have been dispersed in the abrasive liquid having an original pH are aggregated together, and adhere to the surface of the semiconductor substrate. For example, in slurry of colloidal silica which is generally used for polishing Sio 2 layer, silica particles which are abrasive particles are stable in alkali solution having a pH of about 10, and form secondary particles having a diameter of about 0.2 μm due to aggregation of primary silica particles. If this slurry is rapidly diluted with pure water to lower the pH of the slurry to 7 or 8, then the electric potential on the surfaces of silica particles is rapidly changed by so-called pH shock, and the silica particles become unstable to thus aggregate the secondary particles to form larger aggregates. In this specification, the pH shock is defined as a rapid change of a pH. This holds true for the dressing process of the polishing cloth 70 . To be more specific, when pure water as a dressing liquid is supplied onto the polishing cloth 70 holding the abrasive liquid Q thereon, the pH of the abrasive liquid is rapidly lowered to cause abrasive particles to aggregate. These aggregates remain on the polishing cloth 70 and cause the semiconductor substrate to form scratches in the polishing process.
SUMMARY OF THE INVENTION
[0011] It is therefore an object of the present invention to provide a cleaning method which can efficiently perform cleaning of substrates which have been polished without causing abrasive particles contained in an abrasive liquid to be aggregated.
[0012] Another object of the present invention is to provide a dressing method which can efficiently perform dressing of a polishing surface on a turntable without causing abrasive particles contained in an abrasive liquid to be aggregated on the polishing surface.
[0013] Still another object of the present invention is to provide a polishing apparatus employing such cleaning method or dressing method.
[0014] According to a first aspect of the present invention, there is provided a method for polishing and then cleaning a substrate, the method comprising: polishing a substrate using an abrasive liquid containing abrasive particles; and cleaning a polished surface of the substrate by supplying a cleaning liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid so that a pH of the abrasive liquid attached to the polished surface of the substrate is not rapidly changed.
[0015] In the present invention, when using silica slurry having a pH of about 10 as an abrasive liquid, the cleaning liquid whose pH is in the range of 9 to 11 may be used.
[0016] According to the present invention, the pH of the abrasive liquid attached to the substrate in the polishing process is not rapidly changed, and hence cleaning of the substrate is conducted in such a state that the abrasive particles are not aggregated due to pH shock. This cleaning process of the substrate is performed in the case where liquid other than the abrasive liquid is first supplied to the surface of the substrate after the polishing process of the substrate. This cleaning process includes rinsing of the substrate on the turntable or in the vicinity of the turntable by supplying a cleaning liquid to the substrate, and a scrubbing cleaning in which the substrate is scrubbed by a cleaning member while supplying a cleaning liquid to the substrate in a cleaning apparatus.
[0017] According to a second aspect of the present invention, there is provided a method for polishing and then cleaning a substrate, the method comprising: polishing a substrate using an abrasive liquid containing abrasive particles; and cleaning a polished surface of the substrate by supplying a cleaning liquid whose pH is changed during the cleaning.
[0018] In a preferred aspect, the pH of the cleaning liquid is changed from acid or alkali to neutrality. Thus, the substrate may be transferred to the next process in a stable neutral condition.
[0019] According to a third aspect of the present invention, there is provided a method for polishing a substrate and then dressing a polishing surface on a turntable, the method comprising: polishing a substrate using an abrasive liquid containing abrasive particles by contacting the substrate with the polishing surface; and dressing the polishing surface by supplying a dressing liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid so that a pH of the abrasive liquid on the polishing surface is not rapidly changed.
[0020] According to the present invention, the polishing surface on the turntable may be dressed in such a state that the abrasive particles are not aggregated on the polishing surface.
[0021] In a preferred aspect, the cleaning liquid or the dressing liquid comprises electrolytic ionic water. Thus, contamination of the substrate caused by metal ion may be prevented and adjustment of the pH of the abrasive liquid may be made.
[0022] According to a fourth aspect of the present invention, there is provided an apparatus for polishing and then cleaning a substrate, the apparatus comprising: a polishing apparatus for polishing a substrate using an abrasive liquid containing abrasive particles; and a cleaning apparatus for cleaning a polished surface of the substrate by supplying a cleaning liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid so that a pH of the abrasive liquid attached to the polished surface of the substrate is not rapidly changed.
[0023] According to a fifth aspect of the present invention, there is provided an apparatus for polishing and then cleaning a substrate, the apparatus comprising: a polishing apparatus for polishing a substrate using an abrasive liquid containing abrasive particles; and a cleaning apparatus for cleaning a polished surface of the substrate by supplying a cleaning liquid whose pH is changed during the cleaning.
[0024] According to a sixth aspect of the present invention, there is provided an apparatus for polishing a substrate and then dressing a polishing surface on a turntable, the apparatus comprising: a polishing apparatus for polishing a substrate using an abrasive liquid containing abrasive particles by contacting the substrate with the polishing surface; and a dressing apparatus for dressing the polishing surface by supplying a dressing liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid so that a pH of the abrasive liquid on the polishing surface is not rapidly changed.
[0025] The above and other objects, features, and advantages of the present invention will become apparent from the following description when taken in conjunction with the accompanying drawings which illustrate preferred embodiments of the present invention by way of example.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] [0026]FIG. 1 is a cross-sectional view of a primary cleaning apparatus according an embodiment of the present invention;
[0027] [0027]FIG. 2A is a plan view of a workpiece support in the primary cleaning apparatus shown in FIG. 1;
[0028] [0028]FIG. 2B is a cross-sectional view taken along line II-II of FIG. 2A;
[0029] [0029]FIG. 3 is a perspective view of a cover in the primary cleaning apparatus shown in FIG. 1;
[0030] [0030]FIG. 4 is a schematic flow diagram of a cleaning liquid supply system;
[0031] [0031]FIG. 5 is a cross-sectional view of the primary cleaning apparatus;
[0032] [0032]FIG. 6 is a graph showing the change of pH in the cleaning liquid in the primary cleaning process;
[0033] [0033]FIG. 7 is a front view of the polishing apparatus in which a dressing process is carried out;
[0034] [0034]FIG. 8 is a front view of a conventional polishing apparatus; and
[0035] [0035]FIG. 9 is a plan view of the conventional polishing apparatus.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0036] A polishing apparatus which uses a cleaning method of the present invention will be described with reference to FIGS. 1 through 7. The whole structure of the polishing apparatus in the present invention is the same as the conventional polishing apparatus shown in FIGS. 8 and 9, and hence the detailed description thereof is not made.
[0037] As shown in FIGS. 1 through 3, the polishing apparatus of the present invention comprises a substrate transferring apparatus (pusher) 10 in which a primary cleaning apparatus C for primarily cleaning a semiconductor substrate which has been polished is provided. This primary cleaning process is defined as a cleaning process for cleaning or rinsing a polished substrate, for the first time, by supplying liquid other than the abrasive liquid. The pusher 10 comprises a workpiece support 12 for placing a semiconductor substrate thereon, and an actuator unit 14 for vertically moving the workpiece support 12 . The workpiece support 12 is supported on the upper ends of vertical rods 15 that are vertically movably provided from the actuator unit 14 . In FIG. 1, the semiconductor substrate W is shown as being held by the top ring 74 , and the workpiece support 12 is shown as being lowered. The pusher 10 further comprises a water receiving container 18 provided around the pusher 10 and having a drain port 16 , and a nozzle bracket 20 attached to the inside of the container 18 for mounting nozzle units thereon.
[0038] As shown in FIGS. 2A and 2B, the workpiece support 12 has a circular base 22 , and a pair of arcuate holding plates 24 mounted on an outer circumferential edge of the circular base 22 and spaced from each other by a pair of recesses 26 defined therebetween. The recesses 26 serve to receive the arm (not shown) of the transfer robot 86 b (see FIG. 9) for transferring the semiconductor substrate W between the holding plates 24 and the transfer robot 86 b . Three nozzle units 28 , 30 , 32 are mounted on the nozzle bracket 20 . The upper nozzle unit 28 serves to eject a cleaning liquid to the lower surface of the top ring 74 , the middle nozzle unit 30 serves to eject a cleaning liquid to the upper surface of the semiconductor substrate W placed on the workpiece support 12 , and the lower nozzle unit 32 serves to eject a cleaning liquid to the lower surface of the semiconductor substrate W placed on the workpiece support 12 through the recess 26 of the workpiece support 12 .
[0039] These nozzle units 28 , 30 and 32 may eject a cleaning liquid having a pressure of 1.1 to 1.2 kg/cm 2 or a cleaning liquid to which ultrasonic wave is imparted by an ultrasonic wave generating apparatus.
[0040] As shown in FIG. 2A, the nozzle unit 32 comprising a plurality of nozzles 32 a is disposed at one location along a circumferential direction of the workpiece support 12 , but a plurality of nozzle units may be disposed at a plurality of locations along a circumferential direction of the workpiece support 12 . The nozzle units 28 and 30 may be also disposed in the same manner as the nozzle unit 32 .
[0041] As shown in FIG. 1, a cover 34 for preventing a cleaning liquid ejected from the cleaning nozzle units 28 , 30 and 32 from being scattered around is provided so as to enclose a space around the pusher 10 . As shown in FIG. 3, the cover 34 has a window 36 for allowing the top ring 74 to pass therethrough on one side thereof, and a window 38 for allowing the arm (not shown) of the robot 86 b (see FIG. 9) to pass therethrough on the other side thereof.
[0042] As shown in FIG. 4, a cleaning liquid supply apparatus 40 is provided to supply a cleaning liquid to the nozzle units 28 , 30 and 32 in the primary cleaning apparatus C. The cleaning liquid supply apparatus 40 comprises a first cleaning liquid tank 42 for storing a first cleaning liquid having a pH of a certain value, and a second cleaning liquid tank 44 for storing a second cleaning liquid which is neutral. In the case where an abrasive liquid used in the polishing process is silica slurry, the first cleaning liquid has a pH of about 10. The cleaning liquid supply apparatus 40 further comprises flow regulating valves 48 a , 48 b provided in pipes 46 a , 46 b extending from the respective cleaning liquid tanks 42 and 44 , a pipe 50 connected to the pipes 46 a , 46 b at the downstream sides of the flow regulating valves 48 a , 48 b , pipes 54 a , 54 b and 54 c branched from the pipe 50 , and valves 52 a , 52 b and 52 c provided in the respective pipes 54 a , 54 b and 54 c . The pipes 54 a , 54 b and 54 c are connected to the respective nozzle units 28 , 30 and 32 . The opening degrees of the flow regulating valves 48 a , 48 b may be adjusted by a controller or a timer so that first, only the first cleaning liquid is supplied, after a certain period of time has elapsed, the second cleaning liquid starts to be supplied and the ratio of the second cleaning liquid to the first cleaning liquid is gradually increased, and finally, only the neutral second cleaning liquid is supplied.
[0043] In the above embodiment, the pH of the first cleaning liquid is about 10, and KOH or the like is used for adjusting a pH of the first cleaning liquid. If the cleaning liquid having a pH of about 9 is sufficient to prevent pH shock from occurring, then electrolytic ionic water which is obtained by electrolysis using an ion exchange membrane may be used. In this case, metal ion is not contained in the cleaning liquid, and hence there is little chance of contamination of the substrate.
[0044] Next, processes in the polishing apparatus having the above structure will be described with reference to drawings.
[0045] As shown in FIG. 8, the semiconductor substrate W is held under vacuum by the top ring 74 , and pressed against the polishing cloth 70 on the turntable 72 while the abrasive liquid Q is supplied onto the polishing cloth 70 . The polishing cloth 70 constitutes a polishing surface on the turntable 72 . While the turntable 72 and the top ring 74 are rotated independently of each other, the lower surface of the semiconductor substrate W is polished to a flat mirror finish. After the semiconductor substrate W is polished, the ground-off particles and the abrasive liquid Q containing abrasive particles adhere to the semiconductor substrate W and the top ring 74 . After completing polishing of the semiconductor substrate W, the top ring 74 which holds the semiconductor substrate W under the vacuum is angularly moved above the pusher 10 , and the top ring 74 is located at the primary cleaning position inside the cover 34 as shown in FIG. 1. While the top ring 74 holds the semiconductor substrate W, a cleaning liquid is supplied from the upper nozzle unit 28 to thereby clean the polished surface of the semiconductor substrate W. In this case, only the first cleaning liquid is supplied from the first cleaning liquid tank 42 to the semiconductor substrate.
[0046] Then, the actuator unit 14 of the pusher 10 is operated to lift the workpiece support 12 toward the top ring 74 . Thereafter, the semiconductor substrate W is removed from the top ring 74 by breaking vacuum and placed on the workpiece support 12 . The actuator unit 14 is operated again to lower the workpiece support 12 away from the top ring 74 as shown in FIG. 5. Then, the three cleaning nozzle units 28 , 30 and 32 are simultaneously operated to eject the cleaning liquid for thereby cleaning the upper and lower surfaces of the semiconductor substrate W and the lower surface of the top ring 74 . In this case, as shown in FIG. 6, first, the first cleaning liquid is supplied from the first cleaning liquid tank 42 , and after a certain period time, the second cleaning liquid starts to be supplied from the second cleaning liquid tank 44 and the ratio of the second cleaning liquid to the first cleaning liquid is gradually increased. Finally, only the cleaning liquid of pH 7 is supplied from the second cleaning liquid tank 44 .
[0047] In this manner, in the early cleaning stage, the cleaning process is performed to remove the abrasive particles from the semiconductor substrate and the top ring without changing a pH of the liquid attached to the semiconductor substrate and the top ring, and then the cleaning liquid is gradually shifted from alkali to neutrality and the pH of the liquid attached to the semiconductor substrate and the top ring is shifted to neutrality. Therefore, the surface of the semiconductor substrate is returned to neutrality in such a state that the liquid attached to the semiconductor substrate still contains abrasive particles without pH shock. Therefore, abrasive particles are prevented from being aggregated on the semiconductor substrate and the top ring. Further, contamination of the semiconductor substrate and the top ring caused by such abrasive particles is also prevented.
[0048] After this primary cleaning is completed, the top ring 74 is moved toward the turntable 72 , and the arm of the robot 86 b is moved to the pusher 10 and holds the semiconductor substrate W. The robot 86 b transfers the semiconductor substrate W to the cleaning apparatuses 90 a , 90 b and 90 c , and the subsequent cleaning processes are conducted therein using pure water. A new semiconductor substrate W is placed on the pusher 10 by the robot 86 b , and the top ring 74 is moved above the pusher 10 and holds the semiconductor substrate W, and then the subsequent polishing of the new semiconductor substrate W is carried out.
[0049] In the above embodiment, the primary cleaning process of the substrate is conducted in the primary cleaning apparatus C provided in the pusher 10 . However, the primary cleaning process may be conducted by the nozzle units provided above the turntable 72 or in the vicinity of the turntable 72 . Further, the primary cleaning process may be conducted in the cleaning apparatuses 90 a , 90 b and 90 c . That is, in the pusher 10 and the cleaning apparatuses 90 a , 90 b and 90 c , the cleaning liquid may be stepwise shifted from the cleaning liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid to pure water.
[0050] Next, a dressing method according to another embodiment of the present invention will be described with reference to FIG. 7. As shown in FIG. 7, the dressing process is conducted between the polishing processes in such a manner that a dressing tool 94 is pressed against the polishing cloth 70 while a dressing liquid is supplied from a dressing liquid supply nozzle 92 to the polishing cloth 70 . In this embodiment, a dressing liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid is supplied from the first cleaning liquid tank 42 shown in FIG. 4 to the polishing cloth 70 . Thus, when the dressing liquid is supplied to the polishing cloth 70 , the pH of the abrasive liquid remaining on the location where the dressing liquid is supplied is not greatly changed to thus prevent the abrasive particles from being aggregated.
[0051] In the dressing process, by supplying the dressing liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid to the polishing cloth until a subsequent polishing of a substrate is started, the subsequent polishing of the substrate can be started in a stable condition.
[0052] In the above embodiments, the primary cleaning process has been described in the case where silica slurry is used as an abrasive liquid. If alumina (Al 2 O 3 ) particles are used as abrasive particles, they are liable to being aggregated in a pH of 8 to 9, and hence it is necessary to control a pH of the abrasive liquid in the same manner as silica slurry or in the manner milder than the silica slurry.
[0053] In alumina slurry which is generally used for polishing the semiconductor substrate W, alumina (Al 2 O 3 ) particles as abrasive particles are stable in acidic solution having a pH of about 4 and form secondary particles having a diameter of about 0.2 μm. In alumina slurry which is practically used, nitric acid solution is mainly used as acidic solution. In alumina slurry which is practically used for polishing, α-alumina is mainly used as abrasive particles. Although α-alumina is stable in a pH of 7 or below, it is desirable that α-alumina has a pH of 3.5 to 5. Since a-alumina is liable to being aggregated in a pH of 8 to 9, the liquid having the pH range 8-9 is not desirable as a cleaning liquid. Therefore, the liquid having a pH of 7 or below is preferable as a cleaning liquid, and the liquid having a pH of 3.5 to 5 is quite favorable.
[0054] As is apparent from the above description, according to the present invention, the pH of an abrasive liquid attached to the substrate or the polishing tool such as the top ring is not rapidly changed, and hence abrasive particles contained in the abrasive liquid are not aggregated by pH shock. Thus, the cleaning of the substrate or the dressing of the polishing cloth can be efficiently conducted.
[0055] Although certain preferred embodiments of the present invention have been shown and described in detail, it should be understood that various changes and modifications may be made therein without departing from the scope of the appended claims. | A method is suitable for cleaning substrates, after polishing, that require a high degree of cleanliness, such as semiconductor wafers, glass substrates, or liquid crystal displays. The method comprises polishing a substrate using an abrasive liquid containing abrasive particles, and cleaning a polished surface of the substrate by supplying a cleaning liquid having substantially the same pH as the abrasive liquid or similar pH to the abrasive liquid so that a pH of the abrasive liquid attached to the polished surface of the substrate is not rapidly changed. | 8 |
BACKGROUND
[0001] 1. Field
[0002] The present invention relates generally to reservoir management and more particularly to methods of modeling secondary production.
[0003] 2. Background
[0004] This application claims priority to U.S. Provisional Application 61/438,174 filed Jan. 31, 2011 the entire contents of which are incorporated herein by reference.
[0005] Hydrocarbon extraction is typically understood as a three stage process. In the primary stage, a reservoir is drilled, and oil and gas are recovered as a result of natural pressures and flows into the drilled well. In the secondary phase, pressure is applied to force more oil and gas from the reservoir. Water, gas, or other fluids may be pumped in to increase the pressure so that more of the hydrocarbons may be recovered. In the tertiary phase, steam, CO 2 or other materials may be injected into the reservoir to further increase production.
SUMMARY
[0006] An aspect of an embodiment of the present invention includes a method of producing hydrocarbons in a reservoir including determining a relationship between an injection well and a producing well based on an injection rate and a production rate wherein the relationship is filtered to produce a filtered value, and a modified state variable model is selected for each relationship to produce a positive relationship value to determine the production rate.
[0007] Aspects of embodiments of the present invention include computer readable media encoded with computer executable instructions for performing any of the foregoing methods and/or for controlling any of the foregoing systems.
DESCRIPTION OF THE DRAWINGS
[0008] 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:
[0009] FIG. 1 is a representation of a reservoir model relating a single production well to a plurality of injection wells;
[0010] FIGS. 2 a - 2 c illustrate an extended Kalman smoother wherein FIG. 2 a illustrates a predictor step, FIG. 2 b illustrates a corrector step and FIG. 2 c illustrates an overall procedure for the EKF for measurements at all time points;
[0011] FIG. 3 illustrates a fixed-interval EKS for measurements over an interval between 1 and D;
[0012] FIGS. 4 a and 4 b illustrate a producer (P- 130 ) and associated injectors I-n ( 4 a ) and injectors remaining after an elimination process ( 4 b );
[0013] FIGS. 5 a and 5 b illustrate IPR values ( 5 a ) and normalized IPR values ( 5 b ) for the injectors I-n of FIG. 4 a;
[0014] FIGS. 6 a and 6 b illustrate IPR values ( 6 a ) and normalized IPR values ( 6 b ) for the injectors of FIG. 4 b;
[0015] FIG. 7 illustrates historical prediction matching;
[0016] FIG. 8 a shows a portion of the prediction matching process illustrated in FIG. 7 and FIG. 8 b illustrates prediction error for the prediction matching of FIG. 8 a;
[0017] FIG. 9 is a table of values for prediction error for the historical prediction matching process;
[0018] FIG. 10 is an illustration of forward prediction and backward smoothing in accordance with an embodiment of the invention;
[0019] FIG. 11 is an illustration of the mixed application of the EKF and IEKFS methods for data of varying density; and
[0020] FIG. 12 is an illustration of the use of EKF with intermittent measurements.
DETAILED DESCRIPTION
[0021] In secondary and tertiary production, it is useful to understand relationships between injection wells (where water, steam or other materials are injected into a reservoir) and production wells (where hydrocarbons are recovered from the reservoir). In this regard, there have been many approaches to modeling flows between injectors and producers, taking into account fluid properties, capillary pressures, fluid contacts, porosity and subsurface geological structures. It is possible to directly measure fluid connectivity, for example using tracer fluids. On the other hand, direct measurements are expensive and slow, and may tend to detract from production operations.
[0022] In one approach, injection rates are correlated to production rates, and a number of mathematical approaches to modeling the relationship between the input and output have been taken. In an extended Kalman filter (EKF) approach, N injectors are assumed to influence a particular producer, and can be modeled using 2N parameters to characterize the impulse response of the system.
[0023] The inventors have determined that there are issues with the EKF approach, specifically that estimates of the injector-producer relationship (IPR values) may take on negative values, a non-physical result; that it may be difficult to determine whether a particular injector is related (or is related in an important way) to a particular producer; and that estimated IPR values may sum to greater than one for a given group of injectors, which is also a non-physical result. By estimating the square root of IPR values directly, negative values for IPR can be eliminated. Constraining the state vectors by requiring that all values of IPR and a fall between 0 and 1 for all time points, and all injector-centered sums of IPR values must also fall in the [0,1] interval can eliminate the second type of non-physical results.
[0024] Therefore, in an embodiment, the present invention provides a method to apply an iterative extended Kalman filter and smoother (IEKFS) to dynamically interpolate data between two available measured values. A production rate is modeled as a state variable for each of a series of time points, and the EKF is applied to forward-estimate the production rate, then an EKS is used to backward-estimate the production rate. The resulting interpolated data can be used in a variety of signal processing-based approaches.
[0025] A reservoir may be modeled in accordance with the Liu-Mendel model, which assumes a producer-centric system having one producer and N injectors as illustrated in FIG. 1 , where i 1 (t), . . . , i N (t), n 1 (t), . . . , n N (t) and i m,1 (t), . . . , i m,N (t) are injection rates, injection rate measurement noise, and measured injection rates. The actual production rate, the production rate measurement noise and the measured production rate are shown as p(t), n p (t) and p m (t). The production for a given injector j is labeled p j c (t)(j=1, . . . N) and f(r j ,k j ) is a scaling function that determines what portion of the injected material at injector j flows to the producer. The scaling function may be a function of the distance r j and the permeability k j of the formation between the injector and the producer. As will be appreciated, the noise-free data is not available in practice and the measured values are used.
[0026] The modeled system characterizing the impulse response is h(t)=bte −at which is discretized and Z-transformed as
[0000]
H
(
z
)
=
γ
z
-
1
(
1
-
α
z
-
1
)
2
where the parameters a=e −aT and y=baT and T is the sampling period. Thus, the reservoir may be modeled as:
[0000]
P
(
z
)
=
∑
j
=
1
N
P
j
c
(
z
)
=
∑
j
=
1
N
H
j
(
z
)
f
(
r
j
,
k
j
)
I
j
(
z
)
=
∑
j
=
1
N
γ
j
f
(
r
j
,
k
j
)
z
-
1
(
1
-
α
j
z
-
1
)
2
I
j
(
z
)
where P(z),P j r (z)andI j (z) are the Z-transforms of the total production rate p(k), the production rate from the j th injector and the injection rate of the j th injector respectively. By appropriate manipulation of the parameters and using the measured injection rates, IPR j can be shown to be
[0000]
γ
j
′
(
1
-
α
j
)
2
.
[0029] In an embodiment, an initial set of injectors are selected as potentially contributing to a given producer. Typically, this selection may rely on the knowledge of subject-matter experts based on information relating to reservoir structure. For example, in a reservoir having known subsurface parallel fractures along a known angle, it may be expected that injectors aligned along the fracture lines will tend to contribute to producers aligned along those lines.
[0030] FIG. 4 a illustrates a producer centric model of a field having a single producer (P- 130 ) and a plurality of injection wells 1-N where each injector has a short and a long completion illustrated as respective upper and lower triangles at each location. IPR curves are generated for all of the completions as shown in FIG. 5 a . Then, as shown in FIG. 5 b , a threshold is applied (dotted line) to the normalized IPR curves (i.e., each curve divided by the sum of all of the IPR curves) and those completions having IPR values lower than the threshold are eliminated. The remaining completions are shown in FIG. 4 b . For N injectors, an initial estimate of the impact of each injector can be set to be 1/N and the threshold may be set, for example, at 80% of 1/N as illustrated in FIG. 5 b . In the illustrated example, there are 46 initial completions, and the threshold is set to 1.74% resulting in elimination of all but 17 completions (shown in FIG. 4 b ).
[0031] In this example, once the low-impact completions are eliminated, the EKF is applied to the remaining 17 completions. The resulting IPR values are shown in FIG. 6 a . Though a portion of three of the IPR curves are shown to be below the threshold, the mean value for the most recent time periods exceeds the threshold so these completions are retained. In an embodiment, completions falling below the threshold can be iteratively eliminated based on a similar (e.g., 80%/N) threshold, where N remains the initial number of injectors. Once an equilibrium is reached and no further injectors are eliminated, the iterative process of elimination may be halted.
[0032] For each producer, the initial set of injectors selected prior to the thresholding process can be selected based on location. For example, injectors positioned within an elliptical region can be chosen. In an example, the ellipse may be 500×700 feet, and the ellipse may be scaled by a scalar value s. In theory, s can be finely discretized and may be selected to range from a small value to a large value such that a minimized point of an objective function is a global minimum. Large numbers of values for s tends to be computationally expensive. The inventors have determined that for s={0.5, 0.6, 0.7, 0.8, 0.9 and 1.0} a sufficient number of injectors can be included (at s=1). Below about 0.5, only a few injectors are included and lower values for s are not typically useful. As will be appreciated, this lower threshold will tend to depend on the specific site and the density of injectors
[0033] In an embodiment, validation testing may be performed by using a history matching process. In this approach, a past injection rate change is used as a starting point for a production “forecast” where the time of the forecast corresponds to a time after the historical starting point but before the present time. The forecast value may then be compared to a measured production rate using a predictor equation from the EKF. This is illustrated in FIG. 7 where the solid line represents measured data and the dotted line represents forecast data. The forecast data is shown more clearly in FIG. 8 a , and prediction error is plotted in FIG. 8 b . FIG. 9 is a table listing average prediction error and a mean error production ratio (EPR). The EPR for s=1 is about 10%, which falls within the expected noise level for actual production measurements.
[0034] For the selected group of injectors, a state vector model is generated for the injector-producer pair system. The EKF is applied to estimate the state vector at a time k+1 using a predictor based on measurements up to the time k, and a corrector which re-estimates x(k+1). These are illustrated in FIG. 2 a (predictor) and 2 b (corrector). While the EKF estimates the state vector in a forward manner, the EKS performs a reverse estimation process. Future measurements are used to determine estimates for earlier time points, and thus is necessarily not a real-time estimation method. Once measurements over the interval between 1 and D are obtained, an estimate of the state vector can be determined based on the available measurements as shown in FIG. 2 c.
[0035] In practice, the measurements at each time k are intermittent, so the corrector can only be applied at the times k corresponding to measurements. On the other hand, the predictor may be applied for all time points. This is shown in FIG. 9 for a series of time steps k i . Thus, for a given interval the estimation procedure is shown in FIG. 10 in which x is forward estimated for each time period using the predictor (lower row of FIG. 10 ). Once actual data for each k becomes available, x is computed and backward estimated using the smoother (upper row of FIG. 10 ). This process can be iterated until the state estimates converge, or a stopping criterion is reached. A final estimate can then be used to determine a gross production rate based on the sum of the individual estimates.
[0036] In an embodiment, measurement sets may have portions which are intermittent while other portions are consecutive. In this case, EKF state estimation is used for those portions having consecutive measurements (i.e., there is no need for interpolation) and iterative extended Kalman filtering and smoothing (IEKFS) is used for the intermittent portions. This is illustrated in FIG. 11 . FIG. 12 illustrates the use of EKF with intermittent measurements with the corrector only applied at time points where measurements are available (e.g., k i and k 1 +1).
[0037] In an embodiment, a sampling frequency of the production rate may be on the order of several days. As an example, the frequency may be between 1 and 15 days, and more particularly, between 5 and 10 days. By using the IEKFS method to interpolate between available measurements, a frequency of measurement may be reduced compared to EKF alone.
[0038] As will be appreciated, the method as described herein may be performed using a computing system having machine executable instructions stored on a tangible medium. The instructions are executable to perform each portion of the method, either autonomously, or with the assistance of input from an operator. In an embodiment, the system includes structures for allowing input and output of data, and a display that is configured and arranged to display the intermediate and/or final products of the process steps. A method in accordance with an embodiment may include an automated selection of a location for exploitation and/or exploratory drilling for hydrocarbon resources.
[0039] 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. 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. In addition, it should be appreciated that structural features or method steps shown or described in any one embodiment herein can be used in other embodiments as well. | A method of producing hydrocarbons in a reservoir includes determining a relationship between an injection well and a producing well based on an injection rate and a production rate wherein the relationship is filtered to produce a filtered value, and a modified state variable model is selected for each relationship to produce a positive relationship value to determine the production rate. | 4 |
FIELD OF INVENTION
The invention is directed toward sleds, and in particular, to restraint systems for such sleds.
BACKGROUND
Known sleds, such as that disclosed in Sellers, U.S. Pat. No. 4,666,171, feature a strap extending transversely across the rider's knees. Such straps prevent the rider from pitching out of the sled. However, they do little to prevent lateral shifting of the rider's legs. Such lateral shifting is particularly pronounced during tight turns at high speed.
The involuntary lateral shift of the rider's legs during a turn can skew the sled's weight distribution. This can lead to loss of control, which at high speed, can be dangerous.
SUMMARY
In one aspect, the invention includes a sled having a hull having opposed first and second side walls. First and second strap anchors are mounted on the respective first and second side walls. A center strap anchor is disposed between the first and second strap anchors.
In one embodiment, the sled also includes a strap extending from the first strap anchor to the second strap anchor. This strap passes through the center strap anchor.
In another embodiment, the sled includes first and second straps. The first strap extends from the first strap anchor to the center strap anchor and the second strap extends from the center strap anchor to the second strap anchor.
The center strap anchor can take a variety of forms. For example, it can include a bar supported by at least one leg extending from a floor of the hull. Or can be shaped to conform to a rider's thigh.
These and other features of the invention will be apparent from the following detailed description and the accompanying figures, in which:
These and other features and advantages of the invention will be apparent from the following detailed description and the figures, in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are top and side views of a hull for a sled;
FIG. 3 is a cross-section of the hull shown in FIGS. 1 and 2 ;
FIGS. 4–6 show a configuration for attaching a strap to the hull;
FIGS. 7–10 show sleds having variable-length straps;
FIG. 11 shows a sled having a strap configured to secure a rider's calves; and
FIGS. 10–14 show sleds having center anchors.
DESCRIPTION OF THE PREFERRED EMBODIMENT
A downhill racing sled suitable for incorporating the features of the invention is described with particularity in Sellers, U.S. Pat. No. 4,666,171, the contents of which are herein incorporated by reference.
As shown in FIGS. 1–3 , the sled includes a one-piece elongated molded hull 10 , preferably of vacuum-molded thermoplastic. The hull 10 has a bow or front-end, which is on the right as viewed in FIGS. 1 and 2 , and a stern, or rear-end, which is on the left as viewed in FIGS. 1 and 2 . Between the bow end and the stern end are a pair of optional contoured shin pads 40 on which a rider kneels while riding the sled.
The hull 10 presents a generally crescent-shaped profile, best seen in FIG. 2 . An upper outwardly rolled molded edge of the hull 10 forms continuous railings or gunwales 12 surrounding the hull 10 . The gunwales 12 are raised at the bow to afford handholds and to protect against the intrusion of snow. The bottom of the hull 10 while generally curved in profile as shown in FIG. 2 , includes certain features that enhance the sled's performance in deep snow.
Between the two runners 14 and 16 , a main central channel 30 extends along a mid-line of the hull 10 from the bow to the stern with progressively increasing depth as shown in FIGS. 2 and 3 . The inside ribs 20 and 22 define the edges of the channel 30 and are slightly outwardly flared with gradually increasing spacing at both ends of the hull 10 . Inside the hull 10 , the molded channel 30 forms a large longitudinal central rib or keel-like hump 32 running down the center of the hull 10 . Because of the increasing depth of the snow channel 30 toward the rear of the hull 10 , the hump 32 becomes more pronounced toward the rear as shown in phantom in FIG. 2 .
Referring now to FIG. 4 , side portions of the gunwale 12 are rolled outward to form a lip 56 . This lip 56 curls downward to form a rim portion 58 parallel to the hull 10 and separated therefrom by a gap 60 . An outboard hole 62 through the rim portion 58 is aligned with an inboard hole 64 through the hull 10 . Molded retaining walls 66 A–B, seem in isometric view in FIG. 5 flank the inboard hole 64 and extend outward from the hull 10 , part way across the gap 60 .
A strap 36 has a grommet 68 at each of its two ends, one of which is shown in FIG. 6 . To attach the strap 36 to the hull 10 , a grommet hole 70 defined by the grommet 60 is aligned with the inboard hole 64 . Then, a threaded ½ inch bolt 72 is passed through the grommet hole 70 and through the inboard hole 64 . The bolt 72 is long enough to extend through the inboard hole 64 and all the way to the outboard hole 62 . Preferably, the bolt 72 extends approximately 3/16 inches beyond the outboard hole 62 to ensure adequate support by the edge of the outboard hole 62 .
A nut 74 is then threaded onto the bolt 72 to secure the bolt 72 to the hull 10 . When the nut 74 is fully tightened, it comes to rest snugly between the retaining fins 66 A–B, as shown in FIG. 8 . The retaining fins 66 A–B thus limit rotation of the nut 74 in response to torque transmitted by the strap 36 . By doing so, the retaining fins 66 A–B reduce the likelihood that the nut 74 will loosen during use. The nut 74 , the bolt 72 , and the walls forming the inboard and outboard holes 62 , 64 collectively define a strap anchor 65 .
Because of its strength, metal is typically used for making the nut 74 and bolt 72 . However, other materials, such as plastic can be used.
A shear force exerted on the strap 36 is transmitted to the hull 10 by the bolt 72 . However, the hull 10 supports the bolt 72 at two different points, namely at the edge of the inboard hole 64 and also at the edge of the outboard hole 62 . As a result, the strap-anchoring configuration shown in FIGS. 4–6 resists the tendency of the bolt 72 to pivot about a single support in response to a shear force. It does so by resisting shear force using shear resistance provided by the hull 10 at two different support points.
By concealing the nut 74 and bolt 72 from view, the rim portion 58 of the lip provides the hull 10 with a more attractive and streamlined appearance. This appearance can be enhanced by coloring the end of the bolt 72 or by extending the end of the bolt 72 slightly beyond the rim portion 58 so it can be capped.
In addition, by covering the nut 74 and bolt 72 , the rim portion 58 also prevents the nut 74 and bolt 72 from snagging on nearby objects, such as the rider's clothing.
In one embodiment, the strap 36 has a length that varies in response to the force exerted thereon. An example of such a strap 36 is an elastic strap as shown in FIG. 7 . Another example is a strap 36 having one or more elastic sections 76 A–B, as shown in FIG. 8 . In this case, the strap 36 has a pair of inelastic grommet sections 78 A–B that accommodate the grommets 68 and a central inelastic section 80 for securing the rider. Each grommet section 78 A–B is connected to the central inelastic section 80 by a corresponding one of the elastic sections 76 A–B. Yet another example, shown in FIG. 9 is a strap 36 having a pair of inelastic grommet sections 78 A–B joined by a central elastic section 82 .
Preferably, the elasticity of the strap 36 , or the elasticity of an elastic section thereof, is such that the strap 36 changes in length by no more than three inches. A strap 36 that is excessively elastic, in which the length changes significantly, will fail to restrain the rider. A strap 36 that has too little elasticity will be uncomfortable in the presence of high g-forces.
The elastic sections can be made of a manufactured fiber in which the fiber-forming substance is a long-chain synthetic polymer comprised of at least 85% of a segmented polyurethane. An exemplary fiber having these properties is presently sold under the name SPANDEX™. The elastic sections can also be made of a manufactured elastic fiber sold under the name SPANDURA™.
The inelastic sections can be made of a manufactured fiber in which the fiber forming substance is a long-chain synthetic polyamide in which less than 85% of the amide-linkages are attached directly (—CO—NH—) to two aliphatic groups. An exemplary fiber having these properties is presently sold under the name NYLON™.
Another embodiment, shown in FIG. 10 , features an elastic section 76 A in which the elasticity is provided by a spring 84 . The spring 84 is sheathed by a fabric jacket 86 (opened to expose the spring 84 in FIG. 10 ) to protect the rider's clothing from being caught by the spring 84 as it expands and contracts.
The longitudinal position of the strap anchor 65 can be chosen so that the strap 36 extends across the hull 10 above the shin pads 40 . In this configuration, the strap 36 extends over the rider's thighs. However, the strap 36 can also be placed astern of the shin pads 40 so that the strap 36 extends over the rider's upper calves, as shown in FIG. 11 . In this latter configuration, the strap 36 secures the rider's calves and thereby frees the rider from having to ride with fully flexed knees at all times. A rider thus freed is able to kneel erect or partially erect in the sled, thereby enabling the rider to shift the center-of-mass vertically by a distance that corresponds to the difference between the rider's fully erect position and the rider's fully crouched position.
In FIG. 11 , the strap 36 can be switched between a rear pair of strap anchors 65 and a forward pair of strap anchors 88 that are structurally the same as the rear pair of strap anchors 65 but positioned over the shin pads 40 . The sled shown in FIG. 11 is thus convertible between the configuration shown in FIG. 1 , in which the strap 36 secures the rider's calves, and a configuration in which the strap 36 secures the rider's thighs.
A disadvantage of having a single strap 36 that extends across the hull 10 is that in sharp turns, both of the rider's legs are apt to shift laterally. This causes the center-of-mass of the combined rider and sled to also shift laterally. This lateral shift during a turn undermines the stability of the turn and, in extreme cases, can capsize the sled.
To avoid this difficulty, another embodiment of the sled features a center anchor 90 at the mid-line of the hull 10 . An exemplary center anchor 90 , shown in FIG. 12 , is a longitudinally extending horizontal bar 92 supported over the hull by a vertically-extending bow leg 94 A and a vertically-extending stern leg 94 B. The bar 92 and the two legs 94 A–B define an aperture 96 through which a strap 36 extending transversely across the hull 10 passes. When the strap 36 is looped through the center anchor 90 , as shown in FIG. 12 , the rider's legs are individually secured. This makes it more difficult for the rider's legs to shift laterally in a sharp turn.
In FIG. 13 , the single strap 36 extending across the hull 10 is replaced by a pair of straps 98 A, 98 B, each one of which extends from a strap anchor 65 to the center anchor 90 . This embodiment enables the rider to individually adjust the straps 98 A, 98 B.
In another embodiment, shown in FIG. 14 , the center anchor 90 is molded and/or padded to more closely fit the rider's thighs. This embodiment can be configured to accommodate a single strap 36 looping through an aperture in the center anchor 90 or a pair of straps extending in opposite directions from the center anchor 90 to each of the two sides of the hull 10 .
The invention has been described in the context of a specific recreational racing sled. However, the various features of the invention can readily be incorporated other types of recreational sleds. | A sled includes a hull having opposed first and second side walls. First and second strap anchors are mounted on the respective first and second side walls. A center strap anchor is disposed between the first and second strap anchors. | 1 |
TECHNICAL FIELD
[0001] The present invention relates to a printed circuit board pad design and is particularly concerned with maintaining insulative spacings on very tight-pitch grid arrays.
BACKGROUND
[0002] High-speed electronic applications require the mounting of very small components, for example decoupling capacitors, on very tight-pitch grid arrays of, for example 0.8 mm by 0.8 mm, which are compatible with Ball Grid Array (BGA) components.
[0003] One approach which can provide sufficient spacing within the BGA grid pattern is a technology known as Via In Pad Plated Over (VIPPO) which provides circuit board vias placed in the Ball Grid Array circuit board pads. This frees up space on the outer layer which may be used for component placement. However, VIPPO technology has an increased manufacturing cost associated with its use, a cost which can be on the order of 10% to 25% higher than normal plated through hole technologies.
[0004] Therefore, it would be desirable to provide a method of placing small components within tight-pitch BGA grids while avoiding the extra cost associated with more complex and costly circuit board technologies such as Via In Pad Plated Over technologies.
SUMMARY
[0005] A brief summary of various exemplary embodiments is presented below. Some simplifications and omissions may be made in the following summary, which is intended to highlight and introduce some aspects of the various exemplary embodiments, but not to limit the scope of the invention. Detailed descriptions of a preferred exemplary embodiment adequate to allow those of ordinary skill in the art to make and use the inventive concepts will follow in later sections.
[0006] According to an aspect of the invention there is provided a through-hole printed circuit board (PCB) having: a ball grid array (BGA) of BGA pads on one side of the PCB, arranged in a tight-pitch grid pattern; through-hole vias, including respective via pads, arranged in the grid pattern and at least one of the through-hole vias electrically connected to the BGA pads; substantially rectangular component pads on the opposite side of the PCB from the BGA pads, the component pads located between pairs of the through-hole vias; each substantially rectangular component pad having a relieved section at a point of closest approach to a via pad; a solder mask covering the component pad with an opening; a solder pad within the opening electrically connected to the component pad; and a two-lead component attached to the solder pad.
[0007] In some embodiments of this aspect of the invention the grid pattern is square. In other embodiments of this aspect of the invention the grid pattern is rectangular.
[0008] In some embodiments of this aspect of the invention the grid pattern has 0.8 mm pitch.
[0009] In some embodiments of this aspect of the invention the two-lead component is an Imperial 0201 component. In some of these embodiments the Imperial 0201 component is a discrete component. In some of these embodiments the Imperial 0201 component is a capacitor.
[0010] According to another aspect of the invention there is provided a method of manufacturing a PCB having the steps of: selecting two adjacent through-hole vias on a printed circuit board (PCB), wherein each via has a corresponding via pad, wherein the PCB has a ball grid array (BGA) of BGA pads on one side of the PCB arranged in a grid pattern, wherein the PCB has an array of substantially rectangular component pads on the opposite side of the PCB from the BGA pads, the component pads located between pairs of the through-hole vias, and wherein each substantially rectangular component pad having a relieved section at a point of closest approach to a via pad; covering each component pad with a respective solder mask; removing areas from the solder masks; placing solder pads in the areas; and attaching a two-lead component to the two adjacent component pads using the solder pads.
[0011] In some embodiments of this aspect of the invention the grid pattern is square. In other embodiments of this aspect of the invention the grid pattern is rectangular.
[0012] In some embodiments of this aspect of the invention the grid pattern has 0.8 mm pitch.
[0013] In some embodiments of this aspect of the invention the two-lead component is an Imperial 0201 component. In some of these embodiments the Imperial 0201 component is a discrete component. In some of these embodiments the Imperial 0201 component is a capacitor.
[0014] According to yet another aspect of the invention there is provided a computer aided design tool implemented on a computing device for accommodating a two-lead component on in a 0.8 mm by 0.8 mm pitch ball grid array (BGA) printed circuit board (PCB) having: a design tool mode configured to select two adjacent through-hole vias on the printed circuit board (PCB) for connection to a two-lead component; a design tool mode configured to identify a placement of substantially rectangular component pads on the opposite side of the PCB from the BGA pads, the component pads located between pairs of the through-hole vias, wherein each substantially rectangular component pad having a relieved section at a point of closest approach to a via pad; a design tool mode configured to identify a placement of pads and shape of solder pads on two adjacent component pads, wherein the placement allows a two-lead component to connect to two adjacent component pad, and wherein the spacing between component pads and adjacent non-connected vias meets a pre-established requirement.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In order to better understand various exemplary embodiments, reference is made to the accompanying drawings, wherein:
[0016] FIG. 1 shows a bottom view of a portion of a fine-pitch through-hole circuit board according to an embodiment of the invention;
[0017] FIG. 2 shows a sequential embodiment of a process for attaching a surface mount component according to an embodiment of the invention;
[0018] FIG. 3 shows alternative connection arrangements between via pads and component pads according to an embodiment of the invention; and
[0019] FIG. 4 illustrates a cross sectional view of the fine-pitch through-hole circuit board of FIG. 1 having a component mounted thereon.
[0020] To facilitate understanding, identical reference numerals have been used to designate elements having substantially the same or similar structure and/or substantially the same or similar function.
DETAILED DESCRIPTION
[0021] The description and drawings merely illustrate the principles of the invention. It will thus be appreciated that those skilled in the art will be able to devise various arrangements that, although not explicitly described or shown herein, embody the principles of the invention and are included within its scope. Furthermore, all examples recited herein are principally intended expressly to be only for pedagogical purposes to aid the reader in understanding the principles of the invention and the concepts contributed by the inventor(s) to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions. Additionally, the term, “or,” as used herein, refers to a non-exclusive or (i.e., and/or), unless otherwise indicated (e.g., “or else” or “or in the alternative”). Also, the various embodiments described herein are not necessarily mutually exclusive, as some embodiments may be combined with one or more other embodiments to form new embodiments.
[0022] Referring now to the drawings, in which like numerals refer to like components or steps, there are disclosed broad aspects of various exemplary embodiments.
[0023] FIG. 1 shows a bottom view of a portion of a fine-pitch through-hole circuit board according to an embodiment of the invention. This includes a portion of a circuit board 100 , which contains a standard ball grid array (BGA) of BGA pads on the top side (not shown) and a set of through-hole vias also arranged on a grid spaced which is offset from the BGA pad grid, such that they do not overlap the BGA pads. The through-hole vias have pads 102 are which are labeled ( 102 a , 102 b , 102 c , and 101 d ), but other through-hole vias may be present. In an exemplary embodiment BGA pads 102 form a 0.80 mm pitch grid, meaning that through-hole vias pads 102 a , 102 b , 102 c , and 101 d are spaced 0.80 mm center-to-center apart in a square grid.
[0024] The standard structure of the through-hole vias includes via pad 102 a and through-hole via 106 , having via barrel 104 . Typically, through-hole via pad 102 a will be substantially circular in shape; through-hole via 106 will be substantially circular in shape and have a radius of 0.25 mm. All dimensions may have a tolerance of ±10%. Via barrel 104 has an outer radius to fit in through-hole via 106 .
[0025] Further evident in FIG. 1 is component pad 103 upon which a terminal of a surface-mount component may be soldered. Component pad 103 a has solder resist layer 105 a overprinted upon it. The outline of a two-terminal surface mount component 107 is indicated by the dashed lines. Likewise, component pad 103 b having solder resist layer 105 b is located at the other end of the two-terminal surface mount component outline 107 .
[0026] In an exemplary embodiment, two-terminal surface mount component depicted by outline 107 is a two-lead 0201 component, having a length of 0.5 mm and a width of 0.25 mm. In the embodiment the two-terminal surface mount component is a discrete component. In some cases, this component is a capacitor that can be used for decoupling. As will be further described in FIG. 3 , component pads 103 may be connected via conductive copper paths to via pads 102 as required for various layout configurations.
[0027] Through-hole via pad 102 a has an insulative offset distance 108 a indicated by the dashed line surrounding the via pad. Likewise may be seen an insulative offset distance 108 b relative to through-hole via pad 102 b . This offset distance is the requisite spacing required to provide reliable electrical separation between the through-hole via pads and other copper features on the printed circuit board. In order to meet these insulative spacing requirements, component pad 103 a and component pad 103 b have truncated portions which avoid the insulative offset region, while maintaining sufficient landing area to allow surface mount soldering of two-lead 0201 components.
[0028] While these truncated portions are evident in relation to the insulated offset distances as indicated at 108 a and 108 b , one skilled in the art will recognize that the same insulative distance will be maintained to through-hole via pads 102 c and 102 d . Further, as indicated at 108 c , this insulative offset distance may also be maintained between component pads, in this case component pad 103 b and 103 c.
[0029] FIG. 2 illustrates a sequential embodiment of a process for attaching a pair of surface mount components according to an embodiment of the invention. The method generally consists of steps 210 , 220 , 230 , 240 , 250 , and 260 . The final product results in the structure depicted in FIG. 4 .
[0030] At step 210 , four adjacent through-holes are produced in a circuit board. A single such hole is indicated at 216 .
[0031] At step 220 the holes are coated with a conductive material, such as copper, producing a via barrel. Other via construction methods are recognized by those skilled in the art. A single such barrel is indicated at 224 for hole 226 .
[0032] At step 230 , the adjacent vias are entirely covered with etch resist 231 . In an exemplary embodiment, etch resist 231 is a thin layer of a nonconductive polymer which will resist the acids used to remove copper from portions of the printed circuit board.
[0033] At step 240 in an exemplary embodiment, via pad 242 , via barrel 244 and through-hole 246 may be seen after etching is complete and the etch resist 231 removed. Also visible are component pad 243 and solder mask 245 . Solder mask 245 is a thin layer of a nonconductive polymer. Solder mask 245 prevents the copper portions of the via from oxidizing and prevents unintended solder bridges from accidentally forming on the circuit board. Solder mask may be applied using a silkscreen process.
[0034] At step 250 , solder paste 259 is applied to component pad 253 within the boundaries of solder mask 255 .
[0035] At step 250 , a portion of solder mask 255 corresponding to a component landing area on component pad 253 is removed. This may be accomplished by etching the solder mask to remove material. In an exemplary embodiment solder mask 255 is modified using photolithography. However, other processes may be used to remove a portion of solder mask 255 . Solder paste 259 is applied to component pad 253 within the boundaries of removed portion of solder mask 255 .
[0036] At step 260 , component 267 is attached to component pad 263 using reflowed solder paste 269 . Solder mask 265 acts as a part of a barrier between via pad 262 and component pad 263 , preventing solder bridging from occurring during the attachment process.
[0037] The steps 210 , 220 , 230 , 240 , 250 and 260 may be carried out by a computer controlled machine. In an exemplary embodiment, a computer aided design tool allows the selection of vias and arrangement of the solder mask, solder pad, and component to be substantially automated. The computer aided design tool may automatically identify appropriate spacing and shape of the solder pad to place standard components on a BGA. A computer aided design tool may also provide instructions to control a machine to manufacture the modified circuit board. Instructions may be exported to the machine or the design tool may directly control the machine.
[0038] FIG. 3 shows alternative connection arrangements between via pads and component pads according to an embodiment of the invention. Referring to element 310 there may be seen a bottom view of a through-hole printed circuit board having via pads 312 a , 312 b , 312 c , and 312 d ; as well as component pads 313 a , 313 b , 313 c , and 313 d . The via pads are electrically coupled to the respectively numbered component pads by short sections of conductive copper. The spacing between component pads 313 b and 313 d provide the required insulative offset, allowing separate two-lead 0201 components to be mounted between component pads 313 a and 311 b ; and between 313 c and 313 d.
[0039] Referring to element 320 there may be seen a bottom view of a through-hole printed circuit board having via pads 322 a , 322 b , 322 c , and 322 d ; as well as component pads 323 a , 323 b , 323 c , and 323 d . The via pad 322 a is electrically coupled to the component pad 323 a , and likewise, the via pad 322 c is electrically coupled to the component pad 323 c . Via pad 322 b is electrically coupled to the component pad 323 b . In this exemplary embodiment component pad 323 b has been elongated so that it may serve as an attachment point for two separate two-lead 0201 components: one attached between component pad 323 a and 323 b , and the other between 323 c and 323 b . This particular layout arrangement could find application where via pad 322 b is connected to a ground or power rail, for example, and decoupling capacitors are desired to be connected from vias 323 c and 323 a.
[0040] FIG. 4 illustrates a cross sectional view of the fine-pitch through-hole circuit board of FIG. 1 having a component mounted thereon. This view applies to both the device formed at step 260 of FIG. 2 and attached component depicted in outline 107 of FIG. 1 .
[0041] Printed Circuit Board (PCB) 401 has vias with via pads 402 a and 402 b , conductive via barrel 404 a connective the via pads 402 a and 402 b ; and through-hole 406 . Component pad 403 has solder mask 405 a and 405 b . Reflowed solder 409 electrically connects component 407 to component pad 409 . Component pad 409 maintains an appropriate insulative distance 408 from via pad 402 a.
[0042] Thus what has been disclosed is a method of placing small components within tight-pitch BGA grids while avoiding the extra cost associated with more complex and costly circuit board technologies.
[0043] While the figures and descriptions may depict regular circular or rectangular shapes of different elements in exemplary embodiments, it should be understood that alternative shapes may be used such as imperfect polygons and rounded forms. These alternative shapes may be substantially similar to the depicted shapes in area and outline.
[0044] Although the various exemplary embodiments have been described in detail with particular reference to certain exemplary aspects thereof, it should be understood that the invention is capable of other embodiments and its details are capable of modifications in various obvious respects. As is readily apparent to those skilled in the art, variations and modifications can be effected while remaining within the spirit and scope of the invention. Accordingly, the foregoing disclosure, description, and figures are for illustrative purposes only and do not in any way limit the invention, which is defined only by the claims. | A relieved component pad for 0201 component use between vias on a tight-pitch Ball Grid Array is disclosed herein. The relieved component pad for 0201 component use between vias provides substantially rectangular component pads having a relieved section at a point of closest approach to a via pad. The relieved component pad for 0201 component use is particularly useful for overcoming the problem of 0201 component placement on tight-pitch arrays known in the art | 8 |
CLAIM FOR PRIORITY
[0001] This application claims priority to German Application No. 10255848.5 filed Nov. 29, 2002, which is incorporated herein, in its entirety, by reference.
TECHNICAL FIELD OF THE INVENTION
[0002] The invention relates to a semiconductor component, and in particular a memory module, having a carrier board and semiconductor chips and to a method for producing semiconductor components.
BACKGROUND OF THE INVENTION
[0003] SSTL (Series Stub Terminated Logic) topology represents an inexpensive and easily upgradeable solution for memory systems. At high clock frequencies, for example at clock frequencies above 150 MHz, the performance of such memory systems is restricted, however, since the memory controller (MC) can only handle a limited capacitive load. Thus, by way of example, SSTL topology for a DDR II (Double Data Rate) system at a clock rate of 266 MHz is limited to the use of four DRAM (Dynamic RAM) elements. Since conventional computer systems are usually provided with four slots for furnishing memory modules, it is thus possible either for two slots to be furnished with two memory elements in each case or for all four slots to be furnished with one memory element in each case.
[0004] The so-called SLT (Short Loop Through) bus topology has been proposed in order to eliminate this disadvantage. It is based on reducing the number of branch junctions needed to transport signals from the memory bus to the individual memory modules. In order to reduce signal reflections, a series of controller drivers are directly connected to each memory module for this purpose. What is disadvantageous about this solution is that with the number of connection pins at the connection piece (connector) remaining the same, the bus width is halved since the entire data bus has to be led through each memory module. A larger connection piece with more connection pins, which would make it possible to use the full bus width, would lead to problems, however, during production and during installation in the main board (Motherboard).
SUMMARY OF THE INVENTION
[0005] The present invention increases storage density for SLT topologies.
[0006] In one embodiment of the invention, semiconductor chips are arranged directly on the carrier board (PCB, Printed Circuit Board), with the result that the use of the intermediate carriers provided hitherto on the carrier boards in corresponding slots for receiving the semiconductor chips is no longer necessary. With the space requirement on the main board remaining the same compared with conventional solutions, it is thus possible to achieve an increase in the storage density. At the same time, a stable environment is created for the SLT topology. By virtue of the individual semiconductor chips being arranged on edge, it is possible to obtain storage densities that have not been achieved hitherto in SLT topology. In this case, the memory/volume factor may be defined depending on the type of DRAM memory elements used.
[0007] Significantly, unlike hitherto, the semiconductor chips are not fitted with their main side flat on the intermediate carrier, rather the semiconductor chips are now arranged vertically on the carrier board, so that the main plane of the semiconductor chip running parallel to the main side runs perpendicular to the carrier board. In other words, the semiconductor chips are arranged on the carrier board such that they stand on one of their narrow sides.
[0008] The carrier board provided with semiconductor chips may be received as a memory module directly in corresponding receptacle devices of the main board. If it is arranged parallel to the main board in this case, only two connection pieces are required for the mounting of the carrier board. It is furthermore advantageous that the number of soldering points on the main board is thereby significantly reduced.
[0009] In one preferred refinement of the invention, the semiconductor chips are connected to the carrier board by means of soldered connections. The use of soldered connections guarantees a particularly reliable and long-lasting electrical connection between semiconductor chip and carrier board.
[0010] In a further preferred refinement of the invention, the semiconductor chips have printed lines on one of their main sides. The lines serve for electrically connecting the contact points of the semiconductor chips to contact areas of the carrier board. It is particularly advantageous if the printed lines run beyond the lower edges of the main sides of the semi-conductor chips onto the base sides of the semiconductor chips. The semiconductor chips can then be fixed on the carrier board in a particularly simple manner, since the semiconductor chip only has to be placed by its base side onto the corresponding contact areas of the carrier board and subsequently be soldered.
[0011] Another preferred refinement of the invention provides for two semiconductor chips in each case to be combined to form a chip composite. A so-called DDP (Double Density Package) system is thereby produced, which allows two semiconductor chips to be arranged on the same space as one conventional semiconductor chip. For this purpose, the two semiconductor chips are preferably connected to one another by an adhesive at their main sides free of contact points. The storage density can again be considerably raised through the use of such a chip composite. Furthermore, the performance of the memory system is increased and the cost risk in the production of the memory subsystem is reduced.
[0012] The invention furthermore relates to a method for producing semiconductor components. This method provides for electrical lines to be printed on the main sides of semiconductor chips and then for a chip composite to be produced by adhesively bonding two semiconductor chips in each case, which chip composite is subsequently fitted on a carrier board in such a way that the main planes of the semiconductor chips run perpendicular to the carrier board. Semiconductor components with particularly high storage density can be produced by such a method.
[0013] One advantage of the method is that the adhesive bonding of the semiconductor chips is effected in such a way that after the introduction an adhesive between the main sides of the semiconductor chips, the latter are brought together in an adhesive bonding mold in such a way that an at least partial encapsulation of the chip composite is produced. As a result, the chip composite is not only mechanically stabilized but also shielded from external influences. If an elastic adhesive is used, then it is furthermore possible also to compensate for alternating mechanical stresses on account of different coefficients of linear thermal expansion.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The invention is explained further below with reference to the drawing.
[0015] In this case:
[0016] [0016]FIG. 1 shows a side view of a memory chip with printed circuits.
[0017] [0017]FIG. 2 shows a plan view of a main side of the memory chip from FIG. 1.
[0018] [0018]FIG. 3 shows a side view of a chip composite at the beginning of the adhesive bonding process.
[0019] [0019]FIG. 4 shows a side view of a chip composite after the adhesive bonding process has concluded.
[0020] [0020]FIG. 5 shows a side view of a chip composite fitted on a carrier board.
[0021] [0021]FIG. 6 shows a plan view of a carrier board with a plurality of chip composites.
[0022] [0022]FIG. 7 shows a side view of a populated carrier board during installation onto a main board.
DETAILED DESCRIPTION OF THE INVENTION
[0023] [0023]FIGS. 1 and 2 represent a memory chip 1 as is used for producing a memory module according to the invention. The memory chip 1 has contact points (pads) 3 on one of its main sides 2 . Said contact points are provided with lines 4 in order to produce an electrical connection to the contact areas of a carrier board, which lines have previously been printed on the surface of the memory chip 1 by a suitable method. The printed lines 4 run beyond the lower edge 5 of the main side 2 of the memory chip 1 onto the base side 6 of the memory chip 1 , so that the memory chip 1 , for contact connection with the contact areas of the carrier board, merely has to be placed onto the carrier board by its base side 6 .
[0024] [0024]FIGS. 3 and 4 show different phases in the process for producing a chip composite 7 comprising two memory chips 1 . Accordingly, first of all the main sides 8 of the two memory chips 1 that are free of contact points are arranged in such a way that they point toward one another. The interspace 11 between the main sides 8 and the two memory chips 1 is then filled in a so-called underfill process and/or by injecting an adhesive 9 in injection direction 10 . Afterward, the two memory chips 1 are joined together by being moved toward one another in pressure direction 12 . In this case, the memory chips 1 are brought together in an adhesive bonding mold in such a way that an at least partial encapsulation of the chip composite 7 is produced by virtue of the adhesive 9 between the main sides 8 escaping into the adhesive bonding mold. An elastic separation element 14 in the form of an elevation projecting beyond the electrical lines 4 simultaneously forms at the base side 13 of the chip composite 7 between the electrical connection points of the two memory chips 1 . Said separation element 14 serves not only for the insulation of the conductor tracks but also for mechanical stabilization during the mounting of the chip composite 7 .
[0025] For the mounting of the chip composite 7 , the latter is fitted in mounting direction 15 on a carrier board 16 and soldered. FIG. 5 shows a memory module 28 having a PCB carrier board 16 with a chip composite 7 fixed thereon. In this case, the lines 4 at the base side 6 of the memory chips 1 are connected by soldering points 17 to the corresponding contact areas 18 on the carrier board 16 . The memory chips 1 are thus mounted with their main planes 19 perpendicular to the carrier board 16 . The structural height 20 of such a chip composite 7 is 10 mm, for example.
[0026] At its longitudinal sides 21 , the carrier board 16 has contact elements 22 for making contact with edge connectors fitted on a main board. In this case, the contact elements 22 serve either for a purely mechanical safeguarding of the carrier board 16 or else at the same time for a fly-by-termination. FIG. 6 shows the way in which the chip composites 7 are arranged on the carrier board 16 . Only five of them here, by way of example, nine possible locations are occupied in this case.
[0027] Finally, FIG. 7 shows the way in which the memory module, comprising the carrier boards 16 populated with the chip composites 7 , is installed onto a PCB main board 23 of a computer system. Corresponding 90° SMT edge connectors 24 for the mounting of the carrier board 16 are fitted on the main board 23 . For mounting purposes, the carrier board is fed in installation direction 25 onto the main board 23 until the contact elements 22 at the longitudinal sides of the carrier board 16 engage with the edge connectors 24 . For the mechanical support of the carrier board 16 , elastic supporting elements 25 are provided on the main board 24 , the carrier board 16 bearing on the supporting elements in the mounted state. In the mounting end position, the carrier board 16 then runs parallel to the main board 23 . The memory chips 1 are driven by means of a memory controller 27 , which is arranged on the main board 23 and is connected to the memory chips 1 via the edge connectors 24 by means of the circuits printed on the main board 23 .
[0028] List of Reference Symbols
[0029] [0029] 1 Memory chip
[0030] [0030] 2 Main side
[0031] [0031] 3 Contact point
[0032] [0032] 4 Line
[0033] [0033] 5 Lower edge
[0034] [0034] 6 Base side
[0035] [0035] 7 Chip composite
[0036] [0036] 8 Main side
[0037] [0037] 9 Adhesive
[0038] [0038] 10 Injection direction
[0039] [0039] 11 Interspace
[0040] [0040] 12 Pressure direction
[0041] [0041] 13 Base side
[0042] [0042] 14 Separation element
[0043] [0043] 15 Mounting direction
[0044] [0044] 16 Carrier board
[0045] [0045] 17 Soldering point
[0046] [0046] 18 Contact area
[0047] [0047] 19 Main plane
[0048] [0048] 20 Structural height
[0049] [0049] 21 Longitudinal side
[0050] [0050] 22 Contact element
[0051] [0051] 23 Main board
[0052] [0052] 24 Edge connector
[0053] [0053] 25 Installation direction
[0054] [0054] 26 Supporting element
[0055] [0055] 27 Memory controller
[0056] [0056] 28 Memory module | The invention relates to a semiconductor component, in particular memory module, having a carrier board and semiconductor chips, in particular memory chips, the semiconductor chips being fitted on the carrier board such that the main planes thereof run perpendicular to the carrier boards. Furthermore, the invention relates to a method for producing semiconductor components. | 7 |
BACKGROUND OF THE INVENTION
1. Field of The Invention
This invention relates to an image reproduction process, and more particularly to a process for thermally transferring images from a photohardenable image bearing element to a receptor material.
2. Description of The Prior Art
Printing using sublimable colorants has been known and used for many years. One such process, known as heat transfer printing uses subliming dyes for coloring various materials such as synthetic fabrics. In another process printing is accomplished by means of sublimable dyes contained in a resinous binder on a paper transfer sheet. Each of these processes prints on an intermediate receptor followed by transfer to the final receptor material.
U.S. Pat. No. 3,649,268 discloses still another process wherein name plates are produced by fixing a sublimable dye on a sheet of anodized aluminum. The dye is applied as a toner on the surface of an imagewise exposed photopolymerizable layer coated on an anodized aluminum sheet. Toner adheres to the non-photopolymerized areas of the surface and is removed from the polymerized areas. Upon heating of the toned surface for several minutes at 200° C., it is found that the sublimable dye diffuses through the unpolymerized areas and stains the surface of the aluminum. By this process only a single color image can be produced and extreme care must be taken not to disturb or interfere with the toned surface which is unprotected.
SUMMARY OF THE INVENTION
In accordance with this invention an improved process for forming at least a single color image on a receptor material is provided using a photohardenable element, said process comprising the steps of:
(A) EXPOSING IMAGEWISE TO ACTINIC RADIATION A PHOTOHARDENABLE ELEMENT HAVING A PHOTOHARDENABLE LAYER TO FORM IMAGEWISE TACKY AND NON-TACKY AREAS IN THE LAYER;
(B) TONING THE TACKY AREAS OF THE LAYER BY APPLYING AND ADHERING THERETO A TONER MATERIAL COMPRISING A HEAT TRANSFERABLE, SUBLIMABLE DYE OR MIXTURE OF DYES;
(C) LAMINATING A PHOTOHARDENABLE LAYER OVER THE TONED SURFACE AND PHOTOHARDENING SAID LAYER BY NON-IMAGEWISE EXPOSING TO ACTINIC RADIATION;
(D) PLACING THE PHOTOHARDENED SURFACE IN CONTACT WITH THE SURFACE OF A RECEPTOR MATERIAL;
(E) HEATING FOR AT LEAST 5 SECONDS EITHER THE TONED ELEMENT, THE RECEPTOR MATERIAL, OR BOTH, WHILE IN CONTACT TO A TEMPERATURE AT WHICH AT LEAST SOME OF THE DYE SUBLIMES AND IMAGEWISE CONDENSES ON THE RECEPTOR MATERIAL, THE TEMPERATURE BEING BELOW THAT WHICH WOULD MELT OR OTHERWISE DEGRADE EITHER THE PHOTOHARDENABLE LAYER OR THE RECEPTOR MATERIAL; AND
(F) REMOVING THE TONED ELEMENT FROM THE RECEPTOR MATERIAL.
Multicolor images on a receptor material using a multiple, colored, photohardenable element can be easily provided by a process comprising the steps of:
(a) applying a photohardenable layer on a carrier material;
(b) exposing imagewise to actinic radiation the photohardenable layer to form imagewise tacky and non-tacky areas;
(c) toning the tacky areas of the layer by applying and adhering thereto a toner material comprising a heat transferable, sublimable dye or mixtures of dyes;
(d) repeating steps (a) to (c) one or more times, each time applying a photohardenable layer on the preceding layer and using a different color toner;
(e) placing the multicolored toned element in contact with the surface of a receptor material;
(f) heating for at least 5 seconds either the toned element, the receptor material, or both, while in contact to a temperature at which at least some of the dye sublimes and imagewise condenses on the receptor material, the temperature being below that which would melt or otherwise degrade either the photohardenable layer or the receptor material; and
(g) removing the toned element from the receptor material.
BRIEF DESCRIPTION OF THE DRAWING
The FIGURE is a cross-section of a multiple colored element in position for heat transfer of the image to a receptor material.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The process of this invention advantageously uses an image reproduction system which employs photohardenable elements, including photopolymerizable elements, to modulate adherence of the image readout colorant to the imaging layer(s). Such systems are known. A typical system is described in U.S. Pat. No. 3,854,950, the disclosure of which is incorporated by reference. The photohardenable elements comprise a layer of photohardenable composition on a removable support. Over the surface of the photohardenable layer opposite the support can be present a removable cover sheet which is less strongly adherent at room temperature to the photohardenable layer than is the base support.
In practicing a process of this invention, a colored image is produced on a receptor material as follows:
(1) On a carrier material, which can be paper, film, metal sheet or preferably the smooth side of cast-coated one side cover paper, such as Kromekote® manufactured by The Champion Paper Division of Champion International, is laminated a photohardenable layer which had been coated on a transparent removable support.
(2) Following lamination, the photohardenable layer is exposed imagewise through the transparent removable support. Preferably, such exposure occurs in a vacuum frame, as is common in the printing industry, to assure intimate contact between the transparency image and the sample to be exposed. The photohardenable layer exhibits a different degree of tackiness following exposure to actinic radiation.
(3) Following exposure, the transparent support is removed and discarded.
(4) Using any of the techniques known in applying toner material and toning the surface of a color proofing film, as for example is disclosed in U.S. Pat. No. 3,060,024 or in U.S. application Ser. No. 710,102, filed July 30, 1976, now abandoned, a toner comprising a sublimable dye which sublimes at a moderate to fast rate, preferably at a temperature between 120° C. to 220° C., is applied onto the exposed surface. The process may be operable, however, in the temperature range of 60° to 300° C. The toner adheres preferentially onto the tacky areas of the surface and is wiped off the non-tacky sections.
Typical dyes, which may be used pure as toners, or combined with a resin matrix carrier, are the dyes classified in the Colour Index under the general title "Disperse dyes". Chemically, these dyes for the most part belong to one of the three following classes:
(a) Nitroarylamines
(b) Azo, and
(c) Anthraquinone.
They generally contain an amino group, with or without substituents and do not contain a solubilizing sulfonic group. The following is a non-exclusive list of commercially available disperse dyes useful in the practice of this process by trade name as well as the manufacturer of each.
Acetamine dyes (E. I. du Pont de Nemours & Co.)
Acetoquinone dyes (Francolor)
Celliton dyes (B.A.S.F.)
Artisil dyes (Sandoz)
Cibacete dyes (Ciba)
Setacyl dyes (Geigy)
Dispersol-Durand dyes (I.C.I.)
Esteroquinone dyes (Francolor)
Latyl Dyes (E. I. Du Pont de Nemours & Co.)
Foron Dyes (Sandoz)
Palanil Dyes (B.A.S.F.)
Resoline Dyes (Bayer)
Other suitable dyes will be found in U.S. Pat. No. 3,508,492 and the patents referred to therein.
In a preferred embodiment, the toner material used is a disperse dye dispersed in a resin matrix, e.g., cellulose acetate, cellulose acetate butyrate, polyvinyl chloride, polystyrene, polymethyl methacrylate, etc., said toner having a size distribution within the range 0.2 to 30 microns and not more than 50% of the particles being less than one micron equivalence spherical diameter. Preferably, more than 50% of the particles will have a size of 1 to 10 microns to limit background staining as taught in U.S. Pat. No. 3,620,726.
(5) Subsequent to the application of the toner material to the imaged surface, it is preferred that an additional element comprising a layer of photohardenable material on a transparent removable support be laminated over the toned surface. The laminated element is then exposed to actinic radiation for a longer period of time than the imagewise exposure. Typical exposure times are 10 times the imagewise exposure or more. The transparent support is then removed from the exposed element and is discarded.
(6) In the production of multicolored images, the process is repeated as many times as there are desired colors, each time using a different transparency and toner. For a typical four color reproduction, the first step may be to generate the black layer through steps (1) through (4) above, then repeat steps (1) through (4) three more times to overlay the cyan, yellow, and magenta layers, finishing with step (5). In some instances multicolor reproductions can be produced from a single photohardenable layer. The image must be one that permits a tacky area to be toned with one toner and one or more other tacky areas to be toned with different color toners without overlap of toner.
The FIGURE illustrates a typical two color proof ready for the heat transfer step. On a paper carrier material 1 is present a first image bearing photohardenable layer 2 which is imagewise exposed to provide imagewise tacky and non-tacky areas on the layer 2. Toner 3 comprising a sublimable dye is adhered to the tacky areas of layer 2. Over the first photohardenable layer is an intermediate photohardenable layer 4 which is non-imagewise exposed and polymerized. Intermediate layer 4 protects the toned surface of layer 2. A second image bearing photohardenable layer 5 which is imagewise exposed to provide imagewise tacky and non-tacky areas on the layer is present on intermediate layer 4. Toner 6 comprising a sublimable dye different in color from Toner 3 is adhered to the tacky areas of layer 5. A final outer photohardenable layer 7 which is non-imagewise exposed and polymerized is present over toned layer 5. The element is in contact with a receptor material 8 to which the two color image is transferred upon the application of heat sufficient to sublime the dyes on toners 3 and 6.
(7) The prepared color proof is placed in contact with the surface of the receptor material to which it is desired to heat transfer the image. Pressure and heat are then applied for a brief period of time at the end of which both the pressure and heat are removed and the proof and receptor material are separated. Surprisingly, it is observed that the sublimable dyes have diffused through the various imagewise exposed areas of the photohardenable layers, including the non-imagewise exposed barrier layers and have transferred imagewise to the receptor material. Where a multilayered multicolored proof is used, the resulting image is a multicolored reproduction of the original exhibiting excellent color balance and resolution.
While the amount of pressure employed is not critical, there is a minimal amount of required pressure (M.R.P.) to assure good transfer, above which the effect of transfer pressure ceases to be a color density variable. Such M.R.P. varies with the type and texture of the receptor material and is determinable experimentally as follows:
(a) A transfer is made starting with the lowest pressure (P 1 ) setting and a reading is taken of a solid area using a densitometer (D 1 ).
(b) The pressure is increased to a higher setting P 2 and maintaining the transfer time and temperature constant a second transfer and reading are effectuated resulting to a second density value D 2 .
(c) The process is repeated until D n =D n+1 at which point the M.R.P. has been determined. In practice, the M.R.P. may vary, for example, from 0.5 to 3.0 psi (0.035 to 0.21 kg/sq.cm.) depending on fabric construction or surface texture of the receptor material and transfer equipment, for a given dwell time and temperature.
It is believed that upon application of the heat (i.e., through a heating platen or drum) to the Kromekote® paper and photohardenable layers, the following occurs resulting in the dye transfer onto the receiving surface.
(1) The temperature of the paper, photohardenable layers and receptor material rapidly approach the temperature of the heating platen or drum.
(2) With increased temperature, the vapor pressure of the sublimable disperse dye increases and a dynamic equilibrium is established between the dye vapor flow rate, to and from the solid dye crystals in the toner, through the exposed photohardenable layers, the paper carrier and the dye vapor above the paper surface.
(3) The sublimation process continues until the dye vapor atmosphere above the paper reaches supersaturation, at which point the supersaturation is relieved by vapor condensation on the surface of the receptor material.
(4) As soon as this dye concentration gradient is set up on the surface of the receptor material, the process of molecular diffusion of the dye into the interior of the receptor material begins.
(5) This dye transfer mechanism of sublimation, supersaturation, and condensation proceeds in a state of dynamic equilibrium until the partial vapor pressures of the dye vapor over the printed paper and over the receptor material reach equilibrium. Typical transfer times, while dependent on the particular dye and temperature of transfer, as well as on the nature and texture of the carrier and receiving elements vary between 5 seconds and one minute or more. The method described above, used for determining M.R.P., may also be used at a fixed pressure and temperature to experimentally determine the optimum transfer time in a particular case.
Suitable receptor materials are those which accept a sublimable dye. Such materials may have a surface comprising polymer organic compounds, which can be in the form of plastic foils, synthetic fibers, or treated natural fibers and fibers having a synthetic outer layer. Metal surfaces also make useful receptors but must accept the dye, e.g., be porous. Especially useful are homo- or copolymers of vinyl acetate, vinyl alcohols, vinyl chloride, vinylidene chloride, acrylic acid compounds, alkylenes, alkylene-carboxylic acids and -esters, styrene, α-methyl styrene, maleic acid compounds, cellulose esters and ethers such as ethyl cellulose, benzyl cellulose, cellulose propionate, or -acetobutyrate, polyesters of terephthalic acid, carbonic acid, adipic acid, as well as polyamides. Typical commercially available materials include nylon 6 or 66, Perlon®, Orlon®, Dralon®, Dacron®, Terylene®, etc.
Heat transfer images produced by the process of the invention show excellent image quality and color printing. Resolution and print quality is comparable to images produced by high quality printing; however, the preparation of a printing plate, or a number of printing plates in the case of multiple color images, has been eliminated. Registration problems incident to sequential printing are absent, since the multicolored image is produced directly on the photohardenable element, and all colors are transferred simultaneously. The sophisticated technology incident to color proofing is advantageously exploited resulting in a practical method to form color proofs or produce limited quantities of heat transferred prints on various receptor materials with a minimum of expense and effort.
Some of the applications contemplated for the process of this invention include color proofs of proposed fabric patterns and specialty packaging products on films or foils, novelty items, e.g., color printed card table tops, color prints, designs, nameplates on film covered metals, cartographic transfers, overlays for overhead projectors, advertising slogans on fabrics, reflection and transparent display signs on a variety of rigid and flexible supports.
EXAMPLES OF THE INVENTION
The following examples illustrate this invention.
EXAMPLE 1
A photopolymerizable element similar to that described in Example II of U.S. Pat. No. 3,854,950, hereinafter referred to as a color proofing film, was prepared having a 0.0003 inch (˜0.00076 cm) photopolymer layer coated on a 0.0005 inch (˜0.0013 cm) polyethylene terephthalate support, with the other side of the photopolymer layer covered with a 0.00075 inch (˜0.0019 cm) polypropylene film as a cover sheet. As in Example II of U.S. Pat. No. 3,854,950 the cover sheet was removed and the photopolymer layer was laminated to Kromekote®, (cast coated on one side) paper carrier material. The laminate was placed in a vacuum frame with the photopolymerizable layer facing the exposure source. A transparency comprising a blue printer, separation, halftone positive was placed over the photopolymerizable layer, and following the application of vacuum for one minute, the laminate was exposed to actinic radiation for approximately 20 seconds.
The laminate was then removed from the vacuum frame and the polyethylene terephthalate support removed to expose the photopolymerizable layer laminated on the Kromekote® paper. Toner particles of processed Latyl® Blue BCN dye (C.I. disperse Blue 56) were applied over the exposed surface. The toner adhered to the non-exposed areas and was wiped off the exposed areas. Following toning, the toned layer was further exposed to actinic radiation to develop a hardened, non-tacky surface. The toned and hardened photopolymerizable layer was placed in contact with a Dacron® polyester fiber woven fabric. Heat and pressure were applied for 45 seconds, raising the temperature of the layer to about 220° C. The layer was then separated from the fabric. It was observed that a faithful mirror image reproduction of the transparency had transferred from the layer to the fabric. The image had good color density and image resolution. No texture change could be detected on the imaged areas of the fabric, indicating that substantially no polymer had transferred from the layer onto the fabric.
EXAMPLE 2
A multiple color image was produced on a Kromekote® paper carrier by repeating the laminating, exposing, toning and hardening steps three times and using a different color toner for each toning step. The following procedure and dyes were used.
(a) A color proofing film as described in Example 1 was laminated to a Kromekote® paper carrier, and the film was hardened by exposing to ultraviolet actinic radiation. The polyethylene terephthalate support sheet was removed and a second color proofing film was laminated over the hardened photopolymerizable first layer.
(b) A positive, yellow, half-tone separation transparency was placed over the laminate of step (a) in a vacuum frame. Vacuum was applied for 1 minute, then the laminate was exposed through the transparency for 20 seconds to ultraviolet radiation.
(c) The exposed laminate of step (b) was removed from the vacuum frame, the polyethylene terephthalate support was removed, and the exposed photopolymerizable layer was toned with processed Latyl® Yellow 3G dye (CI Disperse Yellow 54).
(d) A third color proofing film was laminated over the Yellow-toned layer, and similarly exposed in a vacuum frame to ultraviolet radiation through a magenta, halftone, positive transparency. The exposed laminate was then toned as before with processed Latyl® Cerise N (C.I. Disperse Red 60).
(e) A fourth color proofing film was laminated over the magenta-toned layer and the exposure process was repeated using a cyan, halftone, positive transparency. Processed Latyl® Blue BCN (C.I. Disperse Blue 56) was used as toner for this layer.
(f) A fifth color proofing film was then laminated over the cyan-toned layer, and was exposed uniformly to ultraviolet radiation in the vacuum frame without an image transparency to generate a hardened, non-tacky protective layer over the toned layers.
(g) The polyethylene terephthalate support was removed and the toned laminate was placed in contact with a receptor material consisting of a piece of woven Dacron® fabric. The combination was subjected to heat of 220° C. and sufficient pressure to maintain good contact between fabric and toned laminate for 60 seconds, whereupon the heat and pressure were removed. The fabric was observed to bear a multicolored mirror image of the original which exhibited good resolution, good color balance and good saturation.
When the time for heat transfer was increased to 90 seconds, the transferred image exhibited excellent color saturation, with no deterioration in the color balance or resolution.
EXAMPLE 3
A color proofing film was laminated to Kromekote® paper as in Example 1 above. It was subsequently placed in a vacuum frame with a halftone transparency over it, and vacuum was applied for a period of one minute. The photopolymerizable layer was exposed through the test transparency to ultraviolet radiation for 20 seconds whereupon the laminate was removed from the vacuum frame and the polyethylene terephthalate cover sheet stripped off the exposed layer. An acrylic pad was first dipped in a container containing a toner material of dyed cellulose acetate having an average particle size between 1 and 10 microns. The dye used was Du Pont Latyl® Yellow 3G (C.I. Disperse dye 54). The acrylic pad was then used to apply and distribute the toner over the exposed, photopolymerizable layer. Toner adhered to the unexposed areas of the image and was wiped off the exposed surfaces. A second color proofing film was laminated over the toned surface and the laminate placed in the vacuum frame, vacuum was applied for one minute and then the laminate was exposed to ultraviolet radiation for 400 seconds. The polyethylene terephthalate support was removed and the exposed laminate was placed in contact with a piece of Dacron® fabric. Heat and pressure sufficient to raise the laminate temperature to about 200° C. were applied to the laminate for a period of 10 seconds at which time the laminate and fabric were separated. A good quality yellow mirror image of the original had transferred to the fabric.
EXAMPLE 4
A multiple color image was produced on Kromekote® paper as follows: On a sheet of Kromekote® paper was laminated a first color proofing film which was then placed in a vacuum frame and after a one minute vacuum application was exposed for 15 seconds through a black, separation, halftone transparency. The polyethylene terephthalate support was removed. Using the procedure described in Example 3, the photopolymerizable layer was toned with a dyed cellulose acetate toner wherein the dyes used were a combination of two dyes, a Sinclair and Valentine Brown Dye 50-1301-06 and a disperse blue dye (C.I. 14). The toned image had a generally black appearance.
A second color proofing film was laminated over the black, toned layer to provide a barrier layer between the black toned layer and subsequent layers. This barrier layer was non-imagewise exposed in a vacuum frame following a one minute vacuum application to ultraviolet radiation for a period of about 200 seconds, whereupon the exposed laminate was removed from the vacuum frame, the polyethylene terephthalate support was removed, and a third color proofing film laminated thereon.
The third color proofing film was exposed in a vacuum frame as described above through a cyan, halftone, separation transparency to ultraviolet radiation for 15 seconds. The polyethylene terephthalate support was removed. The exposed photopolymerizable layer was then toned as described in Example 3 using a cyan dyed, cellulose acetate toner wherein the dyes used were a combination of two dyes, a Sinclair & Valentine Blue dye No. 50-0305-06 and a disperse blue dye (C.I. 14).
The procedure was repeated and a fourth color proofing film was laminated over the third and exposed through a yellow, halftone, separation transparency. The exposed layer, again after removal of the support, was toned with a similar toner as described before, wherein the dye used was Latyl® Yellow 3G (C.I. disperse dye No. 54). A fifth layer was then produced as described before, using a magneta, halftone, separation transparency and toner particles dyed through the use of disperse dyes (C.I. 17) and (C.I. 60). A final sixth layer was laminated over the toned laminate and was given a non-imagewise exposure for 400 seconds to provide a protective overlayer.
After stripping the polyethylene terephthalate support, the laminate was placed in contact with a Dacron® fabric and heated to about 200° C. for 60 seconds. Upon separation, it was observed that a mirror image of the four color original had transferred to the fabric and that the transferred image exhibited excellent color balance and resolution. The cloth texture did not appear any different in the imaged and non-imaged areas.
EXAMPLE 5
A color proofing film of the type disclosed in U.S. application Ser. No. 583,456, filed June 3, 1975, now U.S. Pat. No. 4,019,821, granted Apr. 26, 1977, was used to produce a three color image following the process described in Example 4 above, but with the black layer and the barrier layer steps omitted. The cyan layer was exposed for 9 seconds, the yellow for 12 seconds, the magenta for 12 seconds and the protective overlayer for 80 seconds. The same blue, yellow, and magenta toners as in Example 4 were used. The final laminate was placed in contact with a piece of Dacron® cloth and subjected to 200° C. for 60 seconds. The resultant image on cloth shows reasonable color balance and density.
EXAMPLE 6
Using the procedure described in Example 3, a single color image was produced on a Kromekote® carrier. Without removing the polyethylene terephthalate support, the laminate was subjected to a temperature of 204° C. for 60 seconds under 3 psi (0.21 kg/sq.cm.) pressure in contact with a piece of Dacron® cloth. Upon removal of the cloth and support, both bore a mirror image of the transparency.
EXAMPLE 7
Using the procedure described in Example 4, a multicolor image was produced on a Kromekote® carrier. The multicolor image was placed in contact with a piece of white nylon fabric and subjected to a temperature of 200° C. for 60 seconds. Color balance, image resolution and density of the multicolor image were satisfactory.
EXAMPLE 8
Using the procedure described in Example 4, a multicolor image was produced on a Kromekote® carrier. The multicolor image was placed in contact with a piece of white cellulose acetate fabric and subjected to a temperature of 177° C. for 90 seconds. Color balance, image resolution and density of the multicolor image were satisfactory.
EXAMPLE 9
Using the procedure described in Example 3, except that the cyan toner of Example 4 was used, a single color image was produced on a Kromekote® carrier. The image was transferred to a piece of preheated Dacron® fabric as follows:
1. The piece of Dacron® fabric was subjected for 30 seconds to a temperature of 204° C.
2. Simultaneously, the Kromekote® carrier was preheated for 10 seconds by means of hot air at about 65° C.
3. The imaged Kromekote® carrier was placed in contact with the preheated Dacron® fabric and subjected to a temperature of 204° C. for 5 seconds. A mirror image of the original was transferred to the fabric.
EXAMPLE 10
Using the procedure described in Example 3, except that the toner used was a crude ground dye Latyl® Yellow 3G (C.I. Disperse Dye 54), a single color image was produced on a Kromekote® carrier. The thermal transfer was to a piece of white Dacron® fabric at a temperature of 200° C. for 60 seconds. A mirror image of the original was transferred to the fabric.
EXAMPLE 11
Example 4 was repeated except that the receptor material was an unsealed anodized aluminum plate, about 0.125 inch (3.18 mm) in thickness. The four color laminate when placed in contact with the receptor was heated to about 200° C. for 120 seconds. Upon separation, it was observed that a mirror image of the four color original had transferred to the anodized aluminum. The transferred image exhibited excellent resolution and good color balance. | Process for forming at least a single color image on a receptor material using photohardenable elements which contain one or more imagewise photohardenable layers toned with a toner material comprising a sublimable dye or mixture of dyes, the process comprising heating for at least 5 seconds, while in contact with a receptor material, either the toned element, the receptor material, or both, to a sublimation temperature of said dye and thereby cause at least a portion of the dye to sublime imagewise and condense on the receptor material. The temperature should not degrade the receptor or photohardenable layer. At least one non-imagewise exposed photohardenable layer may be present in the toned element. The process is useful in forming color proofs or proposed fabric patterns, color prints, projector overlays, etc. | 6 |
TECHNICAL FIELD
[0001] The invention relates to wheel assemblies for moving trampolines.
BACKGROUND
[0002] Many homes have a trampoline set up for use by family members, typically on a backyard lawn surface. Such trampolines are typically supported on opposed U-shaped legs, but the size, shape and number of legs is highly variable depending on the manufacturer, size and shape of the trampoline. To avoid having the grass under the trampoline die, and to permit the grass to be cut, it is necessary to periodically move a trampoline which is set up on a user's lawn. This is usually done by lifting or dragging the trampoline, which is difficult for a person to do alone.
[0003] It is known to attach wheel assemblies to trampolines to facilitate moving them. It is known to provide a pair of wheel assemblies, each having two or three wheels. The wheel assemblies are designed for indoor use, such as in gymnasia. Such wheel assemblies are designed to fit into receptacles provided in the trampoline frame when the trampoline is moved, and are removed when the trampoline is ready to be used. Examples are shown in U.S. Pat. Nos. 3,116,809 and 3,156,318. Such assemblies are difficult to store when the trampoline is in use, and not all trampoline designs may be suited or adapted to have one of these assemblies attached to it.
[0004] There is therefore a need for a wheel assembly which can be used on any design of trampoline and which can remain attached to the trampoline during use.
[0005] The foregoing examples of the related art and limitations related thereto are intended to be illustrative and not exclusive. Other limitations of the related art will become apparent to those of skill in the art upon a reading of the specification and a study of the drawings.
SUMMARY
[0006] The following embodiments and aspects thereof are described and illustrated in conjunction with apparatus which are meant to be exemplary and illustrative, not limiting in scope. In various embodiments, one or more of the above-described problems have been reduced or eliminated, while other embodiments are directed to other improvements.
[0007] The invention therefore provides a wheel assembly for attachment to a trampoline leg to enable a trampoline to be rolled on a surface, comprising: i) an attachment element having means for securing the wheel assembly to a trampoline leg; ii) an elongated element mounted on the attachment element and movable in a direction having a component perpendicular to the surface; iii) an axle-mounted wheel pivotally connected to the elongated element; and iv) means for reversibly moving the elongated element from a first position in which the wheel is raised relative to the attachment element to a second position in which said wheel is lowered relative to the attachment element.
[0008] In addition to the exemplary aspects and embodiments described above, further aspects and embodiments will become apparent by reference to the drawings and by study of the following detailed descriptions.
BRIEF DESCRIPTION OF DRAWINGS
[0009] Exemplary embodiments are illustrated in referenced figures of the drawings. It is intended that the embodiments and figures disclosed herein are to be considered illustrative rather than restrictive.
[0010] FIG. 1 is a front perspective view of a first embodiment of the invention.
[0011] FIG. 2 is a rear perspective view of the embodiment shown in FIG. 1 .
[0012] FIG. 3 is a perspective view of the embodiment shown in FIG. 1 attached to a trampoline leg in the wheel up position.
[0013] FIG. 4 is a perspective view of the embodiment shown in FIG. 1 attached to a trampoline leg in the wheel down position.
[0014] FIG. 5 is a cross-section perspective view taken along line B-B of FIG. 1 .
[0015] FIG. 6 is a top cross-section view taken along line B-B of FIG. 1 .
[0016] FIG. 7 is a front elevation view of a second embodiment of the invention.
[0017] FIG. 8 is a rear elevation view of the embodiment shown in FIG. 7 in the wheel down position.
[0018] FIG. 9 is a cross-section view taken along line A-A of FIG. 8 .
[0019] FIG. 10 is a top view of the embodiment shown in FIG. 8 in the wheel down position.
[0020] FIG. 11 is a perspective view of a third embodiment of the invention.
[0021] FIG. 12 is a front elevation view of the embodiment shown in FIG. 11 in the wheel up position.
[0022] FIG. 13 is a rear elevation view of the embodiment shown in FIG. 11 in the wheel down position.
[0023] FIG. 14 is a detail rear perspective view of the embodiment shown in FIG. 11 in the wheel up position.
[0024] FIG. 15 is a perspective view of a fourth embodiment of the invention shown in the wheel up position.
[0025] FIG. 16 is a perspective view of the embodiment of the invention shown in FIG. 15 in the wheel down position.
[0026] FIGS. 17A , 17 B are schematic views in cross-section of the embodiment shown in FIG. 15 illustrating the operation of the locking pin.
DESCRIPTION
[0027] Throughout the following description specific details are set forth in order to provide a more thorough understanding to persons skilled in the art. However, well known elements may not have been shown or described in detail to avoid unnecessarily obscuring the disclosure. Accordingly, the description and drawings are to be regarded in an illustrative, rather than a restrictive, sense.
[0028] With reference to FIG. 1 , a first embodiment of the pivoting wheel assembly is designated by numeral 10 . It comprises a leg 22 , which may be a hollow tube for lightness, for example manufactured from aluminum. Wheel 12 is mounted on axle 14 which is carried on caster 6 which is rotatably secured on the lower end of leg 22 . The upper end of leg 22 is fastened, for example by welding, to rotating ring 21 which is mounted for rotation on cylindrical hub 19 . Hub 19 is fixed to base plate 11 . Rotating ring 21 is fastened, for example by welding, to ring plate 23 which is retained on hub 19 by retaining ring 5 and washer 3 . Ring plate 23 has two holes 17 which are sized to receive retractable pin 16 . Pin 16 slides in holes 18 of pin bracket 13 and plate 11 . Pin 16 is biased into holes 17 by a spring 15 and has secured to its outer end a pin ring 4 to permit the user to withdraw the end of pin 16 from hole 17 .
[0029] Base plate 11 has holes 20 through which are removably secured U-shaped clamps 25 which have threaded ends for securing in holes 20 using threaded nuts. To use the device, as shown in FIG. 3 , with the leg in the wheel up position shown, the base plate 11 is secured to trampoline leg 30 at the appropriate height by clamps 25 . When it is desired to move the trampoline, the user pulls pin 16 out of hole 17 using pin ring 4 , which permits rotating ring 21 and leg 22 to rotate. By raising the trampoline leg slightly, leg 22 is rotated 180 degrees so that pin 16 snaps into the second hole 17 and the trampoline leg 30 is then supported on wheel 12 above the ground, as shown in FIG. 4 . Preferably a minimum of two or three wheel assemblies 10 , and most preferably four wheel assemblies 10 are thus attached to the trampoline legs at spaced locations and when all the wheels are in the down position the trampoline can be readily rolled to a new location. When it is desired to set the trampoline down for use at a location, the process is reversed by the user pulling pin ring 4 to allow the leg 22 to rotate back to the wheel up position. The wheel assemblies 10 can remain on the trampoline legs in the wheel up position without disturbing the use of the trampoline.
[0030] A second embodiment of the pivoting wheel assembly is designated by numeral 70 in FIGS. 7 through 10 . Wheel and pivoting caster assembly 82 is mounted on the end of lever 75 which has grip 74 . Lever 75 is fastened, for example by welding, to bushing 80 which rotates on axle 81 , 83 , 85 which is fixed to base plate 78 . Bushing 80 is welded to locking ring 84 which has holes 72 for receiving a locking pin 73 . Pin 73 is biased into holes 72 by a spring (not shown) and has a handle end 76 which slides in housing 86 . Base plate 78 has holes for removably receiving U-shaped clamps 77 , 79 .
[0031] To use this embodiment, as in the first embodiment, with the lever 75 in the wheel up position shown in FIG. 7 , the base plate 78 is secured to trampoline leg 30 at the appropriate height by clamps 77 , 79 . When it is desired to move the trampoline, the user pulls pin 73 out of hole 72 using handle 76 , which permits rotating ring 84 and lever 75 to rotate. By raising the trampoline leg slightly, lever 75 is rotated 90 degrees to the position shown in FIG. 8 so that pin 73 snaps into a second hole 72 and the trampoline leg 30 is then supported on wheel 82 above the ground. Preferably four wheel assemblies 70 are thus attached to the trampoline legs at four locations and when all the wheels are in the down position the trampoline can be readily rolled to a new location. When it is desired to set the trampoline down for use at a location, the process is reversed by the user pulling out pin 73 and rotating lever 75 back ninety degrees to the wheel up position. The wheel assemblies 70 can remain on the trampoline legs in the wheel up position.
[0032] A third embodiment of the pivoting wheel assembly is designated by numeral 110 in FIG. 11 . Wheel and pivoting caster assembly 122 is mounted on the end of telescoping tube 111 . Tube 111 telescopes inside outer tube 113 which is secured to clamping plate 116 by bolts 121 , 125 or the like. Bracket 112 is fastened, for example by welding, to tube 113 . Lever handle 114 rotates on pin 118 which is fixed in bracket 112 and second pin 118 which connects lever handle 114 to lever driver 115 . The lower end of lever driver 115 rotates on pin 119 in tube 111 . Clamping plate 116 has holes for removably receiving U-shaped clamps 131 , 132 ( FIG. 14 ). To accommodate trampoline legs of differing angle, bolt 125 slides in slot 127 in clamping plate 116 .
[0033] To use this embodiment, as in the first embodiment, with the lever handle 114 in the wheel up position shown in FIG. 12 , the clamping plate 116 is secured to trampoline leg 30 at the appropriate height by clamps 131 , 132 . When it is desired to move the trampoline, the user lowers handle 114 to the position shown in FIG. 13 , which lowers wheel and caster 122 into contact with the ground and raises the trampoline leg above the ground. Preferably four wheel assemblies 110 are thus attached to the trampoline legs at four locations and when all the wheels are in the down position the trampoline can be readily rolled to a new location. Padlock hole 130 is provided to permit the assembly to be locked in the wheel up position so that children cannot easily move the trampoline. When it is desired to set the trampoline down for use at a location, the process is reversed by the user rotating handle 114 back ninety degrees to the wheel up position. The wheel assemblies 110 can remain on the trampoline legs in the wheel up position.
[0034] As will be apparent from FIG. 11-14 , the relative location of the axes created by pins 118 to lever driver 115 and pin 119 causes lever handle 114 to reach an over-center point of rotation when rotated to the position shown in FIG. 13 which retains lever handle 114 securely in that position until a rotational force is applied to overcome the resistance created by the over-center relationship and thereby continue rotation of lever handle 114 to the position shown in FIG. 11 . Similarly the relative location of the axes created by pins 118 to lever driver 115 and pin 119 , and the indentation 123 in the edges of lever driver 115 , causes lever handle 114 to reach an over-center point of rotation when rotated to the position shown in FIG. 12 which retains lever handle 114 securely in that position until a rotational force is applied to overcome the resistance created by the over-center relationship and thereby continue rotation of lever handle 114 to the position shown in FIG. 11 . In addition, one or more dimples may be formed on the inner surface of handle 114 between the two pins 118 , and possibly also corresponding indentations on the outer surface of lever driver 115 , to cause a frictional engagement when handle 114 is in the position shown in FIG. 12 in order to further retain lever handle 114 securely in that position until force is applied to rotate it.
[0035] A fourth embodiment of the pivoting wheel assembly is designated by numeral 150 in FIG. 15 . Wheel and pivoting caster assembly 152 is mounted on the end of telescoping inner tube 151 . Tube 151 telescopes inside outer tube 153 and has a locking pin 154 and handle 157 secured thereto and extending therefrom. Outer tube 153 has a pin-engaging slot 155 and is secured to mounting plate 156 by welding or the like. Mounting plate 156 has holes for removably receiving U-shaped clamps 160 , 162 which have threaded ends which extend through holes in saddle-shaped brackets 164 , 166 and are secured using threaded nuts.
[0036] To use the device, as shown in FIG. 15 , the leg is in the wheel up position shown in FIG. 15 and FIG. 17B , with the locking pin 154 locked in the upper notch 168 of slot 155 due to the weight of the inner tube. The mounting plate 156 is secured to trampoline leg 30 at the appropriate height by tightening clamps 160 , 162 and brackets 164 , 166 against leg 30 . When it is desired to move the trampoline, the user lifts trampoline leg 30 and raises locking pin 154 out of notch 168 using handle 157 to lift inner tube 151 , and rotates inner tube 151 counterclockwise, which permits locking pin 154 to enter the vertical length of slot 155 . The weight of inner tube 151 and wheel 152 then causes inner tube 151 to telescope downwardly relative to outer tube 153 until locking pin 154 reaches the bottom 170 of slot 155 . The trampoline leg 30 is then lowered and supported on wheel 12 above the ground, as shown in FIG. 16 and FIG. 17A with locking pin 154 held in notch 172 by the weight of the trampoline. Preferably a minimum of two or three wheel assemblies 150 , and most preferably four wheel assemblies 150 are thus attached to the trampoline legs at spaced locations and when all the wheels are in the down position the trampoline can be readily rolled to a new location. When it is desired to set the trampoline down for use at a location, the process is reversed by lifting the trampoline, thereby returning locking pin 154 to position 170 . The user then lifts handle 157 to raise the inner tube 151 in slot 155 , and then rotate the locking pin 154 to rest in notch 168 . The wheel assemblies 150 can then remain on the trampoline legs in the wheel up position without disturbing the use of the trampoline.
[0037] While it is preferred that the wheel assembles according to the invention can be quickly secured to and removed from the trampoline legs such as by using threaded clamps and bolts, the invention can also function wherein the wheel assembly is more permanently secured to the trampoline leg, such as by screwing into the trampoline or welding to the leg.
[0038] While a number of exemplary aspects and embodiments have been discussed above, those of skill in the art will recognize certain modifications, permutations, additions and sub-combinations thereof. It is therefore intended that the following appended claims and claims hereafter introduced are interpreted to include all such modifications, permutations, additions and sub-combinations as are within their true spirit and scope. | A wheel assembly for attachment to the leg of a trampoline has means for moving the wheel from a first raised position where the wheel is not supporting the trampoline leg above the ground, to a second position where the wheel is supporting the trampoline leg above the ground. In that way the trampoline can be rolled on wheels without having to subsequently remove the wheel assemblies for storage. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims benefit of priority of U.S. Provisional Patent Application Ser. No. 60/170,772, entitled “Adjustable Flexibility Golf Club Shaft,” filed on Dec. 15, 1999.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to golf clubs, and more particularly to a wood or iron having a shaft whose flexibility can be incrementally increased or decreased while playing or practicing.
2. Description of the Related Art
A golf swing is a set of highly complex body movements requiring precise coordination of the hands, arms, shoulders, torso, hips, legs and knees, occurring in proper sequence. As the body coils and then uncoils, power is transferred from the body through the arms and wrists to the club grip, along the shaft, into the clubhead, and into the ball.
In a full range of motion swing, the position of the leading arm (i.e., the left arm of a right-handed golfer, or the right arm of a left-handed golfer) is critically important. The backswing is performed as a unitary motion, the entire front side of the body moving together as the knees, hips, trunk and shoulders are rotated, with the leading arm pushing the trailing arm back, and the leading elbow and arm remaining straight. To achieve the broadest possible swing arc, the club is swung straight back from the ball, without breaking the wrists, for as long as the turning of the shoulders and hips will allow. The golfer tries to keep the clubface square to the target line for as long as possible without turning the hands and wrists under, and also tries to keep the leading arm and club in a straight line until the momentum of the swinging clubhead causes the wrists to begin cocking naturally as they reach about hip height. The angle between the hands and shaft is maintained, with the trailing arm bending at the elbow and the leading arm remaining straight. The one-piece motion forces the shoulders to turn from the very beginning of the backswing and ensures they will go on turning until the top of the swing is reached. As the arms stretch and turn, the hips are also forced to turn. At the top of the backswing, the shoulders have turned about twice as far as the hips, the leading arm is straight, and the forearms have rotated. The leading forearm is pronated, i.e., rotated clockwise for a right-handed golfer or rotated counterclockwise for a left-handed golfer, and the trailing forearm is supinated, i.e., rotated counterclockwise for a right-handed golfer or rotated clockwise for a left-handed golfer, causing cocking of the wrists with the shaft generally perpendicular to the leading forearm. Ideally, the back of the leading hand, the wrist and the forearm are in a straight line, with the shaft parallel to the ground and to the target line, and the clubhead pointing toward the target.
As the arms reach their fullest extension and the weight of the clubhead causes the wrists to attain their maximum cocking but before the hands reach their highest level or the shoulders finish turning, the lower torso, hips, legs and feet already have initiated the downswing. The golfer pushes hard off the inside of the back foot, throwing weight to the inside of the front foot. The front knee is pulled laterally toward the target and is well forward of the ball before the hands have descended even a few inches. The wrists are kept cocked and the head is kept back behind the ball. The club is pulled into action by the uncoiling of the body and leading arm. Because of the movement of the lower body toward the target and the delay in uncocking the wrists, the arc traversed by the clubhead on the downswing is steeper than the arc on which the clubhead was taken back.
In the hitting zone the hips, which were moving laterally in the same forward direction as the knees, begin to turn with respect to the target line. By turning, the hips “clear” a path for the arms to swing past the body. The thrusting legs and hips, by forcing the shoulders to turn, accelerate the arms and club. Just before impact, a point is reached where no further acceleration is possible and, because of centrifugal force, the club must be released into the ball. At that point, the wrists are forced to uncock spontaneously.
As the wrists uncock and the back arm starts to straighten, the fully released clubhead whips toward the ball. At impact, the back of the leading hand faces the target, and the leading arm and shaft form a straight line so that the leading hand and arm are slightly ahead of the ball. As the clubhead swings through the ball toward the target, the leading arm is kept straight and moves directly toward the target. The golfer must avoid any independent turning or twisting of the club with the hands and wrists.
The release phase is entered just after impact. The trailing arm straightens, but there is no breaking down of the leading arm at the wrist or elbow. Nor is there independent rolling, turning or twisting of the hands, wrists or forearms, until the momentum of the club, combined with the turning body, forces the body to turn and swing to the opposite side of the target line. The leading arm is supinated and the trailing arm is pronated, the forearms being opposite to their rotational position at the top of the backswing.
As millions of golfers can attest, it is difficult to meld the separate motions comprising a full range of motion swing so as to achieve impact with the clubface generally square to the ball while the clubhead is moving at a high rate of speed. The present invention entails increasing clubhead speed by flexing the shaft to impart to potential energy additional to that accumulated during the backswing, which is converted into extra clubhead kinetic energy in the hitting zone and at impact.
Golf clubs having shafts with modifiable flexure are disclosed in the related art. U.S. Pat. No. 2,992,828 to W. A. Stewart discloses a club having a hollow shaft which is prestressed so as to remain relatively straight during the backswing and downswing, compared to a conventional shaft. In one embodiment a wire inside the shaft and adjacent to the leading edge is maintained under tension between plugs at the top and bottom ends of the shaft. The upper plug receives a bolt which when rotated causes the plug to act as a nut and travel upwardly on the bolt, increasing tension in the wire and thereby compressing the shaft leading edge. Tightening the wire tends to bow the shalt in a direction opposite to the direction the shaft would normally bend on the downswing. The wire is not tensioned sufficiently to bow the shaft but just enough to prestress the shaft or apply a bending stress in a direction opposite to the bending stress applied to the shaft during the downswing. In another embodiment an elongated column member extending the length of the shaft between upper and lower plugs has its trailing edge compressed by screwing a bolt down through the upper plug. This puts tension on the trailing side of the shaft, inducing a bending stress in the shaft opposite to the downswing bending stress.
U.S. Pat No. 4,685,682 to J. T. Isabell discloses a golf club connected to a mechanism which increases or decreases shaft flexibility by varying the tension in a wire extending between the handle and clubhead. The wire is offset from the shaft by a bridge which maximizes the effect of small changes in wire tension provided by movement of a threaded connection between the wire and clubhead. Increasing the tension in the mechanism decreases shaft flexibility; decreasing the tension increases flexibility. The device is used to determine the degree of shaft flexibility which maximizes an individual golfer's clubhead speed at impact, so that a set of clubs can be made that have the same flex characteristics.
U.S. Pat. No. 5,865,688 to S. W. Bae discloses a golf club having three flex points along its shaft. At each point, the shaft diameter expands to permit the shaft to flex at that point. When the club is swung, the shaft flexes from a high flex point (i.e., a location proximate to the handle) to a mid flex point to a low flex point (i.e., a location proximate to the clubhead).
U.S. Pat. No. 5,931,744 to L. E. Hackman discloses a method for reducing the stiffness of a hollow golf club shaft divided into three segments with each pair of segments connected by cone-shaped bands. The stiffness is changed by slicing or abrading the inner surface of the sidewall which typically is made from a flexible matrix material such as an epoxy, in which elongated, high strength graphite fibers are embedded. Most of the fibers are arranged longitudinally to provide strength and stiffness to resist bending of the shaft. Severing or removing selected fibers reduces the longitudinal stiffness.
None of these references address the problem of providing a golf club whose shaft easily can be made more or less flexible so that a golfer can determine through experimental trial which degree of flexibility best suits his particular full range of motion swing.
OBJECTS OF THE INVENTION
In view of the limitations of the related art, it is an object of the present invention to provide a golf club incorporating a device which allows a player to easily increase or decrease shaft flexibility when playing or practicing.
Another object of the invention is to provide a golf club whose shaft flexibility is adjustable with the adjustment calibrated so that any particular state within a range of flexibility can be accurately reproduced.
A further object of the invention is to provide a golf club whose shaft imparts kinetic energy to the clubhead in the hitting zone and at impact, additional to that generated in the downswing of a conventional club.
Yet another object of the invention is to provide a device altering shaft flexibility which is reliable to operate, inexpensive to manufacture, and readily adaptable to any club having a hollow shaft and clubhead.
Other objects of the invention will become evident when the following description is considered with the accompanying drawing figures. In the figures and description, numerals indicate the various features of the invention, like numerals referring to like features throughout both the drawings and description.
SUMMARY OF THE INVENTION
These and other objects are achieved by the present invention which in one aspect provides a golf club including a handle with a cavity rotatably connected to a hollow shaft upper portion symmetric about a longitudinal axis. The club further includes a hollow flexible shaft central portion attached to the shaft upper portion and a hollow shaft lower portion both symmetric about the axis. The club further includes means for altering the tension on a metallic wire disposed along the axis whose upper end is longitudinally adjustable within the handle cavity, and whose lower end is attached to the shaft lower portion at its lower end.
In another aspect the invention provides a golf club including a handle having a cap portion and a rotatable grip upper portion with a cylindrical interior surface determining a cavity. The club further includes: an upper wire-end retainer assembly including a cap-shaped outer tension tuner member having a cylindrical outer surface attached to the grip upper portion and an internal thread; a cylindrical collar having an outer surface and an internal thread which extends upwardly in a cylindrical inner tension tuner member having an external thread in threaded combination with the internal thread of the outer tension tuner member, and an internal thread; a cylindrical outer twist-prevention housing having an upper portion with a polygonal bore and an external thread in threaded combination with the collar internal thread; an inner twist-prevention housing having a central portion with a polygonal cross-section disposed between a cylindrical upper portion having a bore and an external thread smoothly slidable within the bore of the inner tension tuner member and a cylindrical lower portion with an external thread, with the central portion of the inner twist-prevention housing closely received within the polygonal bore; a cap-shaped clamp having an internal thread in threaded combination with the external thread of the inner twist-prevention housing, with the clamp tightening a bifurcated collet having opposed jaws received within the bore of the inner twist-prevention housing upper portion. The outer tension tuner member, cap-shaped clamp, collet, collar, inner tension tuner member, outer twist-prevention housing upper portion, and inner twist-prevention upper portion are received within the cavity, and the retainer assembly moves longitudinally within the cavity when the handle is rotated.
The club further includes: a hollow inflexible shaft upper portion, symmetric about a longitudinal axis and covered by a grip lower portion, into which the outer and inner twist-prevention housings extend; a hollow flexible shaft central portion, symmetric about the axis and attached to the shaft upper portion; and a hollow inflexible shaft lower portion attached to the shaft central portion and symmetric about the axis.
The club further includes a lower wire-end retainer assembly including a cylindrical sleeve extending in a cylindrical flange, and a ring received within the flange. The flange is rigidly attached to the shaft lower portion at its lower end.
The club further includes a metallic wire having opposed upper and lower ends disposed along the axis. The upper end is clamped between the collet jaws, and the lower end is attached to the ring. Moving the upper wire-end longitudinally alters the tension on the wire.
A more complete understanding of the present invention and other objects, aspects and advantages thereof will be gained from a consideration of the following description of the preferred embodiment read in conjunction with the accompanying drawings provided herein.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a golf club with a hollow shaft and clubhead according to the invention.
FIG. 2 is a longitudinal sectional view of the FIG. 1 club showing a longitudinally adjustable upper wire-end retainer assembly, a fixed lower wire-end retainer assembly, and a tension wire along the shaft longitudinal axis passing through and centered by six wire support members and clamped between the two assemblies.
FIG. 3 is a greatly enlarged sectional view taken along line 3 — 3 in FIG. 1 showing the FIG. 2 lower wire-end retainer assembly including a flanged sleeve and a ring, and the wire lower portion and two lowermost support members.
FIG. 4 is an exploded perspective view of the FIGS. 2, 3 lower wire-end retainer assembly, and a partial sectional view of the shaft lower portion.
FIG. 5 is an exploded perspective and partial sectional view of the FIG. 1 club handle and upper wire-end retainer assembly, the assembly including a cap-shaped outer tension tuner member, a cap-shaped collet clamp, a bifurcated collet, an inner twist-prevention housing, a collar extending upwardly in an inner tension tuner member, an outer twist-prevention housing, and a stop nut.
FIG. 6 is a greatly enlarged sectional view taken along line 6 — 6 in FIG. 1 showing the upper wire-end retainer assembly in its lowermost position resulting in minimum wire tension.
FIG. 7 shows the same view as FIG. 6 when the upper wire-end retainer is in its uppermost position resulting in maximum wire tension.
FIG. 8 shows one of a plurality of wire support members which is generally spherical and has therethrough a diametral bore.
DESCRIPTION OF THE PREFERRED EMBODIMENT
While the present invention is open to various modifications and alternative constructions, the preferred embodiment shown in the drawings will be described herein in detail. It is to be understood, however, there is no intention to limit the invention to the particular form disclosed. On the contrary, it is intended that the invention cover all modifications, equivalences and alternative constructions falling within the spirit and scope of the invention as expressed in the appended claims.
Where used herein, the word “connected” means that the two parts referred to (e.g., an external thread and a nut, or the mating of external and internal threads) can be readily separated after being joined together in an interlocking combination. Where used herein, the words “attached” and “attachment” mean that the two parts referred to are either fabricated in a single piece, or glued, clamped or crimped together. However, other forms of attachment may be suitable, consistent with simplicity of manufacture and reliability of operation.
Referring to FIGS. 1 and 2, a golf club 10 includes a rotatable handle 12 including a cap portion 13 and a grip upper portion 14 having a generally cylindrical interior surface 14 A and a textured symmetrically tapering exterior surface 14 B, the interior surface and cap portion determining a generally cylindrical cavity 16 . Club 10 further includes a hollow inflexible, downwardly tapering shaft upper portion 18 covered by a grip lower portion 20 having a textured symmetrically tapering exterior surface 20 B, a hollow flexible, downwardly tapering shaft central portion 22 , a hollow clubhead 24 (not part of the invention), and a hollow inflexible shaft lower portion 26 extending into and rigidly attached at an end 26 E to the clubhead. The handle and shaft upper, central and lower portions are symmetric about a common longitudinal axis. Cap portion 13 and grip portions 14 and 20 are conventionally made of a vulcanized rubber. Disposed along and within the shaft upper, central and lower portions is a plurality of wire support members 28 A, 28 B, 28 C, 28 D, 28 E, 28 F, progressively downwardly smaller in size, each of which is generally spherical and has therethrough a diametral bore 30 (see FIG. 8 ). Preferably, the number of support members is six; alternatively, five or seven members can be used. Alternatively, the members can be conical frustums sized to match the shaft's internal taper. The support members are fabricated from a low friction coefficient material such as a synthetic resinous fluorine-containing polymer or a polyvinyl chloride (PVC) and are rigidly attached to the shaft upper, central and lower portions, preferably adhesively, so that each bore is aligned with the longitudinal axis.
Referring to FIG. 2, a tension wire 32 is clamped at opposed upper and lower ends 32 U, 32 L to, respectively, an upper wire-end retainer assembly 34 closely received within the cavity 16 , and a lower wire-end retainer assembly 36 closely received within and rigidly attached to the shaft lower portion end 26 E. As best shown in FIGS. 3 and 6, the wire 32 is threaded through each bore 30 so that the wire is constrained to be disposed along the longitudinal axis. The bores are sized to closely receive but not frictionally interfere with the wire. Preferably, the wire is made from a stainless steel having a Rockwell hardness in the range 40-70, and has a constant diameter in a range from 0.060- to 0.090-inch. Alternatively, the wire is made from a carbon steel having a Rockwell hardness in the range 40-75 with a constant diameter in a range from 0.031- to 0.064-inch, or from tungsten having a Rockwell hardness in the range 75-80 with a constant diameter in a range from 0.031- to 0.055-inch.
Referring to FIGS. 3 and 4, lower wire-end retainer assembly 36 includes a generally cylindrical sleeve 40 extending in a generally cylindrical flange 42 , the sleeve and flange having therethrough a common bore 44 . A generally circular ring 46 is closely received within the flange. After inserting wire-end 32 L through the sleeve and into the ring and flange, the wire-end is rigidly attached to the retainer assembly by crimping the ring which, with the wire under tension, is disposed within the flange and constrained upwardly by the relatively narrow diameter sleeve. Flange 42 is rigidly attached to inner wall 26 W of lower shaft portion 26 at end 26 E, thereby providing additional structural integrity to the shaft-clubhead juncture.
Referring to FIGS. 5 and 6, the upper wire-end retainer assembly 34 includes a cap-shaped outer tension tuner member 50 having an internal thread 52 and an outer surface 50 S, a cap-shaped collet clamp 54 having an internal thread 56 , a bifuracted collet 58 having jaws 60 A, 60 B with generally planar inner faces 62 A, 62 B, respectively, and an inner twist-prevention housing 64 having a central portion 66 with a polygonal cross-section disposed between a generally cylindrical upper portion 70 with a bore 70 B and an external thread 72 , and a generally cylindrical lower portion 74 with an external thread 76 . Wire 32 is rigidly attached to the assembly 34 when wire-end 32 U is gripped between faces 62 A, 62 B with the collet 58 received within the bore 70 B and the clamp screwed onto member 62 by engaging threads 56 and 72 . As shown in FIG. 5 , handle 12 has a circumferential lower edge 12 E proximate to which are ten embossed numerical indicia “0, 1, 2, 3, 4, 5, 6, 7, 8, 9” evenly spaced around the circumference. Handle 12 is adhesively attached to surface 50 S so that when the handle is rotated through a preselected angle the tuner member 50 also rotates through that angle. As shown in FIGS. 5, 6 and 7 , cap portion 13 has therethrough an air release hole 13 H to allow air to escape from the hollow club 10 when the club is assembled.
Referring again to FIGS. 5 and 6, assembly 34 further includes a generally cylindrical collar 80 having an outer surface 80 S adhesively attached to grip upper portion 14 and an internal thread 82 . Collar 80 extends upwardly in a generally cylindrical inner tension tuner member 84 having an external thread 86 and a smooth bore 88 . Assembly 34 further includes a generally cylindrical outer twist-prevention housing 90 having an upper portion 92 with a polygonal bore 94 therethrough and an external thread 96 . Bore 94 closely receives central portion 66 of housing 64 ; member 50 is screwed onto member 84 by engaging threads 52 and 86 ; the lower portion of thread 72 is smoothly slidable within bore 88 ; and member upper portion 92 cooperates with collar 80 through engagement of threads 82 and 96 . A stop-nut 100 is screwed onto thread 76 .
Referring to FIGS. 6 and 7, when handle 12 is rotated, outer tension tuner member 50 moves through the same angle as does inner tension tuner member 84 . Thread pairs ( 52 , 86 ) and ( 56 , 72 ) are right-handed while thread pair ( 82 , 96 ) is left-handed, so rotating the handle clockwise causes the entire upper wire-end retainer assembly 34 to translate upwards, thereby increasing the tension on wire 32 , while the wire is protected from being twisted by the interaction of housings 64 and 90 . Conversely, rotating the handle counterclockwise causes assembly 34 to translate downwards, decreasing the wire tension. Preferably, the pitch of the thread pairs is such that assembly 34 moves about 1 . 75 mm for one complete rotation of handle 12 .
Referring to FIG. 5, grip lower portion 20 terminates upwardly in a shoulder 102 on which is embossed a vertical index 102 V and upper, middle and lower horizontal indices 102 A, 102 B, 102 C, respectively. Index 102 V allows precise alignment with one of the numerical indicia proximate to edge 12 E so a desired shaft flexibility can be reproduced. As shown in FIGS. 6 and 7, shoulder 102 mates with a shoulder 104 in grip upper portion 14 proximate to edge 12 E. FIG. 6 shows assembly 34 when the handle is rotated fully counterclockwise so the assembly is at its extreme downward position where the shoulders mate. In this position, edge 12 E touches lower index 102 C. FIG. 7 shows the assembly when the handle is rotated fully clockwise so the assembly is at its extreme upward position where the shoulders 102 , 104 are at maximum separation. In this position, edge 12 E touches upper index 102 A. Stop nut 100 prevents the handle from being rotated too far.
Increasing the tension of wire 32 causes the shaft central portion 22 to flex more on the backswing than it otherwise would, storing additional potential energy as the top of the swing is reached. During the downswing this energy is converted into kinetic energy, a process analogous to releasing a bow-string to propel an arrow. This kinetic energy is imparted to the clubhead, resulting in a more powerful impact, compared to using a conventional club, as the clubhead contacts the ball. | A golf club having a hollow shaft whose flexibility is altered by rotating the club handle. Change in flexibility results from change in tension on a wire coinciding with the shaft longitudinal axis. The wire is attached between a longitudinally movable assembly in the handle and a fixed assembly at the shaft lower end. The movable assembly includes outer and inner tension tuner members, a collar, a clamp and bifurcated collet, and outer and inner twist-prevention housings. | 0 |
CROSS REFERENCE TO RELATED APPLICATION
This non-provisional application claims priority from provisional application U.S. Ser. No. 60/355,302 filed Feb. 8, 2002.
FIELD OF THE INVENTION
The present invention relates to novel (oxime)carbamoyl derivatives and pharmaceutical compositions comprising said derivatives which inhibit fatty acid amide hydrolase and are useful for the treatment of conditions which can be effected by inhibiting fatty acid amide hydrolase.
BACKGROUND OF THE INVENTION
Effective treatment of pain with current therapies is limited by adverse effects and a lack of efficacy against all components of pain.
Current research is aimed at understanding the molecular and physiological components of pain processing to develop more effective analgesics (Levine, J. D., New Directions in Pain Research: Meeting Report Molecules to Maladies, Neuron 20: 649-654, 1998; Pasternak, G. W., The Central Questions in Pain Perception May Be Peripheral, PNAS 95:10354-10355, 1998).
The analgesic properties of cannabinoids have been known for many years and to many cultures. Cannabinoids are active in many pre-clinical models of pain, including neuropathic pain. Within the last few years, several endogenous cannabinoids, including the fatty acid amides arachidonylethanolamide (anandamide), and arachidonyl amino acids such as N-arachidonylglycine, homo-γ-linolenyl-ethanolamide and docosatetraenyl-ethanolamide, as well as 2-arachidonyl-glycerol, have been shown to induce analgesia in laboratory animals (DeVane, W. A. et. al., Isolation and Structure of a Brain Constituent That Binds to the Cannabinoid Receptors, Science 258: 1946-1949, 1992; Hanus, L. et. al., Two New Unsaturated Fatty Acid Ethanolamides in Brain that Bind to the Cannabinoid Receptor, J. Med. Chem. 36: 3032-3034, 1993; Machoulam, R. et. al., Identification of an Endogenous 2-Monoglyceride, Present in Canine Gut, That Binds To Cannabinoid Receptors, Biochem. Pharmacol. 50: 83-90, 1995; Vogel, Z. et. al., Cannabinomimetic Behavioral Effects of and Adenylate Cyclase Inhibition By Two New Endogenous Anandamides, Eur. J. Pharmacol. 287: 145-152, 1995; Hargreaves, K. M. et al., Cannabinoids Reduce Hyperalgesia and Inflammation Via Interaction With Peripheral CB1 Receptors, Pain 75: 111-119, 1998; Rice, A. S. C., et. al., The Anti-Hyperalgesic Actions of the Cannabinoid Anandamide and the Putative CB2 Receptor Agonist Palmitoylethanolamide in Visceral and Somatic Inflammatory Pain, Pain 76: 189-199, 1998; Huang, S. M., et al., Identification of a New Class of Molecules, the Arachidonyl Amino Acids, and Characterization of One Member That Inhibits Pain, J. Biological Chemistry, 276: 46, 42639-42644, 2001). The ability of cannabinoid receptor antagonists and cannabinoid receptor antisense to induce hyperalgesia in animals suggests that endogenous cannabinoids regulate the nociceptive threshold (Hargreaves, K. M. et al., Hypoactivity of the Spinal Cannabinoid System Results in NMDA-Dependent Hyperalgesia, J. Neurosci. 18: 451-457, 1998; Piomelli, D. et. al., Control of Pain Initiation By Endogenous Cannabinoids, Nature 394: 277-281, 1998; Fields, H. L. et. al., An Analgesia Circuit Activated By Cannabinoids, Nature 395: 381-383, 1998). Elevation of levels of neuroactive fatty acid amides such as anandamide may provide a unique mechanism to achieve analgesia. The mechanisms by which endogenous cannabinoids are synthesized are not well understood; therefore, targets for drugs aimed at increasing the synthesis of these compounds are slow to be identified.
Anandamide and the other identified endogenous cannabinoids are inactivated through a cleavage mechanism by a membrane-bound enzyme, fatty acid amide hydrolase (FAAH). FAAH, therefore, provides an important target for regulating the activity of endogenous cannabinoids. The inhibition of FAAH may elevate levels of anandamide or other endogenous cannabinoids to increase the nociceptive threshold. Furthermore, the inhibition of FAAH would also extend the therapeutic benefits of other cannabinoid agonists in the treatment of emesis, anxiety, feeding behaviors, movement disorders, glaucoma, neuroprotection and cardiovascular disease.
SUMMARY OF THE INVENTION
The above and other objects and advantages, which will be apparent to one of skill in the art, are achieved in the present invention which is directed to, in a first aspect, a compound of Formula I:
or a pharmaceutically acceptable salt or solvate thereof,
wherein
A is dibenzofuranyl, dibenzothienyl, naphthyl, indolyl, fluorenyl, carbazolyl, or represented by Formula II:
wherein
a is 1 or 2, R is C 1-16 alkoxy optionally substituted with phenyl, pyridyl or morpholinyl; phenyl optionally substituted with C 1-4 alkyl; phenoxy; phenyl-C 1-4 alkyloxy-; pyridyloxy; pyridyl-C 1-4 alkyloxy-; —N(H)—C(O)—C 1-16 alkyl; or —C(O)—N(H)—C 1-16 alkyl; R 1 is a bond or a C 1-3 branched or linear aliphatic hydrocarbon; and B is C 1-4 alkyl, indolyl, benzofuranyl, benzothienyl, dibenzofuranyl, dibenzohienyl, fluorenyl, carbazolyl, naphthyl, quinolinyl or isoquinolinyl, wherein each is optionally substituted with one or more of the same or different substituent selected from the group consisting of C 1-4 branched or linear aliphatic hydrocarbon, C 1-4 alkoxy, halo, haloalkyl, nitro and (C 1-3 alkyl) 0-2 amino-; or represented by Formula III, or Formula IV:
wherein
R 2 is hydrogen, halo or C 1-4 alkyl; R 3 is C 1-4 alkyl, pyridyl, or phenyl optionally substituted with one or more of the same or different substituents selected from the group consisting of halo, C 1-4 haloalkyl and nitro; X is CH or nitrogen; R 4 is C 1-4 branched or linear aliphatic hydrocarbon, C 1-4 alkoxy, halo, haloalkyl, nitro or amino; and b is 0 to 3, provided that if R 2 is halo, then R 3 is not halo; and if R 3 is halo, the R 2 is not halo.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein A is dibenzofuranyl.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein A is indolyl.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein A is represented by Formula II:
wherein
a is 1, R is C 1-4 alkoxy optionally substituted with phenyl, phenoxy, pyridyloxy, or amido optionally substituted with C 1-16 alkyl, R 1 is a bond; and B is represented by Formula III:
wherein
R 2 is hydrogen, and R 3 is methyl, pyridyl, phenyl optionally substituted with one or more halo, haloalkyl or nitro.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein B is represented by Formula III:
wherein
R 2 is hydrogen or methyl; and R 3 is methyl or phenyl optionally substituted with one or more halo, haloalkyl or nitro.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein B is represented by Formula III:
wherein R 2 is hydrogen or methyl; and R 3 is methyl, or phenyl optionally substituted with one or more halo, haloalkyl or nitro.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein B is represented by Formula IV:
wherein X is CH; R 4 is halo; and b is 1.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein B is represented by Formula IV:
wherein X is nitrogen; and b is 0.
According to another embodiment of the first aspect of the present invention are provided compounds of Formula I according to the first embodiment of the first aspect wherein B is represented by Formula V:
wherein X is nitrogen.
According to various embodiments of a second aspect of the present invention are provided compounds of Formula III, Formula IV or Formula V:
wherein
R 2 is hydrogen, or methyl, R 3 is C 1-4 alkyl, pyridyl, or phenyl optionally substituted with one or more halo, haloalkyl or nitro, X is CH or nitrogen, R 4 is C 1-4 branched or linear aliphatic hydrocarbon, C 1-4 alkoxy, halo, haloalkyl or amino, and b is 0 to 3.
According to various embodiments of a second aspect of the present invention are provided compounds of Formula VI:
or a pharmaceutically acceptable salt or solvate thereof,
wherein
a is 1; R is C 1-12 alkoxy; R 2 is hydrogen or methyl; and R 3 is methyl, pyridyl, phenyl optionally substituted with one or more halo, haloalkyl or nitro.
According to another embodiment of the second aspect of the present invention are provided compounds of Formula VI according to the first embodiment of the second aspect wherein R 2 is hydrogen and R 3 is phenyl optionally substituted with one or more halo, haloalkyl or nitro.
According to another embodiment of the second aspect of the present invention are provided compounds of Formula VI according to the first embodiment of the second aspect wherein R 2 is methyl and R 3 is methyl.
According to another embodiment of the second aspect of the present invention are provided compounds of Formula VI according to the first embodiment of the second aspect, a member selected from the group consisting of
pyridine-3-carbaldehyde, O-[[(4-undecyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-decyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-octyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 3,4-difluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 2,6-difluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 2,4-difluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 3-fluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-decyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-decyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-dodecyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-octyloxy-phenyl)amino]carbonyl]oxime; 2,3-difluorobenzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-undecyloxy-phenyl)amino]carbonyl]oxime; 2,4,5-trifluorobenzaldehyde, O-[[(4-nonyloxy phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-undecyloxy-phenyl)amino]carbonyl]oxime; 4-trifluoromethyl-benzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-heptyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[[4-(2-phenylethoxy)phenyl]amino]carbonyl]oxime; 2-fluoro-3-trifluoromethyl-benzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; (4-undecyloxy-phenyl)-carbamic acid phenyl ester; propan-2-one, O-[[(4-heptyloxy-phenyl)amino]carbonyl]oxime; propan-2-one, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[[4-(phenylmethoxy)phenyl]amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[[4-(2-phenylethoxy)phenyl]amino]carbonyl]oxime; 2-fluoro-5-trifluoromethyl-benzaldehyde, O-[[(4-nonyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[[4-(phenylmethoxy)phenyl]amino]carbonyl]oxime; 3-pyridinecarboxaldehyde, O-[[(3-phenoxyphenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[[4-(3-phenylpropoxy)phenyl]amino]carbonyl]oxime; benzaldehyde, O-[[(3-phenoxyphenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-pentyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-butoxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-heptyloxyphenyl)amino]carbonyl]oxime; 3-pyridinecarboxaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime; benzaldehyde, O-[[[4-(3-phenylpropoxy)phenyl]amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-pentyloxy-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-dodecyloxy-phenyl)amino]carbonyl]oxime; propan-2-one, O-[[(4-decyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-dodecyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-pentyloxy-phenyl)amino]carbonyl]oxime; 2,4-difluorobenzaldehyde, benzaldehyde, O-[[(4-nonanoylamino-phenyl)amino]carbonyl]oxime; 4-fluorobenzaldehyde, O-[[(4-heptyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-pentyloxy-phenyl)amino]carbonyl]oxime; propan-2-one, O-[[(4-undecyloxy-phenyl)amino]carbonyl]oxime; propan-2-one, O-[[(4-dodecyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-pentyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-propoxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-heptyloxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-butoxy-phenyl)amino]carbonyl]oxime; benzaldehyde, O-[[(4-hexyloxy-phenyl)amino]carbonyl]oxime; propan-2-one, O-[[(4-heptyloxy-phenyl)amino]carbonyl]oxime; pyridine-3-carbaldehyde, O-[[(4-hexyloxy-phenyl)amino]carbonyl]oxime; and pyridine-3-carbaldehyde, O-[[(4-butoxy-phenyl)amino]carbonyl]oxime.
According to various embodiments of a third aspect of the present invention are provided compounds of Formula VII:
or a pharmaceutically acceptable salt or solvate thereof,
wherein
a is 1; R is C 1-12 alkoxy; R 4 is halo; X is CH or nitrogen; and b is 0 to 2, with the proviso that when X is nitrogen then b is 0.
According to another embodiment of the third aspect of the present invention are provided compounds of Formula VI according to the first embodiment of the third aspect wherein X is CH and is a member selected from the group consisting of:
(4-undecyloxy-phenyl)-carbamic acid phenyl ester; (4-decyloxy-phenyl)-carbamic acid phenyl ester; (4-dodecyloxy-phenyl)-carbamic acid phenyl ester; (4-octyloxy-phenyl)-carbamic acid 2-fluoro-phenyl ester; (4-octyloxy-phenyl)-carbamic acid phenyl ester; (4-heptyloxy-phenyl)-carbamic acid phenyl ester; and (4-decyloxy-phenyl)-carbamic acid 2-fluoro-phenyl ester.
According to various embodiments of a fourth aspect of the present invention are provided compounds of Formula VIII
or a pharmaceutically acceptable salt or solvate thereof,
wherein
a is 1; R is C 1-12 alkoxy; R 1 is a C 1-3 branched or linear aliphatic hydrocarbon; R 4 is phenyl, C 1-3 alkoxy or halo; X is CH or nitrogen; and b is 2.
According to another embodiment of the fourth aspect of the present invention are provided compounds of Formula VIII according to the first embodiment of the fourth aspect wherein X is CH and is a member selected from the group consisting of:
(4-butoxy-benzyl)-carbamic acid 4-fluoro-phenyl ester; pyridine-3-carbaldehyde, O-[[(4-butoxy-benzyl)amino]carbonyl]oxime; (4-butoxy-benzyl)-carbamic acid phenyl ester; [1-(4-butoxy-phenyl)-propyl]-carbamic acid 2-fluoro-phenyl ester; (4-butoxy-benzyl)-carbamic acid 2,4-difluoro-phenyl ester; (4-butoxy-benzyl)-carbamic acid 4-methoxy-phenyl ester; [1-(4-butoxy-phenyl)-propyl]-carbamic acid 4-fluoro-phenyl ester; (4-butoxy-benzyl)-carbamic acid 2-fluoro-phenyl ester; and (4-butoxy-benzyl)-carbamic acid 3-chloro-phenyl ester.
According to various embodiments of a fifth aspect of the present invention are provided compounds of Formula IX:
or a pharmaceutically acceptable salt or solvate thereof,
wherein
a is 1; R is C 1-12 alkoxy; R 1 is a C 1-3 branched or linear aliphatic hydrocarbon; and X is CH or nitrogen.
According to another embodiment of the fifth aspect of the present invention are provided compounds of Formula IX according to the first embodiment of the fifth aspect wherein X is CH and is a member selected from the group consisting of:
(4-butoxy-benzyl)-carbamic acid quinolin-6-yl ester; (4-butoxy-benzyl)-carbamic acid naphthalen-2-yl ester; [1-(4-butoxy-phenyl)-propyl]-carbamic acid quinolin-6-yl ester; and (4-butoxy-benzyl)-carbamic acid naphthalen-1-yl ester.
According to various embodiments of a sixth aspect of the present invention is provided a method of treating a condition or disorder by inhibiting fatty acid amidohydrolase in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I or a compound having the structure
According to various embodiment of a seventh aspect of the present invention is provided a method of treating a condition or disorder by inhibiting fatty acid amidohydrolase in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a eighth aspect of the present invention is provided a method of treating neuropathic pain in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a ninth aspect of the present invention is provided a method of treating acute pain in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a tenth aspect of the present invention is provided a method of treating chronic pain in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of an eleventh aspect of the present invention is provided a method of treating emesis in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a twelfth aspect of the present invention is provided a method of treating anxiety in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a thirteenth aspect of the present invention is provided a method of altering feeding behaviors in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a fourteenth aspect of the present invention is provided a method of treating movement disorders in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a fifteenth aspect of the present invention is provided a method treating glaucoma in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a sixteenth aspect of the present invention is provided a method of treating brain injury in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of a seventeenth aspect of the present invention is provided a method of treating cardiovascular disease in a mammal comprising administering to the mammal a therapeutically effective amount of a compound of Formula I.
According to various embodiments of an eighteenth aspect of the present invention is provided a pharmaceutical composition for treating a condition or disorder requiring inhibition of a fatty acid amidohydrolase comprising a therapeutically effective amount of a compound of Formula I and a pharmaceutically acceptable carrier, adjuvant or diluent.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 illustrates results from a rat carrageen-induced thermal hypergesia model used for measuring chronic inflammatory pain.
FIG. 2 illustrates results from a rat Hargreaves test used for measuring acute thermal pain.
FIG. 3 illustrates results from a rat paw edema model used for measuring inflammation-induced edema.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a novel series of compounds of Formula I, its hydrates and solvates thereof:
or a pharmaceutically acceptable salt or solvate thereof,
wherein
A is dibenzofuranyl, dibenzothienyl, naphthyl, indolyl, fluorenyl, carbazolyl, or represented by Formula II:
wherein
a is 1 or 2, R is C 1-16 alkoxy optionally substituted with phenyl, pyridyl or morpholinyl; phenyl optionally substituted with C 1-4 alkyl; phenoxy; phenyl-C 1-4 alkyloxy-; pyridyloxy; pyridyl-C 1-4 alkyloxy-; —N(H)—C(O)—C 1-16 alkyl; or —C(O)—N(H)—C 1-16 alkyl; R 1 is a bond or a C 1-3 branched or linear aliphatic hydrocarbon; and B is C 1-4 alkyl, indolyl, benzofuranyl, benzothienyl, dibenzofuranyl, dibenzothienyl, fluorenyl, carbazolyl, napthyl, quinolinyl or isoquinolinyl, wherein each is optionally substituted with one or more of the same or different substituent selected from the group consisting of C 1-4 branched or linear aliphatic hydrocarbon, C 1-4 alkoxy, halo, haloalkyl, nitro and (C 1-3 alkyl) 0-2 amino- or represented by Formula III or Formula IV:
wherein
R 2 is hydrogen, methyl, R 3 is C 1-4 alkyl, pyridyl, or phenyl optionally substituted with one or more of the same or different substituents selected from the group consisting of halo, C 1-4 haloalkyl and nitro, X is CH or nitrogen, R 4 is C 1-4 branched or linear aliphatic hydrocarbon, C 1-4 alkoxy, halo, haloalkyl, nitro or amino, and b is 0 to 3.
Preferably, A is represented by Formula II:
wherein a is 1, R is C 1-12 alkoxy; phenoxy; pyridyloxy; or amido optionally substituted with C 1-16 alkyl; and R 1 is a bond.
When B is represented by Formula III:
R 2 is preferably hydrogen or methyl, and R 3 is preferably methyl, or phenyl optionally substituted with one or more halo, haloalkyl or nitro.
When B is represented by Formula IV:
X is preferably CH, R 4 is preferably halo, and b is 1. When X is nitrogen, however, b is preferably 0.
When B is represented by Formula V:
X is preferably nitrogen.
The description of the invention herein should be construed in congruity with the laws and principals of chemical bonding. For example, when a moiety is optionally substituted and said substitution requires the removal of a hydrogen atom from the moiety to be substituted, the description of the moiety should be read to include the moiety with or without said hydrogen atom. As another example, if a variable is defined as a particular moiety or atom and is further defined to have value of 0 or some integer, the bond(s) attaching said moiety should be suitably removed in the event the variable equals 0.
An embodiment or aspect which depends from another embodiment or aspect, will describe only the variables having values and provisos that differ from the embodiment or aspect from which it depends. For example, if a dependnent embodiment describes a variable as being “phenyl or pyridyl”, wherein said phenyl and pyridyl were described in the independent embodiment as being “optionally substituted”, then the phenyl and pyridyl of the dependent embodiment will also be optionally substituted.
It is to be understood that the present invention may include any and all possible stereoisomers, geometric isomers, diastereoisomers, enantiomers, anomers and optical isomers, unless a particular description specifies otherwise. More particularly, the groups attached to the oxime portion of compounds of Formula (I), i.e., N═C, may assume transoid or cisoid configurations.
As used herein, “halo” or “halogen” includes fluoro, chloro, bromo and iodo.
As used herein, “alkyl” or “alkylene” includes straight or branched chain configurations.
The compounds of this invention can exist in the form of pharmaceutically acceptable salts. Such salts include addition salts with inorganic acids such as, for example, hydrochloric acid and sulfuric acid, and with organic acids such as, for example, acetic acid, citric acid, methanesulfonic acid, toluenesulfonic acid, tartaric acid and maleic acid. Further, in case the compounds of this invention contain an acidic group, the acidic group can exist in the form of alkali metal salts such as, for example, a potassium salt and a sodium salt; alkaline earth metal salts such as, for example, a magnesium salt and a calcium salt; and salts with organic bases such as a triethylammonium salt and an arginine salt. The compounds of the present invention may be hydrated or non-hydrated.
The compounds of this invention can be administered in such oral dosage forms as tablets, capsules (each of which includes sustained release or timed release formulations), pills, powders, granules, elixirs, tinctures, suspensions, syrups and emulsions. The compounds of this invention may also be administered intravenously, intraperitoneally, subcutaneously, or intramuscularly, all using dosage forms well known to those skilled in the pharmaceutical arts. The compounds can be administered alone, but generally will be administered with a pharmaceutical carrier selected upon the basis of the chosen route of administration and standard pharmaceutical practice. Compounds of this invention can also be administered in intranasal form by topical use of suitable intranasal vehicles, or by transdermal routes, using transdermal skin patches. When compounds of this invention are administered transdermally the dosage will be continuous throughout the dosage regimen.
The dosage and dosage regimen and scheduling of a compounds of the present invention must in each case be carefully adjusted, utilizing sound professional judgment and considering the age, weight and condition of the recipient, the route of administration and the nature and extent of the disease condition. In accordance with good clinical practice, it is preferred to administer the instant compounds at a concentration level that will produce effective beneficial effects without causing any harmful or untoward side effects.
Compounds of the present invention may be synthesized according to the description provided below. Variables provided in the schema below are defined in accordance with the description of compounds of Formula (I) unless otherwise specified.
Experimentals
The following Intermediates 1 to 39 may be used to synthesize Examples 1 to 124 in accordance with Schemes 1, 1A and 1B.
4-Propoxy-benzoic acid ethyl ester: (Scheme 1, Compound A) To a solution of ethyl 4-hydroxybenzoate (2.0 g, 12 mmol) and bromopropane (4.0 g, 32.8 mmol) in DMF (50 mL) was added NaH (60% in mineral oil, 0.80 g, 20.8 mmol). The resultant suspension was stirred at room temperature for 1.0 hour. The mixture was diluted with ethyl acetate (EtOAc) (300 mL), washed with H 2 O, and then was dried over Na 2 SO 4 . After filtration and concentration in vacuo, the residue was purified by flash chromatography (SiO 2 : EtOAc/Hexanes). This compound was obtained as a yellow oil (2.26 g, 10.9 mmol, 91% yield). 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.24 (q, 2H, J=6.9 Hz), 3.98 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (t, 3H, J=6.6 Hz), 0.97 (t, 3H, J=7.2 Hz); Anal. Calcd for C 12 H 16 O 3 .0.47C 6 H 14 : C, 71.54; H, 9.14; N, 0.00. Found: C, 71.57; H, 8.78; N, 0.00; Mass Spec.: 209.04 (MH+).
4-Ethoxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=9.0 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.24 (q, 2H, J=6.9 Hz), 4.08 (q, 2H, J=6.9 Hz), 1.31 (m, 6H); Anal. Calcd for C 11 H 14 O 3 .0.47C 6 H 14 : C, 70.71; H, 8.83; N, 0.00; Found: C, 71.10; H, 8.43; N, 0.00; Mass Spec.: 194.93 (MH+).
4-Pentyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.24 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 7H, J=6.6 Hz), 0.97 (t, 3H, J=7.2 Hz); Anal. Calcd for C 14 H 20 O 3 .0.37C 6 H 14 : C, 72.63; H, 9.46; N, 0.00; Found: C, 72.69; H, 9.12; N, 0.00; Mass Spec.: 237.11 (MH+).
4-Butoxy-3-methoxy-benzoic acid methyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.57 (dd, 1H, J=8.4, 1.8 Hz), 7.43 (d, 1H, J=1.8 Hz), 7.06 (d, 1H, J=8.4 Hz), 4.02 (q, 2H, J=6.6 Hz), 3.82 (s, 3H), 3.80 (s, 3H), 1.72 (m, 2H), 1.44 (m, 2H), 0.92 (t, 3H, J=7.5 Hz); Mass Spec.: 239.21 (MH+).
4-Hexyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO- d6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 9H), 0.89 (t, 3H, J=7.2 Hz); Mass Spec.: 251 (MH+).
4-Heptyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 11H), 0.85 (t, 3H, J=7.2 Hz); Mass Spec.: 265 (MH+).
4-Octyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 13H), 0.84 (t, 3H, J=7.2 Hz); Mass Spec.: 279.36 (MH+).
4-Nonyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 15H), 0.84 (t, 3H, J=7.2 Hz); Mass Spec.: 293.32 (MH+).
4-Decyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 17H), 0.83 (t, 3H, J=7.2 Hz); Mass Spec.: 307.27 (MH+).
4-Undecyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 19H), 0.83 (t, 3H, J=7.2 Hz); Mass Spec.: 321.28 (MH+).
4-Dodecyloxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 21H), 0.83 (t, 3H, J=6.6 Hz); Mass Spec.: 335.29 (MH+).
4-(3-Morpholin-4-yl-propoxy)-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.26 (q, 2H, J=6.9 Hz), 4.08 (t, 2H, J=6.6 Hz), 3.56 (t, 4H, J=4.5 Hz), 2.36 (m, 6H), 1.72 (m, 2H), 1.32 (m, 2H), 1.29 (t, 3H, J=6.9 Hz); Mass Spec.: 294.32 (MH+).
(4-Butoxy-phenyl)-acetic acid methyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.16 (dd, 2H, J=6.6, 1.8 Hz), 6.85 (dd, 2H, J=6.6, 1.8 Hz), 3.93 (t, 2H, J=6.3 Hz), 3.59 and 3.58 (5H, CH 2 , CH 3 ), 1.67 (m, 2H), 1.40 (m, 2H), 0.92 (t, 3H, J=7.2 Hz).
3-Butoxy-benzoic acid ethyl ester: (Scheme 1, Compound A) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.53 (dd, 1H, J=7.8, 1.5 Hz), 7.42 (m, 2H), 7.20 (dd, 1H, J=8.4, 1.5 Hz), 4.31 (q, 2H, J=6.9 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.47 (m, 2H), 1.32 (t, 3H, J=6.9 Hz), 0.93 (t, 3H, J=7.5 Hz); Mass Spec.: 223.24 (MH+).
4-Butoxy-benzoic acid: (Scheme 1, Compound B) To a solution of ethyl 4-butoxybenzoate (2.0 g, 9.6 mmol) in EtOH (30 mL) was added NaOH (10 N, 6 mL, 60 mmol). The resulting mixture was stirred at room temperature for 3 hours, diluted with H 2 O (30 mL), acidified to about pH 1.0 using HCl (6N). The precipitates were filtered off by filter paper, washed by H 2 O and hexanes. This compound was obtained as a white solid. (1.63 g, 9.1 mmol, 94% yield). 1 H NMR (DMSO-d 6 ) δ 12.59 (br. s, 1H), 7.88 (d, 2H, J=9.5 Hz), 6.97 (d, 2H, J=9.5 Hz), 4.01 (t, 2H, J=6.5 Hz), 1.68 (m, 2H), 1.42 (m, 2H), 0.91 (t, 3H, J=6.5 Hz); 13 C NMR (DMSO): 166.9, 162.2, 131.2, 122.7, 114.0, 67.3, 30.5, 18.6 and 13.5; Mass Spec.: 195.17 (MH+).
4-Pentyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.59 (br, s, 1H), 7.88 (d, 2H, J=9.6 Hz), 6.97 (d, 2H, J=9.6 Hz), 4.01 (t, 2H, J=6.9 Hz), 1.69 (m, 2H), 1.32 (m, 4H), 0.89 (t, 3H, J=6.9 Hz); Mass Spec.: 209.23 (MH+).
4-Propoxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.6 (br, s, 1H), 7.88 (d, 2H, J=9.6 Hz), 6.97 (d, 2H, J=9.6 Hz), 4.01 (t, 2H, J=6.9 Hz), 1.72 (m, 2H), 0.97 (t, 3H, J=7.5 Hz); Mass Spec.: 181.18 (MH+).
4-Ethoxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.59 (br. s, 1H), 7.88 (d, 2H, J=9.6 Hz), 6.97 (d, 2H, J=9.6 Hz), 4.08 (q, 2H, J=7.2 Hz), 1.33 (t, 3H, J=6.9 Hz); Mass Spec.: 167.13 (MH+).
4-Butoxy-3-methoxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.6 (br, s, 1H), 7.54 (dd, 1H, J=8.4, 1.8 Hz), 7.43 (d, 1H, J=1.8 Hz), 7.06 (d, 1H, J=8.4 Hz), 4.02 (q, 2H, J=6.6 Hz), 3.80 (s, 3H), 1.72 (m, 2H), 1.44 (m, 2H), 0.92 (t, 3H, J=7.5 Hz).
4-Hexyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.59 (s, 1H), 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 6H), 0.89 (t, 3H, J=7.2 Hz); Mass Spec.: 223 (MH+).
4-Heptyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.59 (s, 1H), 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 8H), 0.85 (t, 3H, J=7.2 Hz); Mass Spec.: 237.16 (MH+).
4-Octyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 10H), 0.84 (t, 3H, J=7.2 Hz); Mass Spec.: 251.11 (MH+).
4-Nonyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.58 (s, 1H), 7.89 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 12H), 0.84 (t, 3H, J=7.2 Hz).
4-Dodecyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.6 (s, 1H), 7.86 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 18H), 0.84 (t, 3H, J=6.6 Hz).
4-Undecyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.6 (s, 1H), 7.86 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 16H), 0.84 (t, 3H, J=6.6 Hz).
4-Decyloxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.6 (s, 1H), 7.86 (d, 2H, J=8.7 Hz), 7.00 (d, 2H, J=9.0 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.29 (m, 14H), 0.84 (t, 3H, J=6.6 Hz).
4-(3-Morpholin-4-yl-propoxy)-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.78 (d, 2H, J=8.4 Hz), 6.79 (d, 2H, J=8.4 Hz), 4.08 (t, 2H, J=6.6 Hz), 3.56 (t, 4H, J=4.5 Hz), 2.36 (m, 6H), 1.85 (m, 2H).
(4-Butoxy-phenyl)-acetic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 12.21 (br. s, 1H), 7.16 (dd, 2H, J=6.6, 1.8 Hz), 6.85 (dd, 2H, J=6.6, 1.8 Hz), 3.93 (t, 2H, J=6.3 Hz), 3.46 (s, 2H), 1.69 (m, 2H), 1.43 (m, 2H), 0.92 (t, 3H, J=7.2 Hz).
3-Butoxy-benzoic acid: (Scheme 1, Compound B) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.53 (dd, 1H, J=7.8, 1.5 Hz), 7.42 (m, 2H), 7.17 (dd, 1H, J=8.4, 1.5 Hz), 4.01 (t, 2H, J=6.6 Hz), 1.72 (m, 2H), 1.47 (m, 2H), 0.93 (t, 3H, J=7.2 Hz).
2,4-Difluoro-benzaldehyde oxime: (Scheme 1, Compound C) To a mixture of 2,4-difluorobenzaldehyde (0.80 g, 5.6 mmol) and hydroxyamine HCl salt (0.43 g, 6.2 mmol) in EtOH (5 mL) was added K 2 CO 3 (0.85 g, 6.2 mmol). The resultant mixture was stirred at rt for 24 hours. The mixture was diluted with MeOH (20 mL). The precipitates were filter off and washed with MeOH. The product from filtrate was purified by recrystalization (EtOAc/Hexanes). This compound was obtained as a white solid (0.84 g, 5.3 mmol, 94% yield). 1 H NMR (DMSO-d 6 ) δ 12.98 (br. s, 1H), 8.17 (s, 1H), 7.79 (m, 1H), 7.32 (m, 1H), 7.11 (m, 1H); Analytical HPLC 1.03 min. (95%); Mass Spec.: 158.06 (MH+).
2-Fluoro-6-trifluoromethyl-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 11.96 (br. s, 1H), 8.21 (m, 1H), 7.65 (m, 3H); Analytical HPLC 1.20 min. (96%); Mass Spec.: 208.14 (MH+).
3,4-Difluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 1.00 min. (92%); Mass Spec.: 158 (MH+).
3-Fluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 0.90 min. (95%); Mass Spec.: 138 (MH−).
4-Trifluoromethyl-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 1.31 min. (95%); Mass Spec.: 188.01 (MH+).
2-Fluoro-3-trifluoromethyl-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 1.41 min. (90%); Mass Spec.: 206.00 (MH−).
2,3,5,6-Tetrafluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 0.83 min. (96%); Mass Spec.: 191.98 (MH−).
2,6-Difluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 0.86 min. (95%); Mass Spec.: 158.05 (MH+).
2,3-Difluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 0.83 min. (90%); Mass Spec.: 156.04 (MH−).
2,4,5-Trifluoro-benzaldehyde oxime: (Scheme 1, Compound C) Prepared as described for the example above. Analytical HPLC 0.89 min. (91%); Mass Spec.: 174.00 (MH−).
EXAMPLE 1
3-Pyridinecarboxaldehyde, O-[[[4-(Heptyloxy)phenyl]amino]carbonyl]oxime (Scheme 1, Compound D) To a solution of 4-heptyloxybenzoic acid (0.20 g, 0.85 mmol) and Et 3 N (0.18 g, 1.8 mmol) in toluene (5 mL) was added diphenylphosphoryl azide (0.322 g, 1.2 mmol). The resultant mixture was stirred at r.t. for 10 min. and then at 105° C. under N 2 for 60 min. After the mixture was cooled to r.t., 3-pyridinealdoxime (0.20 g, 1.7 mmol) was added. The reaction mixture was stirred at r.t. for 10 min. and then at 80° C. for 1 h. The product (free base) was purified by flash chromatography (SiO 2 : EtOAc/Hexanes) and then was dissolved in a solution of TFA in THF (5.0 mg/mL, 17.8 mL, 0.78 mmol). Removal of solvent provided this compound (TFA salt) as a pale yellow solid (0.244 g, 0.52 mmol, 61% yield). 1 H NMR (DMSO-d 6 ) δ 9.72 (s, 1H), 8.99 (s, 1H), 8.72 (m, 2H), 8.32 (d, 1H, J=9.0 Hz), 7.56 (m, 1H), 7.40 (d, 2H, J=8.5 Hz), 6.91 (d, 2H, J=6.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.32 (m, 8H), 0.87 (t, 3H, J=7.0 Hz); Anal. Calcd for C 20 H 25 N 3 O 3 .0.98C 2 F 3 O 2 H 1 : C, 56.44; H, 5.60; N, 8.99. Found: C, 56.41; H, 5.64; N, 8.94. Mass Spec: 356.28 (MH + ).
EXAMPLE 2
(4-Butoxyphenyl)methylcarbamic acid, 3-pyridinyl ester (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 8.51 (m, 3H), 7.75 (m, 1H), 7.55 (m, 1H), 7.24 (d, 2H, J=9.0 Hz), 6.91 (d, 2H, J=8.7 Hz), 4.22 (d, 2H, J=6.0), 3.92 (t, 2H, J=6.6 Hz), 1.70 (m, 2H), 1.36 (m, 2H), 0.92 (t, 3H, J=7.5 Hz); Anal. Calcd for C 17 H 20 N 2 O 3 .1.55C 2 F 3 O 2 H 1 : C, 50.64; H, 4.56; N, 5.88. Found: C, 50.49; H, 4.58; N, 5.73. Mass Spec: 301.17 (MH + ).
EXAMPLE 3
3-Pyridinecarboxaldehyde, O-[[[4-(undecyloxy)phenyl]amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.72 (s, 1H), 8.99 (s, 1H), 8.72 (m, 2H), 8.32 (d, 1H, J=9.0 Hz), 7.56 (m, 1H), 7.40 (d, 2H, J=8.5 Hz), 6.91 (d, 2H, J=6.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.32 (m, 16H), 0.87 (t, 3H, J=7.0 Hz). Mass Spec: 412.33 (MH + ).
EXAMPLE 4
3-Pyridinecarboxaldehyde, O-[[[4-(nonyloxy)phenyl]amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.72 (s, 1H), 8.99 (s, 1H), 8.72 (m, 2H), 8.32 (d, 1H, J=9.0 Hz), 7.56 (m, 1H), 7.40 (d, 2H, J=8.5 Hz), 6.91 (d, 2H, J=6.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.32 (m, 12H), 0.87 (t, 3H, J=7.0 Hz). Mass Spec: 384.89 (MH + ).
EXAMPLE 5
4-Fluorobenzaldehyde, O-[[(4-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above in a form of free base. No trifluoroacetic acid was used. 1 H NMR (DMSO-d 6 ) δ 9.66 (s, 1H), 8.64 (s, 1H), 7.90 (m, 2H), 7.38 (m, 2H), 7.34 (t, 2H, J=6.0 Hz), 6.92 (d, 2H, J=4.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.40 (m, 2H), 0.92 (t, 3H, J=7.5 Hz); Anal. Calcd for C 18 H 19 FN 2 O 3 : C, 65.44; H, 5.79; N, 8.48. Found: C, 65.48; H, 5.88; N, 8.46. Mass Spec: 331.14 (MH + ).
EXAMPLE 6
2-Propanone, O-[[(4-ethoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. This compound was purified by preparative HPLC (YMC 30×100 mm (5 uM packing), 10% MeOH/90% water/01% TFA as mobile phase A, 90% MeOH/10%water/0.1% TFA as mobile phase B). Analytical HPLC 1.10 min. (95%). Mass Spec: 237 (MH+).
EXAMPLE 7
2-Propanone, O-[[(4-propoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.36 (s, 1H), 7.34 (d, 2H, J=9.0 Hz), 6.85 (dd, 2H, J=6.9, 2.1 Hz), 3.87 (t, 2H, J=6.9 Hz), 1.97 (s, 6H), 1.72 (m, 2H), 0.96 (t, 3H, J=7.5 Hz); Analytical HPLC 1.27 min. (95%). Mass Spec: 251.24 (MH+).
EXAMPLE 8
2-Propanone, O-[[(4-pentyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.67 min. (95%). Mass Spec: 279.18 (MH+).
EXAMPLE 9
Benzaldehyde, O-[[(4-ethoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.41 min. (85%). Mass Spec: 285.21 (MH+).
EXAMPLE 10
Benzaldehyde, O-[[(4-propoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.64 min. (85%). Mass Spec: 299.15 (MH+).
EXAMPLE 11
Benzaldehyde, O-[[(4-pentyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.85 min. (95%). Mass Spec: 327.20 (MH+).
EXAMPLE 12
4-Fluorobenzaldehyde, O-[[(4-ethoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.66 (s, 1H), 8.64 (s, 1H), 7.90 (m, 2H), 7.38 (m, 4H), 6.90 (d, 2H, J=4.5 Hz), 3.92 (q, 2H, J=6.5 Hz), 1.31 (t, 3H, J=7.2 Hz). Analytical HPLC 1.46 min. (95%). Mass Spec: 303 (MH+).
EXAMPLE 13
4-Fluorobenzaldehyde, O-[[(4-propoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.67 min. (94%). Mass Spec: 317 (MH+).
EXAMPLE 14
4-Fluorobenzaldehyde, O-[[(4-pentyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.76 min. (97%). Mass Spec: 345.24 (MH+).
EXAMPLE 15
3-Pyridinecarboxaldehyde, O-[[(4-ethoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 0.99 min. (95%). Mass Spec: 286.24 (MH+).
EXAMPLE 16
3-Pyridinecarboxaldehyde, O-[[(4-propoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.28 min. (95%). Mass Spec: 300.15 (MH+).
EXAMPLE 17
3-Pyridinecarboxaldehyde, O-[[(4-pentyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.50 min. (95%). Mass Spec: 328.27 (MH+).
EXAMPLE 18
2-Propanone, O-[[(4-butoxy-3-methoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.35 min. (98%). Mass Spec: 295.27 (MH+).
EXAMPLE 19
Benzaldehyde, O-[[(4-butoxy-3-methoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.59 min. (99%). Mass Spec: 343 (MH+).
EXAMPLE 20
4-Fluorobenzaldehyde, O-[[(4-butoxy-3-methoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.61 min. (95%). Mass Spec: 361.24 (MH+).
EXAMPLE 21
3-Pyridinecarboxaldehyde, O-[[(4-butoxy-3-methoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.27 min. (99%). Mass Spec: 344.30 (MH+).
EXAMPLE 22
2-Propanone, O-[[(4-hexyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.70 min. (94%). Mass Spec: 293 (MH+).
EXAMPLE 23
Benzaldehyde, O-[[(4-hexyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.84 min. (99%). Mass Spec: 341.26 (MH+).
EXAMPLE 24
4-Fluorobenzaldehyde, O-[[(4-hexyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.86 min. (99%). Mass Spec: 359.22 (MH+).
EXAMPLE 25
3-Pyridinecarboxaldehyde, O-[[(4-hexyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.64 min. (90%). Mass Spec: 342.30 (MH+).
EXAMPLE 26
2-Propanone, O-[[(4-heptyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.98 min. (91%). Mass Spec: 307.19 (MH+).
EXAMPLE 27
Benzaldehyde, O-[[(4-heptyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.11 min. (93%). Mass Spec: 355.18 (MH+).
EXAMPLE 28
4-Fluorobenzaldehyde, O-[[(4-heptyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.10 min. (90%). Mass Spec: 373.11 (MH+).
EXAMPLE 29
2-Propanone, O-[[(4-octyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.89 min. (87%). Mass Spec: 321 (MH+).
EXAMPLE 30
3-Pyridinecarboxaldehyde, O-[[(4-octyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.0 min. (85%). Mass Spec: 370.13 (MH+).
EXAMPLE 31
2-Propanone, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.64 min. (97%). Mass Spec: 335.31 (MH+).
EXAMPLE 32
2-Propanone, O-[[(4-decyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.03 min. (99%). Mass Spec: 349.35 (MH+).
EXAMPLE 33
Benzaldehyde, O-[[(4-decyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.10 min. (99%). Mass Spec: 397.38 (MH+).
EXAMPLE 34
4-Fluorobenzaldehyde, O-[[(4-decyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.11 min. (97%). Mass Spec: 415.34 (MH+).
EXAMPLE 35
3-Pyridinecarboxaldehyde, O-[[(4-decyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.01 min. (85%). Mass Spec: 398.34 (MH+).
EXAMPLE 36
2-Propanone, O-[[(4-undecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.25 min. (90%). Mass Spec: 363.26 (MH+).
EXAMPLE 37
Benzaldehyde, O-[[(4-undecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.36 min. (96%). Mass Spec: 411.28 (MH+).
EXAMPLE 38
4-Fluorobenzaldehyde, O-[[(4-undecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.37 min. (97%). Mass Spec: 429.30 (MH+).
EXAMPLE 39
Benzaldehyde, O-[[(4-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.66 (s, 1H), 8.62 (s, 1H), 7.82 (m, 2H), 7.52 (m, 3H), 7.40 (d, 2H, J=8.5 Hz), 6.90 (d, 2H, J=9.0 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.40 (m, 2H), 0.92 (t, 3H, J=7.5 Hz); Analytical HPLC 1.67 min. (90%). Mass Spec: 313.15 (MH+).
EXAMPLE 40
2-Propanone, O-[[(4-dodecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.15 min. (99%). Mass Spec: 377.43 (MH+).
EXAMPLE 41
Benzaldehyde, O-[[(4-dodecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.20 min. (99%). Mass Spec: 425.41 (MH+).
EXAMPLE 42
4-Fluorobenzaldehyde, O-[[(4-dodecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.21 min. (99%). Mass Spec: 443.37 (MH+).
EXAMPLE 43
3-Pyridinecarboxaldehyde, O-[[(4-dodecyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.27 min. (85%). Mass Spec: 426.32 (MH+).
EXAMPLE 44
3-Pyridinecarboxaldehyde, O-[[(4-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.48 min. (95%). Mass Spec: 314.20 (MH+).
EXAMPLE 45
Benzaldehyde, O-[[(4-octyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.99 min. (99%). Mass Spec: 369.27 (MH+).
EXAMPLE 46
4-Fluorobenzaldehyde, O-[[(4-octyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.99 min. (96%). Mass Spec: 387.39 (MH+).
EXAMPLE 47
Benzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.04 min. (95%). Mass Spec: 383.30 (MH+).
EXAMPLE 48
4-Fluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.0 min. (95%). Mass Spec: 401.30 (MH+).
EXAMPLE 49
3,4-Difluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.66 (s, 1H), 8.62 (s, 1H), 7.90 (m, 1H), 7.65 (m, 2H), 7.40 (d, 2H, J=8.7 Hz), 6.90 (d, 2H, J=9.0 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.25 (m, 12H), 0.85 (t, 3H, J=7.5 Hz). Analytical HPLC 2.03 min. (95%). Mass Spec: 419.20 (MH+).
EXAMPLE 50
2,6-Difluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.05 min. (85%). Mass Spec: 419 (MH+).
EXAMPLE 51
2,4-Difluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.07 min. (99%). Mass Spec: 419.31 (MH+).
EXAMPLE 52
3-Fluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.05 min. (95%). Mass Spec: 401.33 (MH+).
EXAMPLE 53
4-(Trifluoromethyl)benzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.64 min. (99%). Mass Spec: 451.25 (MH+).
EXAMPLE 54
2-Fluoro-3-(trifluoromethyl)benzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.11 min. (85%). Mass Spec: 469.07 (MH+).
EXAMPLE 55
2,3-Difluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.08 min. (90%). Mass Spec: 419.17 (MH+).
EXAMPLE 56
2,4,5-Trifluorobenzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.01 min. (95%). Mass Spec: 437 (MH+).
EXAMPLE 57
2-Fluoro-5-(trifluoromethyl)benzaldehyde, O-[[(4-nonyloxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.11 min. (95%). Mass Spec: 469.13 (MH+).
EXAMPLE 58
4-Fluorobenzaldehyde, O-[[4-[3-(4-morpholinyl)propoxyphenyl]amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 2.68 min. (85%). Mass Spec: 402.30 (MH+).
EXAMPLE 59
4-Nitrobenzaldehyde, O-[[(4-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.83 min. (85%). Mass Spec: 358.17 (MH+).
EXAMPLE 60
2-Propanone, O-[[(4-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.39 (br. s, 1H), 7.36 (d, 2H, J=8.1 Hz), 6.90 (dd, 2H, J=7.0, 2.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.97 (s, 6H), 1.67 (m, 2H), 1.42 (m, 2H), 0.91 (t, 3H, J=7.0 Hz). Analytical HPLC 1.59 min. (95%). Mass Spec: 265.16 (MH+).
EXAMPLE 61
2-Propanone, O-[[(4-butoxyphenylmethyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.44 min. (95%). Mass Spec: 279.32 (MH+).
EXAMPLE 62
Benzaldehyde, O-[[(4-butoxyphenylmethyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.66 min. (95%). Mass Spec: 327.31 (MH+).
EXAMPLE 63
4-Fluorobenzaldehyde, O-[[(4-butoxyphenylmethyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.66 min. (85%). Mass Spec: 345.28 (MH+).
EXAMPLE 64
3-Pyridinecarboxaldehyde, O-[[(4-butoxyphenylmethyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.55 min. (95%). Mass Spec: 328.29 (MH+).
EXAMPLE 65
3-Pyridinecarboxaldehyde, O-[[(3-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.39 min. (95%). Mass Spec: 314.28 (MH+).
EXAMPLE 66
2-Propanone, O-[[(3-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.47 min. (97%). Mass Spec: 265.32 (MH+).
EXAMPLE 67
Benzaldehyde, O-[[(3-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.69 min. (92%). Mass Spec: 313.27 (MH+).
EXAMPLE 68
4-Fluorobenzaldehyde, O-[[(3-butoxyphenyl)amino]carbonyl]oxime (Scheme 1, Compound D) Prepared as described for the example above. Analytical HPLC 1.71 min. (92%). Mass Spec: 331.30 (MH+).
EXAMPLE 69
3-Pyridinecarboxaldehyde, O-[[([1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method A: filtration of the reaction mixture, and the solid was recrystallized from EtOAc/hexanes, provided the title compound as light yellow solid in 38% yield. 1 H NMR (DMSO, 400 MHz) δ 10.06 (s, 1H), 8.96 (d, J=2.0 Hz, 1H), 8.74 (s, 1H), 8.72 (dd, J=1.6 Hz, J=4.8 Hz, 1H), 8.25 (dt, J=1.8 Hz, J=6.2 Hz 1H), 7.68-7.63 (m, 6H), 7.67-7.64 (dd, J=4.8 Hz, J=8.4 Hz, 1H), 7.45 (t, J=7.2 Hz, 2H), 7.34 (t, J=7.2 Hz, 1H); 13C NMR (DMSO, 400 MHz) δ 152.7, 152.0, 151.5, 149.3, 139.5, 137.5, 135.0, 134.6, 128.8, 127.0, 126.5, 126.2, 124.0, 119.5; Mass spec.: 318.0 (MH+); Anal. Calcd. for C 19 H 14 N 3 O 2 : C=72.14%, H=4.46%, N=13.28%; found: C=72.09%, H=4.68%, N=13.14%.
EXAMPLE 70
3-Pyridinecarboxaldehyde, O-[[(4′-ethyl-[1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. 1 H NMR (DMSO, 400 MHz) δ 10.03 (s, 1H), 8.97 (d, J=1.7 Hz, 1H), 8.74 (s, 1H), 8.72 (dd, J=1.7 Hz, J=4.8 Hz, 1H), 8.25 (dt, J=1.6 Hz, J=8.0 Hz 1H), 7.63 (m, 4H), 7.57-7.54 (m, 3H), 7.28 (d, J=8.3 Hz, 2H), 2.63 (q, J=7.2 Hz, 2H), 1.20 (t, J=7.6 Hz, 3H); 13 C NMR (DMSO, 400 MHz) δ 152.6, 151.9, 151.5, 149.3, 142.6, 137.2, 136.9, 135.0, 134.6, 128.2, 126.7, 126.5, 126.1, 124.0, 119.5, 27.7, 15.5; Mass spec.: 346.1 (MH + ); Anal. Calcd. for C 21 H 18 N 3 O 2 : C=73.24%, H=5.26%, N=12.20; found: C=73.10%, H=5.46%, H=12.25%.
EXAMPLE 71
3-Pyridinecarboxaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method A provided the title compound as white need like crystal in 24% yield. 1 H NMR (DMSO, 400 MHz) δ 9.94, (s, 1H), 8.96 (d, J=1.7 Hz, 1H), 8.72 (s, 1H), 8.71 (dd, J=1.8 Hz, J=4.9 Hz, 1H), 8.25 (dt, J=1.9 Hz, J=8.0 Hz, 1H), 7.56-7.53 (m 3H), 7.37 (t, J=7.4 Hz, 2H), 7.11 (t, J=8.4 Hz, 1H), 7.03 (d, J=6.8 Hz, 2H), 6.98 (d, 8.2 Hz, 2H); 13 C NMR (DMSO, 400 MHz) δ 157.2, 152.5, 151.9, 151.7, 149.3, 134.6, 133.8, 129.9, 126.5, 124.0, 122.9, 121.1, 119.5, 117.8; Mass spec.: 334.0 (MH + ); Anal. Calcd. for C 19 H 14 N 3 O 3 : C=68.66%, H=4.24%, N=12.64%; found: C=68.50%, H=4.49%, N=12.57%.
EXAMPLE 72
Benzaldehyde, O-[[([1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method B: after removal of the solvent, the residue was chromatographed by silica gel column packed with EtOAc/hexanes or EtOAc/dichloromethane, to provide the title compound as white solid in 25% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 8.44 (s, 1H), 8.18 (br, 1H), 7.75-7.73 (m 2H), 7.61-7.58 (m, 6H), 7.54-7.42 (m, 5H), 7.34 (tt, J=1.2 Hz, J=7.4 Hz, 1H). Anal. Calcd. for C 20 H 15 N 2 O 2 .0.198H 2 O: C=75.32%, H=4.87%, N=8.78%; found: C=75.33%, H=5.16%, N=8.66%.
EXAMPLE 73
Benzaldehyde, O-[[([1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method B provided the title compound as white solid in 14% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 8.40 (s, 1H), 8.09 (br, 1H), 7.77-7.73 (m 2H), 7.60-7.58 (m, 6H), 7.44 (t, J=7.3 Hz, 2H), 7.34 (tt, J=1.2 Hz, J=7.4 Hz, 1H), 7.18 (t, J=8.56 Hz, 2H); 166.6, 164.0, 1.52.7, 151.7, 140.4, 137.4, 136.1, 130.4, 130.3, 128.8, 127.8, 127.2, 126.9, 126.0, 120.0, 116.6, 116.4.
EXAMPLE 74
Benzaldehyde, O-[[(4′-ethyl-[1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C: after removal of solvent, the residue was dissolved in methanol and filtrated, the filtrate was purified by preparative HPLC with methanol:H 2 O (30:70 to about 100:0 v/v, containing 1% TFA) as a mobile phase to provide the title compound as white solid in 11% yield. 1 H NMR (DMSO, 500 MHz) δ 9.99 (s, 1H), 8.66 (s, 1H), 7.84 (d, J=8.1 Hz, 2H), 7.66-7.60 (m, 4H), 7.57-7.50 (m, 5H), 7.28 (d, J=88.11 Hz, 2H), 2.63 (q, J=7.5 Hz, 2H), 1.21 (m, 3H); 13 C NMR (DMSO, 500 MHz) δ 154.8, 151.7, 142.5, 137.4, 136.9, 131.4, 130.3, 128.9, 128.2, 128.0, 126.7, 126.1, 119.4, 27.7, 15.5; Mass spec.: 345.1 (MH + ); Anal. Calcd. for C 22 H 20 N 2 O 2 : C=76.72%, H=5.85%, N=8.13%; found: C=76.67%, H=5.91%, N=8.02%.
EXAMPLE 75
4-Fluorobenzaldehyde, O-[[(4′-ethyl-[1,1′-biphenyl]-4-yl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 10% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 8.40 (s, 1H), 8.06 (s, 1H), 7.76-7.73 (m, 2H), 7.59 (m, 4H), 7.52-7.50 (m, 2H), 7.27 (d, J=8.2 Hz, 2H), 7.18 (t, J=8.6 Hz, 2H), 2.70 (q, J=7.6 Hz, 2H), 1.28 (t, J=7.6 Hz, 3H); 13 C NMR (CDCl 3 , 400 MHz) δ 166.0, 164.0, 152.7, 151.7, 143.4, 137.8, 137.4, 135.8, 130.4, 130.3, 128.3, 127.6, 126.8, 120.0, 116.5, 116.4, 28.5, 15.6; Anal. Calcd. for C 22 H 19 FN 2 O 2 : C=72.91%, H=5.28%, N=7.73%; found: C=72.51%, H=5.40%, N=7.63%.
EXAMPLE 76
Benzaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method B provided the title compound as white solid in 28% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.35 (s, 1H), 8.03 (br, 1H), 7.66 (d, J=8.5 2H), 7.47-7.39 (m, 5H), 7.28-7.25 (m, 2H), 7.02 (t, J=7.4 Hz, 1H), 6.98-6.92 (m, 4H); Mass spec.: 333.1 (MH + ); Anal. Calcd. for C 20 H 16 N 2 O 3 : C=72.28%, H=4.85%, N=8.43%; found: C=72.12%, H=4.80%, N=8.39%.
EXAMPLE 77
4-Fluorobenzaldehyde, O-[[(4-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method B provided the title compound as white solid in 26% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 8.39 (s, 1H), 7.99 (br, 1H), 7.75-7.71 (m, 2H), 7.48 (m, 2H), 7.33 (m, 2H), 7.19-7.15 (m, 2H), 7.09 (t, J=7.4 Hz, 1H), 7.05-6.98 (m, 4H); Anal. Calcd. for C 20 H 15 FN 2 O 3 .0.185H 2 O: C=68.11%, H=4.11%, N=7.94%; found: C=68.11%, H=4.36%, N=7.88%.
EXAMPLE 78
3-Pyridinecarboxaldehyde, O-[[[4-(phenylmethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method A provided the title compound as white solid in 50% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.90 (br, 1H), 8.75 (br, 1H), 8.43 (s, 1H), 8.09 (d, J=7.9 Hz, 1H), 7.84 (br, 1H), 7.44-7.31 (m, 8H), 6.98 (d, J=8.9 Hz, 2H), 5.07 (s, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 155.9, 152.6, 151.8, 151.1, 149.7, 136.9, 134.5, 129.9, 128.6, 128.0, 127.5, 123.9, 121.8, 115.5, 70.3; Mass spec.: 348.1 (MH + ); Anal. Calcd. for C 20 H 17 N 3 O 3 : C=69.15%, H=4.93%, N=12.10%; found: C=68.90%, H=5.05%, N=12.10%.
EXAMPLE 79
3-Pyridinecarboxaldehyde, O-[[[4-(2-phenylethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method A provided the title compound as white solid in 21% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.92 (br, 1H), 8.77 (br, 1H), 8.44 (s, 1H), 8.11 (d, J=7.9 Hz, 1H), 7.81 (br, 1H), 7.44 (br, 1H), 7.39 (d, J=8.9 Hz, 2H), 7.34-7.28 (m, 4H), 7.26-7.22 (m, 1H), 6.90 (dt, J=3.4 Hz, J=8.9 Hz, 2H), 4.17 (q, J=7.15 Hz, 2H), 3.10 (t, J=7.1 Hz, 3H); 13 C NMR (CDCl 3 , 500 MHz) δ 152.4, 151.8, 151.0, 149.5, 180.0, 136.5, 134.6, 129.0, 128.5, 126.5, 122.0, 115, 69.0, 35.8; Mass spec.: 362.0 (MH + ); Anal. Calcd. for C 21 H 19 N 3 O 3 : C=69.79%, H=5.30%, N=11.63%; found: C=69.42%, H=5.26%, N=11.65%.
EXAMPLE 80
3-Pyridinecarboxaldehyde, O-[[[4-(3-phenylpropoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method A provided the title compound as white solid in 26% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.94 (br, 1H), 8.79 (br, 1H), 8.44 (s, 1H), 8.10 (d, J=7.9 Hz, 1H), 7.82 (br, 1H), 7.45 (br, 1H), 7.40 (d, J=8.9 Hz, 2H), 7.30-7.28 (m, 2H), 7.22-7.18 (m, 3H), 6.90 (dt, J=3.4 Hz, J=8.9 Hz, 2H), 3.96 (t, J=6.3 Hz, 2H), 2.82 (t, J=7.35 Hz, 2H), 2.11 (m, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 161.5, 152.0, 150.5, 141.5, 134.5, 129.5, 128.5, 128.4, 125.9, 121.8, 115.1, 67.2, 32.1, 30.8; Mass spec.: 376.1 (MH + ); Anal. Calcd. for C 22 H 21 N 3 O 3 : C=70.38%, H=5.64%, N=11.19%; found: C=69.96%, H=5.59%, N=11.03%.
EXAMPLE 81
4-Fluorobenzaldehyde, O-[[[4-(phenylmethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 10% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.31 (s, 1H), 7.86 (br, 1H), 7.65 (dd, J=5.3 Hz, J=8.7 Hz, 2H), 7.37-7.30 (m, 6H), 7.27-7.24 (t, J=7.2 Hz, 1H), 7.09 (t, J=8.6 Hz, 2H), 6.91 (dt, J=3.4 Hz, J=8.9 Hz, 2H), 4.99 (s, 2H); Mass spec.: 365.1 (MH + ); Anal. Calcd. for C 21 H 17 FN 2 O 3 : C=69.22%, H=4.70%, N=7.69%; found: C=69.44%, H=4.84%, N=7.54%.
EXAMPLE 82
4-Fluorobenzaldehyde, O-[[[4-(2-phenylethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 48% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.31 (s, 1H), 7.85 (br, 1H), 7.67-7.63 (m, 2H), 7.32 (d, J=8.9 Hz, 2H), 7.27-7.21 (m, 4H), 7.18 (t, J=7.0 Hz, 1H), 6.83 (dt, J=3.4 Hz, J=8.9 Hz, 2H), 4.10 (t, J=7.2 Hz, 2H), 3.03 (t, J=7.1 Hz, 2H); Mass spec.: 379.1 (MH + ); Anal. Calcd. for C 22 H 19 FN 2 O 3 : C=69.83%, H=5.06%, N=7.40%; found: C=69.71%, H=5.05%, N=7.21%.
EXAMPLE 83
4-Fluorobenzaldehyde, O-[[[4-(3-phenylpropoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 32% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.30 (s, 1H), 7.85 (br, 1H), 7.67-7.63 (m, 2H), 7.33 (d, J=8.9 Hz, 2H), 7.22 (t, J=6.0 Hz, 2H), 7.15-7.01 (m, 5H), 6.82 (dt, J=3.4 Hz, J=8.9 Hz, 2H), 3.88 (t, J=6.3 Hz, 2H), 2.74 (t, J=7.4 Hz, 2H), 2.03 (m, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.2, 152.5, 141.5, 130.3, 130.3, 129.7, 128.5, 128.4, 125.9, 121.8, 116.5, 116.3, 115.0, 67.2, 32.1, 30.8; Mass spec.: 393.0 (MH + ); Anal. Calcd. for C 23 H 21 FN 2 O 3 .0.1H 2 O: C=70.07%, H=5.42%, N=7.10%; found: C=70.09%, H=5.46%, N=6.71%.
EXAMPLE 84
Benzaldehyde, O-[[[4-(phenylmethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 33% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.41 (s, 1H), 8.02 (br, 1H), 7.72-7.70 (m, 2H), 7.54-7.37 (m, 9H), 7.34-7.31 (m, 1H), 6.98 (dt, J=3.4 Hz, J=6.9 Hz, 2H), 5.07 (s, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 155.7, 153.6, 136.9, 131.9, 130.1, 129.8, 129.1, 128.6, 128.2, 128.0, 127.5, 121.8, 115.4; Mass spec.: 347.0 (MH + ); Anal. Calcd. for C 21 H 18 N 2 O 3 : C=72.82%, H=5.24%, N=8.09%; found: C=72.69%, H=5.28%, N=8.00%.
EXAMPLE 85
Benzaldehyde, O-[[[4-(2-phenylethoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 23% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.41 (s, 1H), 8.01 (br, 1H), 7.72-7.70 (m, 2H), 7.54-7.45 (m, 3H), 7.41 (d, J=8.9 Hz, 2H), 7.34-7.28 (m, 4H), 7.26-7.23 (m, 2H), 6.90 (dt, J=3.3 Hz, J=9.0 Hz, 2H), 4.17 (t, J=7.2 Hz, 2H), 3.10 (t, J=7.1 Hz, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 153.6, 152.3, 138.2, 136.2, 131.9, 129.9, 129.8, 129.1, 129.0, 128.5, 128.2, 126.5, 121.8, 115.1, 69.0, 35.8; Mass spec.: 361.0 (MH + ); Anal. Calcd. for C 22 H 20 N 2 O 3 : C=73.32%, H=5.59%, N=7.77%; found: C=73.34%, H=5.82%, N=7.73%.
EXAMPLE 86
Benzaldehyde, O-[[[4-(3-phenylpropoxy)phenyl]amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 25% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.41 (s, 1H), 8.02 (br, 1H), 7.72-7.71 (m, 2H), 7.54-7.46 (m, 3H), 7.41 (d, J=8.9 Hz, 2H), 7.30 (t, J=6.85 Hz, 2H), 7.23-7.19 (m, 3H), 6.90 (dt, J=3.4 Hz, J=9.0 Hz, 2H), 3.96 (t, J=6.3 Hz, 2H), 2.82 (t, J=7.4 Hz, 2H), 2.12 (m, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.1, 153,6, 152.4, 141.5, 136.2, 131.9, 129.85, 129.80, 128.5, 128.4, 128.2, 126.0, 121.8, 115.0, 67.2, 32.1, 30.8; Mass spec.: 375.0 (MH + ); Anal. Calcd. for C 23 H 22 N 2 O 3 : C=73.78%, H=5.92%, N=7.48%; found: C=73.82%, H=6.02%, N=7.35%.
EXAMPLE 87
3-Pyridinecarboxaldehyde, O-[[(3-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 34% yield. 1 H NMR (DMSO, 400 MHz) δ 10.06 (s, 1H), 8.93 (d, J=1.6 Hz, 1H), 8.70 (d, J=1.6 Hz, 1H), 8.69 (s, 1H), 8.21 (dt, J=2.0 Hz, J=8.1 Hz, 1H), 7.54 (dd, J=4.9 Hz, J=7.8 Hz, 1H), 7.40 (t, J=7.4 Hz, 2H), 7.34 (t, J=8.1 Hz, 1H), 7.29-7.26 (m, 2H), 7/16 (t, J=7.4 Hz, 1H), 7.03 (dd, J=1.1 Hz, J=8.7 Hz, 2H), 6.71 (m, 1H); 13 C NMR (DMSO, 400 MHz) δ 158.1, 152.6, 151.3, 149.7, 138.1, 134.6, 130.3, 129.8, 123.6, 119.2, 114.7, 114.3, 110.2; Mass spec.: 334.0 (MH + ); Anal. Calcd. for C 19 H 14 N 3 O 3 : C=68.46%, H=4.54%, N=12.61%; found: C=68.42%, H=4.42%, N=12.62%.
EXAMPLE 88
4-Fluorobenzaldehyde, O-[[(3-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 34% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.36 (s, 1H), 8.00 (br, 1H), 7.12 (m, 2H), 7.37-7.27 (m, 4H), 7.22 (t, J=2.1 Hz, 1H), 7.17-7.10 (m, 3H), 7.04 (dt, J=1.1 Hz, J=7.6 Hz, 2H), 6.78 (dt, J=2.1 Hz, J=7.1 Hz, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 165.9, 163.9, 158.0, 156.9, 152.8, 151.6, 138.3, 130.4, 130.3, 130.2, 129.8, 126.0, 125.9, 123.5, 119.1, 116.5, 116.4, 114.6, 114.4, 110.3; Mass spec.: 350.9 (MH + ); Anal. Calcd. for C 20 H 15 FN 2 O 3 : C=68.57%, H=4.32%, N=8.00%; found: C=68.77%, H=4.48%, N=7.76%.
EXAMPLE 89
4-Fluorobenzaldehyde, O-[[(2-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 16% yield, mp 141.5-142.0° C. 1 H NMR (CDCl 3 , 500 MHz) δ 8.73 (br, 1H), 8.32 (dd, J=1.3 Hz, J=8.2 Hz, 1H), 8.30 (s, 1H), 7.55-7.51 (m, 2H), 7.36 (t, J=8.7 Hz, 2H), 7.21 (t, J=7.8 Hz, 1H), 7.12 (t, J=7.4 Hz, 1H), 7.11-7.08 (m, 3H), 7.03 (d, J=8.7 Hz, 2H), 6.98 (d, J=1.4 Hz, J=8.1, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.8, 152.2, 145.0, 130.2, 130.1, 129.9, 129.4, 124.8, 124.1, 123.5, 119.9, 119.1, 117.4, 116.3, 116.2; Mass spec.: 351.0 (MH + ); Anal. Calcd. for C 20 H 15 FN 2 O 3 .0.41H 2 O: C=67.15%, H=4.46%, N=7.83; found: C=67.13%, H=4.39%, N=7.76%.
EXAMPLE 90
Benzaldehyde, O-[[(2-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 16% yield, mp 141.5-142.0° C. 1 H NMR (CDCl 3 , 500 MHz) δ 8.73 (br, 1H), 8.32 (dd, J=1.3 Hz, J=8.2 Hz, 1H), 8.30 (s, 1H), 7.55-7.51 (m, 2H), 7.36 (t, J=8.7 Hz, 2H), 7.21 (t, J=7.8 Hz, 1H), 7.12 (t, J=7.4 Hz, 1H), 7.11-7.08 (m, 3H), 7.03 (d, J=8.7 Hz, 2H), 6.98 (d, J=1.4 Hz, J=8.1, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.8, 152.2, 145.0, 130.2, 130.1, 129.9, 129.4, 124.8, 124.1, 123.5, 119.9, 119.1, 117.4, 116.3, 116.2; Mass spec.: 351.0 (MH + ); Anal. Calcd. for C 20 H 15 FN 2 O 3 .0.41H 2 O: C=67.15%, H=4.46%, N=7.83; found: C=67.13%, H=4.39%, N=7.76%.
EXAMPLE 91
Benzaldehyde, O-[[(3-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as gel-like material in 50% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.39 (s, 1H), 8.11 (br, 1H), 7.70 (d, J=5.1 Hz, 2H), 7.53-7.45 (m, 3H), 7.37-7.28 (m, 4H), 7.24-7.23 (m 1H), 7.12 (t, J=7.4 Hz, 1H), 7.04 (m, J=7.7 Hz, 2H), 6.79-6.76 (m, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 158.0, 156.9, 153.9, 151.7, 138.3, 132.0, 130.2, 129.8, 129.6, 129.1, 128.9, 128.2, 123.5, 119.2, 119.1, 114.6, 114.4, 110.4; Mass spec.: 333.0 (MH + ); Anal. Calcd. for C 20 H 16 N 2 O 3 : C=72.28%, H=4.85%, N=8.43%; found: C=72.10%, H=4.72%, N=8.40%.
EXAMPLE 92
3-Pyridinecarboxaldehyde, O-[[(2-phenoxyphenyl)amino]carbonyl]oxime (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 42% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 13.26 (br, 1H), 8.91 (d, J=1.6 Hz, 1H), 8.81 (dd, J=1.4 Hz, J=5.2 Hz, 1H), 8.45 (s, 1H), 8.38 (br, 1H), 8.29-8.27 (m, 2H), 7.66 (dd, J=5.2 Hz, J=8.0 Hz, 1H), 7.37 (t, J=7.5 Hz, 2H), 7.20 (t, J=7.8 Hz, 1H), 7.15 (t, J=7.4 Hz, 1H), 7.08 (td, J=1.5 Hz, J=8.1 Hz, 1H), 7.04 (d, J=8.0 Hz, 1H), 6.95 (dd, J=1.3 Hz, J=8.1 Hz, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 16101, 160.7, 156.5, 150.6, 149.2, 147.9, 145.5, 145.3, 138.3, 130.1, 128.8, 128.5, 125.6, 124.7, 124.5, 123.8, 119.8, 118.7, 117.8, 116.7, 114.4; Mass spec.: 334.0 (MH + ); Anal. Calcd. for C 19 H 15 N 3 O 3 .0.185H 2 O: C=67.78%, H=4.60%, N=12.48%; found: C=67.74%, H=4.46%, N=12.47%.
EXAMPLE 93
4-Hexyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.81 min. (99%). Mass Spec: 314 (MH+).
EXAMPLE 94
4-Hexyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.80 min. (97%). Mass Spec: 331.39 (MH+).
EXAMPLE 95
4-Butoxyphenylcarbamic acid, methyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.40 (br. s, 1H), 7.32 (d, 2H, J=8.0 Hz), 6.83 (dd, 2H, J=7.5, 2.5 Hz), 3.89 (t, 2H, J=6.5 Hz), 1.65 (m, 2H), 1.40 (m, 2H), 0.92 (t, 3H, J=7.5 Hz). Analytical HPLC 1.51 min. (95%). Mass Spec: 224.15 (MH+).
EXAMPLE 96
4-Heptyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.08 min. (91%). Mass Spec: 328.18 (MH+).
EXAMPLE 97
4-Heptyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.06 min. (99%). Mass Spec: 346.17 (MH+).
EXAMPLE 98
4-Octyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.97 min. (85%). Mass Spec: 342.29 (MH+).
EXAMPLE 99
4-Octyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.64 min. (90%). Mass Spec: 360.26 (MH+).
EXAMPLE 100
4-Butyloxyphenylcarbamic acid, 4-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.47 (d, 2H, J=7.0 Hz), 7.38 (d, 2H, J=4.0 Hz), 7.25 (d, 2H, J=7.0 Hz), 6.90 (dd, 2H, J=6.0, 2.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.40 (m, 2H), 0.92 (t, 3H, J=7.5 Hz); Analytical HPLC 1.90 min. (95%). Mass Spec: 320 (MH+).
EXAMPLE 101
4-Decyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.09 min. (97%). Mass Spec: 370.38 (MH+).
EXAMPLE 102
4-Decyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.07 min. (98%). Mass Spec: 388.43 (MH+).
EXAMPLE 103
4-Undecyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.33 min. (93%). Mass Spec: 384.26 (MH+).
EXAMPLE 104
4-Undecyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.31 min. (96%). Mass Spec: 402.25 (MH+).
EXAMPLE 105
4-Dodecyloxyphenylcarbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.18 min. (85%). Mass Spec: 398.36 (MH+).
EXAMPLE 106
4-Dodecyloxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 2.18 min. (95%). Mass Spec: 416.38 (MH+).
EXAMPLE 107
4-Butoxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.61 min. (97%). Mass Spec: 304.18 (MH+).
EXAMPLE 108
4-Butoxyphenylcarbamic acid, 4-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 7.33 (d, 2H, J=8.1 Hz), 7.23 (m, 4H), 6.90 (dd, 2H, J=7.0, 2.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.72 (m, 2H), 1.42 (m, 2H), 0.91 (t, 3H, J=7.0 Hz). Analytical HPLC 1.65 min. (95%). Mass Spec: 304.18 (MH+).
EXAMPLE 109
4-Butoxyphenylcarbamic acid, 3,4-difluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.71 min. (97%). Mass Spec: 322 (MH+).
EXAMPLE 110
4-Butoxyphenylcarbamic acid, 2-methoxyphenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.57 min. (97%). Mass Spec: 316.18 (MH+).
EXAMPLE 111
4-(Butoxyphenylmethyl)carbamic acid, phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.59 min. (95%). Mass Spec: 300.0 (MH+).
EXAMPLE 112
4-(Butoxyphenylmethyl)carbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.40 (br. s, 1H), 7.26 (m, 6H), 6.90 (d, 2H, J=8.4 Hz), 4.19 (d, 2H, J=6.0 Hz), 3.92 (t, 2H, J=6.5 Hz), 1.67 (m, 2H), 1.42 (m, 2H), 0.91 (t, 3H, J=7.0 Hz). Analytical HPLC 1.59 min. (95%). Mass Spec: 318 (MH+).
EXAMPLE 113
4-(Butoxyphenylmethyl)carbamic acid, 4-methoxyphenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.60 min. (95%). Mass Spec: 330.25 (MH+).
EXAMPLE 114
4-(Butoxyphenylmethyl)carbamic acid, 6-quinolinyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.30 min. (95%). Mass Spec: 351.25 (MH+).
EXAMPLE 115
4-(Butoxyphenylmethyl)carbamic acid, 1-naphthalenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.77 min. (95%). Mass Spec: 350 (MH+).
EXAMPLE 116
4-(Butoxyphenylmethyl)carbamic acid, 2-naphthalenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.80 min. (98%). Mass Spec: 350.26 (MH+).
EXAMPLE 117
4-(Butoxyphenylmethyl)carbamic acid, 4-(1-methylethyl)phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.82 min. (95%). Mass Spec: 342 (MH+).
EXAMPLE 118
4-(Butoxyphenylmethyl)carbamic acid, 3-(dimethylamino)phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.32 min. (90%). Mass Spec: 343.29 (MH+).
EXAMPLE 119
4-(Butoxyphenylmethyl)carbamic acid, 4-(trifluoromethyl)phenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.77 min. (99%). Mass Spec: 368.14 (MH+).
EXAMPLE 120
4-(Butoxyphenylmethyl)carbamic acid, 2,4-difluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.66 min. (99%). Mass Spec: 336.14 (MH+).
EXAMPLE 121
4-(Butoxyphenylmethyl)carbamic acid, 4-fluorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.61 min. (85%). Mass Spec: 318.15 (MH+).
EXAMPLE 122
4-(Butoxyphenylmethyl)carbamic acid, 3-chlorophenyl ester (Scheme 1B, Compound D″) Prepared as described for the example above. Analytical HPLC 1.72 min. (86%). Mass Spec: 334.12 (MH+).
EXAMPLE 123
4-Phenoxyphenylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method C provided the title compound as white solid in 11% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 7.43 (br, 1H), 7.41 (br, 1H), 7.35-7.30 (m, 2H), 7.28-7.13 (m, 4H), 7.09 (dt, J=0.9 Hz, J=7.4 Hz, 1H), 7.03-6.97 (m, 5H); (s, 1H), 8.06 (s, 1H), 7.76-7.73 (m, 2H), 7.59 (m, 4H), 7.52-7.50 (m, 2H), 7.27 (d, J=8.2 Hz, 2H), 7.18 (t, J=8.6 Hz, 2H), 2.70 (q, J=7.6 Hz, 2H), 1.28 (t, J=7.6 Hz, 3H); 13 C NMR (CDCl 3 , 400 MHz) δ 153.6, 129.8, 129.7, 127.0, 126.9, 124.4, 124.1, 123.1, 120.5, 119.8, 119.6, 118.6, 118.5, 116.8, 116.7; Anal. Calcd. for C 19 H 14 FNO 3 : C=70.58%, H=4.36%, N=4.33%; found: C=70.54%, H=4.31%, N=4.21%.
EXAMPLE 124
4′-Ethyl-[1,1′-biphenyl]-4-ylcarbamic acid, 2-fluorophenyl ester (Scheme 1B, Compound D′) Prepared as described for the example above. Using work-up method B provided the title compound as white solid in 30% yield. 1 H NMR (CDCl 3 , 400 MHz) δ 7.57-7.55 (m, 2H), 7.52-7.49 (m, 4H), 7.36-7.33 (m, 1H), 7.30-7.27 (m, 2H), 7.25-7.14 (m, 3H), 7.05 (br, 1H), 2.70 (q, J=7.6 Hz, 2H), 1.28 (t, J=7.6 Hz, 3H); Anal. Calcd. for C 21 H 18 FNO 2 : C=75.21%, H=5.41%, N=4.18%; found: C=75.27%, H=5.40%, N=4.25%.
The following Intermediates 40 to 41 may be used to synthesize Examples 125 to 135.
2-(4-Butoxy-phenyl)-butyric acid methyl ester: (Scheme 2, Compound E) The mixture of methyl 4-butoxyphenylacetate (1.20 g, 5.4 mmol) and NaH (60% in mineral oil, 0.50 g, 12.5 mmol) in DMF (25.0 mL) was stirred at 50° C. for 40 min. Bromoethane (2.0 g, 18.3 mmol) was added and the stirring continued at rt for one hour. The reaction mixture was diluted with EtOAc (300 mL), washed with H 2 O, and then was dried over Na 2 SO 4 . After filtration and concentration in vacuo, the residue was purified by flash chromatography (SiO 2 : EtOAc/Hexanes). This compound was obtained as a yellow oil (0.85 g, 3.4 mmol, 63% yield). 1 H NMR (DMSO-d 6 ) δ 7.16 (d, 2H, J=7.0 Hz), 6.87 (d, 2H, J=8.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 3.55 (s, 3H), 3.45 (t, 1H, J=9.0), 1.93 (m, 1H), 1.63 (m, 2H), 1.42 (m, 2H), 0.97 (t, 3H, J=7.2 Hz), 0.79 (t, 3H, J=4.0 Hz).
2-(4-Butoxy-phenyl)-butyric acid: (Scheme 2, Compound F) To a solution of 2-(4-butoxy-phenyl)-butyric acid methyl ester (2.0 g, 8.0 mmol) in EtOH (30 mL) was added NaOH (10 N, 6 mL, 60 mmol). The resulting mixture was stirred at rt for 3 hours, diluted with H 2 O (30 mL), acidified to pH˜1.0 using HCl (6N). The precipitates were filtered off by filter paper, washed by H 2 O and hexanes. This compound was obtained as a white solid. (1.4 g, 5.9 mmol, 74% yield). 1 H NMR (DMSO-d 6 ) δ 12.20 (br. s, 1H), 7.16 (d, 2H, J=7.0 Hz), 6.87 (d, 2H, J=8.5 Hz), 3.92 (t, 2H, J=6.5 Hz), 3.31 (t, 2H, J=6.9 Hz), 1.93 (m, 1H), 1.63 (m, 3H), 1.42 (m, 2H), 0.97 (t, 3H, J=7.2 Hz), 0.79 (t, 3H, J=4.0 Hz).
EXAMPLE 125
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid quinolin-6-yl ester (Scheme 2, Compound G) To a solution of 2-(4-butoxy-phenyl)-butyric acid (0.050 g, 0.23 mmol) and Et 3 N (0.053 g, 0.53 mmol) in toluene (2 mL) was added diphenylphosphoryl azide (0.096 g, 0.35 mmol). The resultant mixture was stirred at r.t. for 10 min. and then at 107° C. under N 2 for 60 min. After the mixture was cooled to r.t., quinolin-6-ol (0.050 g, 0.34 mmol) was added. The reaction mixture was stirred at r.t. for 10 min. and then at 80° C. for 1 h. The mixture was diluted with EtOAc, washed with H 2 O. After filtration and concentration in vacuo, the residue was purified by by preparative HPLC (YMC 30×100 mm (5 uM packing), 10% MeOH/90% water/01% TFA as mobile phase A, 90% MeOH/10% water/0.1% TFA as mobile phase B). This compound was obtained as a pale yellow solid (0.040 g, 0.11 mmol, 46% yield): mp 115-118° C.; 1 H NMR (DMSO-d 6 ) δ 8.93 (m, 1H), 8.45 (d, 1H, J=9.0 Hz), 8.40 (d, 1H, J=8.5), 8.02 (d, 1H, J=9.0 Hz), 7.77 (s, 1H), 7.62 (dd, 1H, J=8.5, 4.5 Hz), 7.55 (dd, 1H, J=9.0, 2.5 Hz), 7.25 (d, 2H, J=8.5 Hz), 6.98 (d, 2H, J=8.5 Hz), 4.43 (m, 1H), 3.95 (t, 2H, J=6.5 Hz), 1.75 (m, 1H), 1.65 (m, 3H), 1.42 (m, 2H), 0.90 (m, 6H). Mass Spec: 379.33 (MH + ).
EXAMPLE 126
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 4-methoxy-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.73 min. (88%). Mass Spec: 358.25 (MH+).
EXAMPLE 127
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid naphthalen-1-yl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.86 min. (98%). Mass Spec: 378.25 (MH+).
EXAMPLE 128
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid naphthalen-2-yl ester (Scheme 2, Compound G) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 8.30 (d, 1H, J=9.0 Hz), 7.90 (m, 3H), 7.60 (s, 1H), 7.45 (m, 2H), 7.25 (m, 3H), 6.90 (d, 2H, J=8.5 Hz), 4.43 (m, 1H), 3.95 (t, 2H, J=6.5 Hz), 1.75 (m, 1H), 1.65 (m, 3H), 1.42 (m, 2H), 0.90 (m, 6H). Analytical HPLC 1.87 min. (99%). Mass Spec: 378.12 (MH+).
EXAMPLE 129
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 4-isopropyl-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.91 min. (96%). Mass Spec: 370.31 (MH+).
EXAMPLE 130
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 3-trifluoromethyl-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.84 min. (96%). Mass Spec: 396.18 (MH+).
EXAMPLE 131
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 2,4-difluoro-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.77 min. (89%). Mass Spec: 364.17 (MH+).
EXAMPLE 132
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 4-fluoro-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.72 min. (89%). Mass Spec: 346.18 (MH+).
EXAMPLE 133
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 4-dimethylamino-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.53 min. (96%). Mass Spec: 371 (MH+).
EXAMPLE 134
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.70 min. (88%). Mass Spec: 328.19 (MH+).
EXAMPLE 135
[1-(4-Butoxy-phenyl)-propyl]-carbamic acid 2-fluoro-phenyl ester (Scheme 2, Compound G) Prepared as described for the example above. Analytical HPLC 1.70 min. (89%). Mass Spec: 346.18 (MH+).
The following Intermediates 42 and 43 may be used to synthesize Examples 136 to 140.
4-Decanoylamino-benzoic acid ethyl ester: (Scheme 3, Compound H) To a solution of 4-amino-benzoic acid ethyl ester (2.0 g, 12.1 mmol) and decanoyl chloride (2.35 g, 13.3 mmol) in methylene chloride (20 mL) was added Et 3 N (1.34 g, 13.3 mmol). The resultant mixture was stirred at room temperature for one hour and then was diluted with EtOAc, washed by H 2 O, dried over MgSO 4 . After filtration and concentration in vacuo, the product was directly used in the next step.
4-Decanoylamino-benzoic acid: (Scheme 3, Compound I) To a solution of 4-decanoylamino-benzoic acid ethyl ester (2.0 g, 6.6 mmol) in EtOH (30 mL) was added NaOH (10 N, 6 mL, 60 mmol). The resulting mixture was stirred at rt for 3 hours, diluted with H 2 O (30 mL), acidified to pH˜1.0 using HCl (6N). The precipitates were filtered off by filter paper, washed by H 2 O and hexanes. This compound was obtained as a white solid. (1.8 g, 6.5 mmol, 98% yield). 1 H NMR (DMSO-d 6 ) δ 9.91 (br. s, 1H), 7.76 (d, 2H, J=8.7 Hz), 6.50 (d, 2H, J=8.7 Hz), 2.29 (t, 2H, J=7.5 Hz), 1.57 (m, 2H), 1.25 (m, 12H), 0.85 (t, 3H, J=6.9 Hz). Mass Spec: 278.21 (MH + ).
EXAMPLE 136
Benzaldehyde, O-[[(4-Nonanoylamino-phenyl)amino]carbonyl]oxime (Scheme 3, Compound J) To a solution of 4-decanoylamino-benzoic acid (0.050 g, 0.18 mmol) and Et 3 N (0.053 g, 0.53 mmol) in toluene (2 mL) was added diphenylphosphoryl azide (0.096 g, 0.35 mmol). The resultant mixture was stirred at r.t. for 10 min. and then at 107° C. under N 2 for 60 min. After the mixture was cooled to r.t., benzaldehyde oxime (0.050 g, 0.41 mmol) was added. The reaction mixture was stirred at r.t. for 10 min. and then at 80° C. for 30 min. The mixture was diluted with EtOAc, washed with H 2 O. After filtration and concentration in vacuo, the residue was purified by preparative HPLC (YMC 30×100 mm (5 uM packing), 10% MeOH/90% water/01% TFA as mobile phase A, 90% MeOH/10% water/0.1% TFA as mobile phase B). This compound was obtained as a pale yellow solid (0.038 g, 0.10 mmol, 53% yield): 1 H NMR (DMSO-d 6 ) δ 9.78 (d, 2H, J=9.0 Hz), 8.63 (s, 1H), 7.82 (dd, 2H, J=7.7, 2.4 Hz), 7.52 (m, 5H), 7.44 (d, 2H, J=9.0 Hz), 2.27 (t, 2H, J=9.0 Hz), 1.55 (m, 2H), 1.26 (m, 10H), 0.85 (t, 3H, J=6.6 Hz). Mass Spec: 396.22 (MH + ).
EXAMPLE 137
4-Fluorobenzaldehyde, O-[[(4-Nonanoylamino-phenyl)amino]carbonyl]oxime (Scheme 3, (Compound J) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.78 (d, 2H, J=9.0 Hz), 8.63 (s, 1H), 7.82 (dd, 2H, J=8.7, 5.4 Hz), 7.52 (d, 2H, J=9.0 Hz), 7.32 (m, 4H), 2.27 (t, 2H, J=9.0 Hz), 1.55 (m, 2H), 1.26 (m, 10H), 0.85 (t, 3H, J=6.6 Hz). Anal. Calcd for C 23 H 28 FN 3 O 3 : C, 66.81; H, 6.82; N, 10.16. Found: C, 67.07, H, 6.82; N, 10.09. Mass Spec: 414.21 (MH+).
EXAMPLE 138
3-Trifluoromethylbenzaldehyde, O-[[(4-Nonanoylamino-phenyl)amino]carbonyl]oxime (Scheme 3, Compound J) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.78 (d, 2H, J=9.0 Hz), 8.63 (s, 1H), 8.15 (m, 2H), 7.92 (d, 1H, J=9.0 Hz), 7.80 (t, 1H, J=7.5 Hz), 7.52 (d, 2H, J=9.0 Hz), 7.32 (d, 2H, J=9.0 Hz) 2.27 (t, 2H, J=9.0 Hz), 1.55 (m, 2H), 1.26 (m, 10H), 0.85 (t, 3H, J=6.6 Hz). Anal. Calcd for C 24 H 28 F 3 N 3 O 3 : C, 62.19; H, 6.08; N, 9.06. Found: C, 62.45, H, 6.12; N, 8.99. Mass Spec: 464.21 (MH+).
EXAMPLE 139
2,4-Difluorobenzaldehyde, O-[[(4-Nonanoylamino-phenyl)amino]carbonyl]oxime (Scheme 3, Compound J) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.78 (s, 2H), 8.63 (s, 1H), 8.05 (m, 1H), 7.52 (m, 4H), 7.22 (m, 1H), 2.27 (t, 2H, J=9.0 Hz), 1.55 (m, 2H), 1.26 (m, 10H), 0.85 (t, 3H, J=6.6 Hz). Mass Spec: 432.20 (MH+).
EXAMPLE 140
3,4-Difluorobenzaldehyde, O-[[(4-Nonanoylamino-phenyl)amino]carbonyl]oxime (Scheme 3, Compound J) Prepared as described for the example above. 1 H NMR (DMSO-d 6 ) δ 9.78 (d, 2H, J=8.1 Hz), 8.63 (s, 1H), 8.00 (m, 1H), 7.72-7.42 (m, 6H), 2.27 (t, 2H, J=9.0 Hz), 1.55 (m, 2H), 1.26 (m, 10H), 0.85 (t, 3H, J=6.6 Hz). Mass Spec: 432.20 (MH+).
Scheme 4 Reaction conditions: (i) (a) Et 3 N, DPPA/toluene, room temp. to 120° C., (b) oxime, room temp. to 85° C.; A is indolyl wherein K is the corresponding indole carboxylic acid, pyridyl wherein K is the corresponding pyridyl carboxylic acid, or benzofuranyl wherein K is the dibenzofurancarboxylic acid.
Examples 141 to 145 were made accordingly.
EXAMPLE 141
3-Pyridinecarboxaldehyde, O-[[(1H-indol-5-yl)amino]carbonyl]oxime (Scheme 4, Compound L) To a suspension of indole-5-carboxylic acid (commercially available) (1 mmol) in toluene was added triethylamine (4.0 mmol) and diphenylphosphoryl azide (DPPA) (1.2 mmol) subsequently at room temperature under nitrogen atmosphere. The resultant was stirred for 15 minutes at room temperature followed by 90 minutes at reflux. The reaction mixture was cooled down to room temperature followed by the addition of the corresponding oxime, 3-pyridinealdoxime, (1 mmol). The resultant was stirred for 1 hour at room temperature or followed by heating up to 85° C. Using work-up method A: filtration of the reaction mixture, and the solid was recrystallized from EtOAc/hexanes, provided the title compound as a white solid in 57% yield. 1 H NMR (DMSO, 500 MHz) δ 10.99 (s, 1H), 9.68 (s, 1H), 8.94 (d, J=1.7 Hz, 1H), 8.68-8.66 (m, 2H), 8.25 (dt, J=7.9 Hz, J=1.8 Hz, 1H), 7.66 (br, 1H), 7.53 (dd, J=4.8 Hz, J=8.0 Hz, 1H), 7.35 (d, J=8.6 Hz, 1H), 7.31 (t, J=2.8 Hz, 1H), 7.16 (dd, J=1.8 Hz, J=8.6 Hz, 1H), 6.40 (s, 1H); Mass spec.: 281.1 (MH + ); Anal. Calcd. for C 15 H 12 N 4 O 2 : C=64.28%, H=4.32%, N=19.99%; found: C=64.09%, H=4.45%, N=19.759%.
EXAMPLE 142
4-Fluorobenzaldehyde, O-[[(1H-indol-5-yl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method C: after removal of solvent, the residue was dissolved in methanol and filtrated, the filtrate was purified by preparative HPLC with methanol:H 2 O (30:70 to about 100:0 v/v, containing 1% TFA) as a mobile phase to provide the title compound as white solid in 19% yield. 1 H NMR (DMSO, 500 MHz) δ 11.03 (s, 1H), 9.59 (s, 1H), 8.64 (s, 1H), 7.93 (dd, J=5.6 Hz, J=8.8 Hz, 2H), 7.69 (br, 1H), 7.38-7.32 (m, 3H), 7.20 (dd, J=1.8 Hz, J=8.7 Hz, 1H), 6.39 (t, J=2.0 Hz, 1H); Mass spec.: 298.0 (MH + ); Anal. Calcd. for C 16 H 12 N 3 O 2 F.0.51H 2 O: C=62.713%, H=4.28%, N=13.71%; found: C=62.73%, H=4.13%, N=14.02%.
EXAMPLE 143
Benzaldehyde, O-[[(1H-indol-5-yl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method C provided the title compound as white solid in 20% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.43 (s, 1H), 8.19 (br, 1H), 8.15 (br, 1H), 7.82 (br, 1H), 7.74 (d, J=6.8 Hz, 2H), 7.54-7.46 (m, 3H), 7.38 (d, J=8.6 Hz, 1H), 7.29 (dd, J=1.8 Hz, J=8.7 Hz, 1H), 7.24 (t, J=2.7 Hz, 1H), 6.55 (t, J=2.2 Hz, 1H); Mass spec.: 280.0 (MH + ); Anal. Calcd. for C 16 H 13 N 3 O 2 .0.16H 2 O: C=68.11%, H=4.76%, N=14.89%; found: C=68.15%, H=4.77%, N=14.75%.
EXAMPLE 144
4-Fluorobenzaldehyde, O-[[(1H-indol-3-yl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using workup method C and then B provided the title compound as light blue solid in 20% yield. 1 H NMR (DMSO, 500 MHz) δ 10.91 (s, 1H), 9.59 (s, 1H), 8.66 (s, 1H), 7.93 (t, J=5.7 Hz, 1H), 7.66 (d, J=7.9 Hz, 1H), 7.44 (m, 1H), 7.36 (t, J=8.1 Hz, 2H), 7.25 (m, 1H), 7.10 (t, J=8.1 Hz, 1H), 7.0 (t, J=7.7 Hz, 1H).
EXAMPLE 145
Benzaldehyde, O-[[(1H-indol-3-yl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method C and then B (after removal of the solvent, the residue was chromatographed by silica gel column packed with EtOAc/hexanes or EtOAc/dichloromethane) provided the title compound as a light blue solid in 11% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.45 (s, 1H), 8.15 (br, 1H), 8.05 (br, 1H), 7.75 (d, J=6.9 Hz, 2H), 7.62 (d, J=1.5 Hz, 1H), 7.57 (d, J=8.0 Hz, 1H), 7.55-7.48 (m, 3H), 7.39 (d, J=8.2 Hz, 1H), 7.25 (t, J=8.0 Hz, 1H), 7.18 (t, J=7.9 Hz, 1H); Mass spec.: 280.0 (MH + ). Anal. Calcd. for C 16 H 13 N 3 O 2 .0.21H 2 O: C=67.89%, H=4.78%, N=14.84%; found: C=67.91%, H=4.94%, N=14.17%.
EXAMPLE 146
4-Fluorobenzaldehyde, O-[[[4-[(4-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method B provided the title compound as light blue solid in 29% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.47 (d, J=6.0 Hz, 2H), 8.40 (s, 1H), 8.15 (br, 1H), 7.74 (dd, J=8.05 Hz, J=11.55 Hz, 2H) 7.6 (d, J=8.9 Hz, 2H), 7.17 (t, J=8.55 Hz, 2H), 7.11 (d, J=8.9 Hz, 2H), 6.86 (dd, J=1.5 Hz, J=4.8 Hz, 2H); Mass spec.: 352.34 (MH + ).
EXAMPLE 147
3-Pyridinecarboxaldehyde, O-[[[4-[(2-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method B provided the title compound as white solid in 30% yield. 1 H NMR (DMSO, 300 MHz) δ 9.96 (s, 1H), 8.97 (d, J=1.8 Hz, 1H), 8.73 (s, 1H), 8.72 (dd, J=1.8 Hz, J=4.9 Hz, 1H), 8.25 (dt, J=8.0 Hz, J=2.0 Hz, 1H), 8.14 (dd, J=2.1 Hz, J=5.2 Hz, 1H), 7.84 (td, J=1.9 Hz, J=7.1 Hz, 1H), 7.57-7.53 (m, 3H), 7.13-7.09 (m, 3H), 7.01 (d, J=8.4 Hz, 1H); Mass spec.: 335.11 (MH + ). Anal. Calcd. for C 18 H 14 N 4 O 3 : C=64.67%, H=4.22%, N=16.76%; found: C=64.41%, H=4.16%, N=16.50%.
EXAMPLE 148
4-Fluorobenzaldehyde, O-[[[4-[(2-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using workup method B provided the title compound as white solid in 22% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.39 (s, 1H), 8.20 (dd, J=4.9 Hz, J=1.4 Hz, 1H), 8.05 (br, 1H), 7.75-7.68 (m, 3H), 7.55 (d, J=8.85 Hz, 2H), 7.19-7.14 (m, 4H), 7.00 (dd, J=5.1 Hz, J=7.2 Hz, 1H), 6.91 (d, J=8.30 Hz, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 165.9, 163.9, 163.7, 152.7, 151.9, 150.5, 147.5, 139.7, 133.5, 130.4, 130.3, 126.03, 126.00, 121.9, 121.2, 118.5, 116.5, 116.4, 111.4; Mass spec.: 352.25 (MH + ). Anal. Calcd. for C 19 H 14 N 3 O 3 F.0.36H 2 O: C=63.78%, H=4.15%, N=11.74% found: C=63.74%, H=3.79%, N=11.77%.
EXAMPLE 149
Benzaldehyde, O-[[[4-[(2-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using workup method C provided the title compound as white solid in 76% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.42 (s, 1H), 8.27 (dd, J=5.05 Hz, J=1.55 Hz, 1H), 8.17 (br, 1H), 7.76 (td, J=8.65 Hz, J=1.95 Hz, 1H,), 7.72 (d, J=7.05 Hz, 2H), 7.58 (d, J=8.85 Hz, 2H), 7.53 (tt, J=7.25 Hz, J=1.35 Hz, 1H), 7.48 (t, J=6.25 Hz, 2H), 7.15 (dt, J=8.85 Hz, J=3.2 Hz, 2H), 7.07 (dd, J=5.6 Hz, J=6.5 Hz, 1H), 6.89 (d, J=8.35 Hz, 1H); 13 C NMR (CDCl 3 , 500 MHz) δ 163.5, 153.9, 152.0, 150.2, 146.7, 140.7, 134.0, 132.0, 129.7, 129.1, 128.2, 121.9, 121.4, 118.7, 111.3; Mass spec.: 334.27 (MH + ). Anal. Calcd. for C 19 H 15 N 3 O 3 .0.185H 2 O: C=67.78%, H=4.60%, N=12.48%; found: C=67.79%, H=4.29%, N=12.55%.
EXAMPLE 150
4-Fluorobenzaldehyde, O-[[[4-[(3-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using workup method B provided the title compound as white solid in 93.5% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.39 (s, 1H), 8.38 (d, J=12.5 Hz, 2H), 8.08 (br, 1H), 7.75-7.72 (m, 2H), 7.54 (d, J=8.8 Hz, 2H), 7.34-7.29 (m, 2H), 7.19-7.15 (t, J=8.45 Hz, 2H), 7.05 (d, J=8.8 Hz, 2H); Mass spec.: 352.09 (MH + ). Anal. Calcd. for C 19 H 14 FN 3 O 3 .1.38H 2 O: C=60.66%, H=4.49%, N=11.17%; found: C=60.62%, H=4.24%, N=11.30%.
EXAMPLE 151
Benzaldehyde, O-[[[4-[(3-pyridinyl)oxy]phenyl]amino]carbonyl]oxime (Scheme 4, Compound L) This material was prepared by the general method where R=4-(3-pyridoxy)benzoic acid, R′=benzaldehyde oxime. Using workup method C and then B provided the title compound as white solid in 7% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.43 (s, 1H), 8.38 (d, J=20.0 Hz, 2H), 8.17 (br, 1H), 7.12 (d, J=7.0 Hz, 2H), 7.56-7.46 (m, 5H), 7.32 (m, 2H), 7.05 (d, J=6.9 Hz, 2H); Mass spec.: 334.12 (MH + ). Anal. Calcd. for C 19 H 15 N 3 O 3 .0.21H 2 O: C=67.69%, H=4.61%, N=12.46%; found: C=67.75%, H=4.81%, N=12.22%.
EXAMPLE 152
3-Pyridinecarboxaldehyde, O-[[(2-dibenzofuranyl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method A provided the title compound as white solid in 25% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.94 (br, 1H), 8.77 (d, J=3.0 Hz, 1H), 8.49 (s, 1H), 8.25 (s, 1H), 8.14 (d, J=6.75 Hz, 1H), 8.09 (br, 1H), 7.97 (d, J=7.6 Hz, 1H), 7.57 (t, J=7.3 Hz, 2H), 7.50-7.46 (m, 3H), 7.36 (t, J=7.8 Hz, 1H); Mass spec.: 332.24 (MH + ). Anal. Calcd. for C 19 H 13 N 3 O 3 0.19H 2 O: C=68.19%, H=4.03%, N=12.56%; found: C=68.18%, H=3.99%, N=12.49.
EXAMPLE 153
4-Fluorobenzaldehyde, O-[[(2-dibenzofuranyl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using workup method C provided the title compound as white solid in 8% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.43 (s, 1H), 8.25 (s, 1H), 8.20 (br, 1H), 7.97 (dd, J=7.7 Hz, J=0.45 Hz, 1H), 7.76 (m, 2H), 7.56 (t, J=9.75 Hz, 2H), 7.48 (t, J=7.3 Hz, 2H), 7.35 (t, J=7.5 Hz, 1H), 7.19 (t, J=8.65 Hz, 2H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.9, 152.7, 152.3, 130.4, 130.3, 127,5, 122.8, 120.9, 116.5, 116.4, 111.9, 111.7; Mass spec.: 349.10 (MH + ). Anal. Calcd. for C 20 H 13 FN 2 O 3 : C=68.96%, H=3.76%, N=8.04%; found: C=68.82%, H=3.77%, N=7.77%.
EXAMPLE 154
Benzaldehyde, O-[[(2-dibenzofuranyl)amino]carbonyl]oxime (Scheme 4, Compound L) Prepared as described above. Using work-up method C provided the title compound as white solid in 21% yield. 1 H NMR (CDCl 3 , 500 MHz) δ 8.46 (s, 1H), (8.29 (br, 1H), 8.26 (d, J=1.95 Hz, 1H), 7.97 (d, J=7.5 Hz, 1H), 7.75 (dd, J=8.5 Hz, J=1.5 Hz, 2H), 7.58-7.46 (m, 7H), 7.36 (t, J=7.7 Hz, J=1H); 13 C NMR (CDCl 3 , 500 MHz) δ 156.9, 153.8, 153.2, 152.4, 132.1, 132.0, 129.7, 129.1, 128.3, 127.5, 124.9, 124.1, 122.8, 121.0, 120.0, 112.6, 111.9, 111.8; Mass spec.: 331.12 (MH + ). Anal. Calcd. for C 20 H 14 N 2 O 3 .0.135H 2 O: C=72.19%, H=4.07%, N=8.42%; found: C=72.20%, H=4.07%, N=8.33.
EXAMPLE 155
(1Z)-N-[[[(4-butoxyphenyl)amino]carbonyl]oxy]ethanimidoyl chloride This compound was synthesized in accordance with the following literature references: Ivanov, Y. et al., Anticholinesterase activity of O-carbamoylated acylhydroxymoyl chlorides, Khim - Farm Zh., 26:5, 62-63,1992; and Sakamoto, T. et al., A new synthesis of nitriles from N-alkoxyimidoyl halides with zinc, Synthesis, 9: 750-752, 1991.
Biological Data:
Homogenates of crude membranes were prepared from H4 cells that express transfected human FAAH (H4-FAAH cells). Briefly, cells were grown in DMEM supplemented with 10% FBS and Geneticin at a final concentration of 500 μg/ml (Gibco BRL, Rockville, Md.). Confluent cultures of H4-FAAH cells were rinsed twice with phosphate-buffered saline [138 mM NaCl, 4.1 mM KCl, 5.1 mM Na 2 PO 4 , 1.5 mM KH 2 PO 4 (pH 7.5), 37° C.] and incubated for 5 to 10 minutes at 4° C. in lysis buffer [1 mM sodium bicarbonate]. Cells were transferred from plates to polypropylene tubes (16×100 mm), homogenized and centrifuged at 32,000×g for 30 minutes. Pellets were resuspended by homogenization in lysis buffer and centrifuged at 32,000×g for 30 minutes. Pellets were resuspended in lysis buffer (15-20 μg protein/ml) then stored at −80° C. until needed. On the day of an experiment, membranes were diluted to 2.67 μg protein/ml in 125 mM Tris-Cl, pH 9.0.
Activity of FAAH was measured using a modification of the method described by Omeir et al., 1995 (Life Sci 56:1999, 1995). Membrane homogenates (240 ng protein) were incubated at room temperature for one hour with 1.67 nM anandamide [ethanolamine 1- 3 H] (available from American Radiolabeled Chemical Inc., St Louis, Mo.) and 10 μM anandamide (available from Sigma/RBI, St. Louis, Mo.) in the absence and presence of inhibitors. The reaction was stopped by the addition of 1 volume of a solution of 1:1 methanol and dichloroethane. The mixture was shaken and then centrifuged at 1000×g for 15 minutes to separate the aqueous and organic phases. An aliquot of the aqueous phase, containing [ 3 H]-ethanolamine was withdrawn and counted by scintillation spectroscopy. Data were expressed as the percentage of [ 3 H]-ethanolamine formed versus vehicle, after subtraction of the background radioactivity determined in the presence of 10 μM arachidonyl trifluoromethyl ketone (ATFMK), an inhibitor of FAAH. IC 50 values were determined using a four-parameter logistic equation for dose-response curves. Compounds for which IC 50 values are not provided herein showed no FAAH inhibition or marginal FAAH inhibition in preliminary tests.
TABLE I
Ex. No.
IC 50 (nM)
1
++++
2
++++
3
++++
4
++++
5
++++
6
++
7
++
8
+++
9
+++
10
++++
11
++++
12
+++
13
+++
14
++++
15
++
16
+++
17
++++
18
+
19
++
20
++
21
+
22
+++
23
++++
24
++++
25
++++
26
++++
27
++++
28
++++
29
++++
30
++++
31
++++
32
++++
33
++++
34
++++
35
++++
36
++++
37
++++
38
++++
39
++++
40
++++
41
++++
42
++++
43
++++
44
+++
45
++++
46
++++
47
++++
48
++++
49
++++
50
++++
51
++++
52
++++
53
++++
54
++++
55
++++
56
++++
57
++++
58
+
59
++++
60
+++
61
+
62
+++
63
+++
64
+++
65
+++
66
+
67
+++
68
+++
69
+++
70
+++
71
++++
72
+++
73
+++
74
++++
75
++++
76
++++
77
++++
78
++++
79
++++
80
++++
81
++++
82
++++
83
++++
84
++++
85
++++
86
++++
87
++++
88
++++
89
+
90
+++
91
++++
92
+
93
+++
94
+
95
+
96
++++
97
+++
98
++++
99
+++
100
+++
101
++++
102
++++
103
++++
104
+++
105
++++
106
+++
107
++
108
++
109
+
110
+
111
++++
112
++++
113
++++
114
++++
115
+++
116
+++
117
+++
118
+++
119
+++
120
++++
121
++++
122
+++
123
+
124
+
125
+++
126
+++
127
++
128
+++
129
++
130
+++
131
+++
132
+++
133
+++
134
+++
135
++++
136
+++
137
+++
138
+++
139
++++
140
+++
141
+
142
+
143
+
144
+
145
+
146
++
147
++
148
+++
149
+++
150
++++
151
++++
152
++
153
+++
154
+++
155
++++
++++ = <10 nM;
+++ = ≧10-100 nM;
++ = ≧101-500 nM;
+ = >500 nM
The following in vivo pain models below utilized Example 5. CARRAGEENAN-INDUCED THERMAL HYPERALGESIA (Chronic Inflammatory Pain): Example 5 (40 mg/kg, i.p.) suppressed the development of thermal hyperalgesia induced by paw carrageenan. Paw carrageenan injection (⋄, 0:45 hr, Carr) produced strong thermal hyperalgesia as evidenced by the short escape latencies seen in vehicle treated rats (⋄, 2:15 hr, Carr) as compared to the long baseline latencies (0:00 hr). Animals pretreated with Example 5 (#1, 0:15 hr) failed to exhibit hyperalgesic responses (compare ⋄ to ▪ at 2:15 hr) and instead the latencies for drug treated animals were comparable to baseline. By 120 min post-carrageenan (2:45 hr), partial development of hyperalgesia was observed, that was reversed by a second injection of Example 5 (#2, 3:00 hr) which maintained thermal escape responses at basal levels for another hour (3:00-4:00 hr). No side effects were observed at 40 mg/kg, i.p. in drug (▪) or vehicle (⋄) treated controls (CEW=Cremophor:Ethanol:Water 10:10:80, 2 ml/kg). Data are mean+/−s.e.m. (n=8 per group). *p<0.05, **p<0.01 Tukey's HSD, compared to vehicle. The results are shown in FIG. 1 .
HARGREAVES TEST (Acute Thermal Pain) Example 5 (10 & 30 mg/kg; 2 ml/kg; i.v. hand infusion) produced a significant reversal of acute thermal pain behavior at 15 min post injection, which did not persist beyond this time. No significant side effects were observed at 10 mg/kg. However, at 30 mg/kg side effects included strong sedation, reduced activity and splayed hindlimbs. Data are mean+/−s.e.m. (n=8 per group). **p<0.01 Dunnett's Test, compared to vehicle control. The results are shown in FIG. 2 .
PAW EDEMA MODEL (Inflammation-induced Edema) The effects of Example 5 on carrageenan-induced edema were examined in a quantitative manner (plethysmometry). Injections of carrageenan (2% lambda) into the plantar aspect of both hind paws, resulted in an increase in combined total paw volume (swelling) measured 3 hours post-injection. Example 5 inhibited swelling by 26% at 40 mg/kg (Ex. 5-40, ip administered at −30 min and +2 hr relative to carrageenan) but showed no efficacy at 20 mg/kg (Ex. 5-20, ip). The reference agent dexamethasone (Dex, 1 mg/kg, ip) inhibited swelling by 70%. FIG. 3 summarizes the data. | The present invention relates to novel oxime carbamyl derivatives and pharmaceutical compositions comprising said derivatives which inhibit fatty acid amide hydrolase. These pharmaceutical compositions are useful for the treatment of conditions which can be effected by inhibiting fatty acid amide hydrolase including, but not limited to, neuropathic pain, emesis, anxiety, altering feeding behaviors, movement disorders, glaucoma, brain injury, and cardiovascular disease. | 2 |
BACKGROUND
[0001] In a computing environment, one may wish to automate functional steps of an application, for example, for functional testing or user interaction automation in an application. As an example, in a web-based application, one may wish to test results of changes to a web page by recreating typical user interactions on that page after the changes have been made. In this example, it may be desirable to record events that resulting from actions upon the web page during the user interaction. Recording the events yields an ability to playback the user actions on a web page during a functional test for the web-based application.
SUMMARY
[0002] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key factors or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
[0003] In computing environments, functional testing and user interface (UI) application automation is a process by which functional steps of an application are recreated from previously performed user actions or actions imitated for functional testing or process automation. The purpose of recreating these steps is to recreate all performance of intended actions on a target application without user interaction. In order to accomplish this task, the functional steps of an application need to be recorded, along with all relevant events that may occur as a result of performing the steps in the application. Therefore, to faithfully recreate original user intent when interacting with an application, a recording of the user's action may be performed, followed by performing those actions upon the application using a playback. However, current techniques may not effectively record the user's intent, are typically resource intensive, and may not provide effective functionality.
[0004] As provided herein, a technique and system for reliable and efficient recording of functional steps in an application, allow for reliable and efficient playback of the functional steps. The technique and system use instruction (e.g., JavaScript code) injection to apply wrapper functions to event handlers and elements in an application, as necessary, to monitor a state of an event generator before and after actions have be called upon the event generator. In this way, properties of the event generator may be recorded for use by a playback engine, or the properties may be processed to determine a user's intent when performing an action upon the event generator.
[0005] For example, if a user clicks on an item on a web page, then intent of that click may not be able to be determined by current techniques. However, the technique and system, provided herein, may be able to determine whether the user intended to select the item, deselect the item, or simply clicked the item for another intent (e.g., to edit or copy the item). To facilitate, at least some of, the same, when a page loads event handler monitoring wrappers are injected into the page and event handlers on the page are associated with the monitoring wrappers. When an event is called upon an element attached to the event handler, the monitoring wrapper function is called to record a state of the element prior to an event handler function being called. Once the event handler function has been called, the monitoring wrapper function is called again to record a state of the element. State sets of the element (e.g., sets of element properties) can be sent to a recording engine, or the state sets can be processed (e.g., compared) to determine user intent.
[0006] To the accomplishment of the foregoing and related ends, the following description and annexed drawings set forth certain illustrative aspects and implementations. These are indicative of but a few of the various ways in which one or more aspects may be employed. Other aspects, advantages, and novel features of the disclosure will become apparent from the following detailed description when considered in conjunction with the annexed drawings.
DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 is a flow diagram illustrating an exemplary method for recording an event set from a user interface by monitoring event handlers.
[0008] FIG. 2 is a flow diagram illustrating an exemplary method for recording an event set from a user interface with dynamic event handlers.
[0009] FIG. 3 is an illustration of a portion of an exemplary embodiment of a method for recording an event set from a user interface.
[0010] FIG. 4 is an illustration of a portion of an exemplary embodiment of a method for recording an event set from a user interface.
[0011] FIG. 5 is a block diagram illustration of exemplary system for recording an event set from a user interface by monitoring event handlers.
[0012] FIG. 6 is a block diagram illustration of a portion of an exemplary system for recording an event set from a user interface with dynamic event handlers.
[0013] FIG. 7 is a block diagram illustration of a portion of an exemplary system for recording an event set from a user interface with dynamic event handlers.
[0014] FIG. 8 is an illustration of an exemplary computer-readable medium comprising processor-executable instructions configured to embody one or more of the techniques provided herein.
[0015] FIG. 9 illustrates an exemplary computing environment wherein one or more of the provisions set forth herein may be implemented.
DETAILED DESCRIPTION
[0016] The claimed subject matter is now described with reference to the drawings, wherein like reference numerals are used to refer to like elements throughout. In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the claimed subject matter. It may be evident, however, that the claimed subject matter may be practiced without these specific details. In other instances, well-known structures and devices are shown in block diagram form in order to facilitate describing the claimed subject matter.
[0017] Embodiments described herein relate to techniques for recording actions in application interfaces (e.g., web-based applications, browser applications, user interfaces) by injecting wrapper functions into application instructions, and monitoring a state of an application interface element before and after an event is called upon the element.
[0018] In computing environments, to record actions in application interfaces based on external events, for example, the recorder should intercept the event and attempt to locate the element that is the target of the action. The process of looking for the element, in this example, involves inter process communication, which can be quite lengthy. Further, external observation of the event may not be useful for realizing “intent” of the action. As an example, a click on a list item may have “intent” to select, unselect, or change item to an editable state. Capturing “intent” may be possible by using an external application programming interface (API), but this technique often has a significant impact on computing resources (e.g., performance). For example, in the Windows® operating system (OS), there is a default time limit of 500 ms for how long an event can be held before it must be allowed to proceed. While this limit can be changed, changing it may create undesired effects in the OS behavior. Further, this default limit is often hit when attempting to record from an external API provided by a browser.
[0019] An alternate technique for recording events from application interfaces involves injecting instructions (e.g., JavaScript code) for event handler wrapper functions into the application interface. When called, the wrapper function collects and processes a set of current state information (e.g., relevant properties) of an event generator (e.g., an element) receiving the event call. The wrapper function then calls an event handler function on the element, then again collects and processes a set of current state information of the event generator. Both sets of information (e.g., properties of the element before the event handler function and properties after) can be sent to a recording engine, or processed (e.g., determining intent of an action by comparing the sets of element states). By employing wrappers around respective event handlers for an event generator (e.g., an element), one can examine information on the state of the event generator (e.g., element properties) before and after an action was taken upon the event generator (e.g., clicking on an element). Further, by using this technique, more than one set of information may be recorded at one time for a given event generator. Therefore, a playback engine may search a list of information sets (e.g., property sets) for the element in order to produce a more accurate playback experience.
[0020] One embodiment of the technique described above is illustrated by an exemplary method 100 in FIG. 1 . Exemplary method 100 begins at 102 and involves injecting instructions, in an application interface, for wrapper monitoring functions at 104 ; one of which may be configured to record a first state of an event generator (e.g., an element), and one of which may be configured to record a second state of an event generator, compare the first state to the second state, and send event generator properties to a recording engine. At 106 , a first reference to a monitoring wrapper function is associated with an event handler. At 108 , a second reference to a monitoring wrapper function is associated with the event handler, at a position in the event handler's instructions subsequent to the first reference, with at least one set of instructions between the first reference and the second reference. Having associated the second reference, the method 100 ends at 110 .
[0021] As an example of this embodiment, one may record actions executed by a user on web page elements having dynamic properties. For example, as a web page is loaded, JavaScript code for one or more monitoring wrapper functions may be injected into the web page code. A first monitoring wrapper may be configured to record a set of properties of a state of an element, prior to an event handler function being called upon the element. A second monitoring wrapper may be configured to record the set of properties of the state of the element after the event handler function is called upon the element, and send both sets of properties of the element to a recording engine. Concurrently, a JavaScript code event handler wrapper, referencing the first and second monitoring wrapper functions, may be inserted in the page code for all event handlers on the page. This event handler wrapper wraps the event handler and includes the event handler function call at a point after a call to the first monitoring wrapper function. For example, the following html code line:
[0000] <td onclick=”appClickHandler”></td> becomes: <td onclick= ”clickWrapper(appClickHandler)” onkeydown= ”keyDownWrapper( )”...
Therefore, when an event handler is called (e.g., when an element is acted upon by an event), prior to the event handler function being called, the first monitoring wrapper is called by the event handler wrapper, which records the state of the element at that time. After the event handler function has proceeded, the second monitoring wrapper is called by the event handler wrapper, which records the state of the element at that time. The second monitoring wrapper then sends the property sets (e.g., before and after execution of the event handler function on the element) to the recording engine. Because the recording engine collects information on element's properties before and after event handler functions have been called upon the elements, a record of events initiated by the user on the web page may be recorded.
[0022] In one aspect, there are applications that programmatically attached event handlers (e.g., dynamic event handlers) to elements in response to actions taken in the application, a timer, or other code execution that invokes attachment. Problems may arise when attempting to record actions involving programmatically attached event handlers, such as, an application (e.g., a browser) may not allow for a list of these event handlers to be received (e.g., by a recording system), and these event handlers may be added after a page has loaded or other code has been executed. Therefore, attempting to wrap event handlers, as described above, may not account for programmatically attached event handlers. As such, in order to overcome possible problems additional steps may be included in the technique.
[0023] An embodiment of a technique to overcome problems described above is illustrated in FIG. 2 . In FIG. 2 an exemplary method 200 is devised to record events from applications interfaces by monitoring attachment of programmatically attached event handlers and creating wrappers for event handlers. The exemplary method 200 begins at 202 and involves replacing one or more references to event handler attaching and detaching function(s), found in respective elements (e.g., event generator) in an application interface page, with one or more references to one or more wrapper attach and detach functions at 204 . Instructions for the one or more wrapper functions for attaching and detaching event handlers are injected into page instructions at 206 . At 208 , when an event is invoked on an element, the wrapper attach function is called by the wrapper reference in the element. At 210 , the wrapper attach function uses an event handler wrapper generator to generate a monitoring wrapper function for an event handler. Once the one or more monitoring wrapper functions are generated, event handler functions are associated with a first reference and second reference (e.g., subsequent to the first) to the monitoring wrapper function at 212 . The event handler function reference and the monitoring wrapper function reference are stored at 214 . When an event is invoked on the element, the monitoring wrapper function records a first state of the element, prior to the event handler function being called at 216 . The event handler function is called at 218 , and second state of the element is recorded by the monitoring wrapper function at 220 . The property sets of the first state and second state are passed to a recording engine at 222 . Once the information is recorded, the stored references are used to activate the event handler detach function for an element at 224 , where a wrapper detach function finds the stored event handler function reference. Detachment of the event handler occurs at 226 . Having completed the event handler detachment, the exemplary method 200 ends at 228 .
[0024] It is to be appreciated that there is not necessarily an attach/detach handler per every event invocation. Rather, event handlers are attached and detached as necessary, generally at the beginning of page loading and/or upon completion of certain conditions. To effectively detect such programmatically added handlers, references to one or more wrapper attach and detach functions are substituted for references to event handler attaching and detaching function very early on. Should an event handler be attached, arriving events can be readily diverted since the attach method itself is “hijacked”, and so had a chance to make the aforementioned wrapper for handler substitution. Essentially, attach and detach methods for respective elements are substituted or “hijacked” (as early as possible), an application decides whether to attach or detach event handlers (e.g., whenever the application wants to monitor events, where timing of such monitoring is generally unknown), and events then arrive at the wrapper if an event handler was attached.
[0025] As an example, one embodiment of the exemplary method 200 in FIG. 2 is illustrated in FIGS. 3 and 4 . In FIG. 3 , the method 302 acts upon an exemplary web page 304 as the page loads all its elements 306 . When the web page finishes loading 308 a wrapper attach function 310 and a wrapper detach function 312 have been injected into the web page code. Further, references to the wrapper attach function 314 and the wrapper detach function 316 have been inserted in each of the elements 318 on the loaded web page 308 , in place of references that pointed to the original registration and deregistration functions for each element 318 .
[0026] In FIG. 4 a user 402 acts upon an element 406 in a web page 404 (e.g., by clicking on the element), which calls for dynamically attaching an event handler 420 . A wrapper attach function reference 408 in the element 406 calls to a wrapper attach function 412 in the web page's code, which initiates a method 416 . The method 416 collects a set of properties of the element 406 in the web page 404 prior to the event handler 420 acting upon the element 406 . Further, the method 416 initiates the dynamically attached event handler 420 that is called when the user 402 clicked on the element 406 in the web page 404 . The event handler 420 acts upon the web page 404 , as it would have without the method 416 . When the event handler 420 has completed its function on the web page 404 , the method 416 again collects a set of properties of the element 406 in the web page 404 . The collected sets of properties of the element 406 are sent to a recording engine 424 . The method 416 calls back to the wrapper detach function reference 410 in the element 406 , which calls to the wrapper detach function 414 in the web page 404 . The wrapper detach function 414 activates the event handler detach function 422 , dynamically detaching the event handler 420 from the element 406 .
[0027] In another aspect, some elements in an application interface may be created dynamically, for example, by invoking document object model (DOM) methods to create and add elements to a browser page. In this example, creation of an element is a DOM method, whereas adding created elements is either a method of the page or a method of an element to which elements are added as children. Both the addition of an element as a method of a page and the addition of an element as a method of an element to which elements are added as children can be “wrapped” by having a wrapper function perform all actions performed on preexisting elements in an application interface. In this aspect, instructions for wrappers are injected around event handlers that are placed as attributes on created elements. Further, as described above, event handler attach and detach wrapper functions are injected for respective newly created and/or newly attached elements. Also, attach element wrapper function instructions are injected around an attach element method of respective elements, such that children added to the element may also be wrapped, as described above.
[0028] Therefore, as an example, a user's action on a web browser page may call a DOM method “createElement” and add a newly created element to the web page. In this example, as described in method 200 above, wrapper attach and detach event handler functions are injected into the page code for the newly created and added element, and event handlers attached to the newly added element are wrapped with wrapper monitoring functions. Further, an attach element function for the newly added element is wrapped with a wrapper function that creates wrappers for any newly added children of the element. As in method 200 , the newly added element from the user's action on the web page may be monitored during respective actions upon the element, and its properties may be sent to a recording engine. In this example, when a tester wishes to perform functional testing of the user's action upon the web page, an automated playback of the user's actions will include creating and adding an element to the web page, and any other actions that the user may have performed upon the newly added element.
[0029] In yet another aspect, a mouse over is an action of passing a mouse cursor over an element. Some application interfaces (e.g., dynamic web pages) may use this action to activate additional functionality (e.g., activating menus not previously visible when a mouse cursor passes over an element on a browser page). Because a mouse over is not visible as an event outside of the DOM, a problem may arise when attempting to record a mouse hover. At levels outside of the DOM the only action indicating a mouse over is an act of moving a mouse. Currently, there may be several solutions for recording a mouse over event. One solution may be to record all mouse movements; however, system performance is negatively affected and playback failure invariably occurs in some situations. Another solution may be to record all mouse moves in correlation with underlying elements; however, while failure during playback is less likely, system resources are taxed even more than the previous solution. Yet another solution may be to perform a lookup of an element's bounding rectangle each time there is a given mouse position change, and ignore further movements if they occur within the rectangle; however, while system performance is better than the previous solutions, one must still record many mouse movements, which is more likely to lead to playback failure and decreased system performance.
[0030] In this aspect, an alternate technique for recording mouse over events in an application interface is to use the methods, described herein, for injecting wrapper functions, wrapping event handlers and monitoring an element's properties. Further, this method can account for elements that do not activate an event when a mouse over occurs, by ignoring such actions. As an example, during wrapping of registered event handlers, if an element does not have an attached event handler for a mouse event, this element can be ignored during recording. However, if the element does have an attached event handler for mouse motion events, the wrapping method, described herein, can monitor and record the event as a mouse over event on the element, as described above. Further, if the mouse over action results in a change to the element's layout, its properties are recorded using the method herein. As an example, when wrapping event handlers for mouse over events injected wrapper functions (e.g., programming code instructions) may be executed before an action is taken by an element for an event, and after all actions are executed by the element. In this example, a wrapper function (e.g., a mouseenter wrapper) is injected at the element level as an event is first detected at this level, then injecting a wrapper function (e.g., a mouseexit wrapper) at the document level. In this example, the mouse movements and actions that occur as a result of a mouse over can be recorded.
[0031] In yet another aspect, element selection/deselection may be an action, for example, upon an element in a list, table, or on an application page. A problem with state of the art solutions for recording such an event is that intent of a click upon an element cannot be determined. For example, clicking on an element may be an action selecting the item, deselecting the item, or no action other than a click. Therefore, proper functional playback of such a recorded event may be affected. However, in this aspect, one may use the method for injecting wrapper functions, wrapping event handlers and monitoring an element's properties, described herein, to record element selection/deselection events in an application interface.
[0032] In this aspect, as an example, by wrapping all event handlers by injecting instructions (e.g., JavaScript code), including selection handlers (e.g., onchange event) and mouse event handlers (e.g., onclick event), effective recording of element selection/deselection events may occur. As a result, a “click” on an element may be intercepted before propagating it to the element. Further, the element's properties may be checked to determine whether it supports “selection.” After the “click” event proceeds, properties of the element are again recorded, capturing the intent of the “click” action. Once properties of the element prior to the “click” and after the “click” are captured, the intent of the “click” can be determined and recorded.
[0033] A system may be configured to record events from web-based applications or user interfaces by registering event handlers with references to wrappers and creating wrappers for event handlers, such as illustrated by an exemplary system 500 in FIG. 5 . The exemplary system 500 has an event handler registerer 502 that injects an event handler wrapper function 506 and replaces an event handler function reference 510 in an event handler 508 with a wrapper function reference 504 . When an event 518 is invoked upon an element 514 , the element calls to the registered event handler 508 , which calls to the wrapper function 506 via the wrapper function reference 504 now in place in the event handler 508 . The wrapper function 506 collects and sends information 520 associated with the event to the recording engine 516 . After the information 520 is collected and sent, the wrapper function 506 calls to the original event handler function 512 , which performs its functions upon the element 514 .
[0034] FIGS. 6 and 7 illustrate one embodiment of exemplary systems 600 and 700 for recording events from web-based applications or user interfaces by monitoring registration of event handlers and creating wrappers for event handlers. As illustrated in FIG. 6 , a code injector 602 creates a wrapper attach event handler function for 604 and a wrapper detach event handler function 606 . The code injector 602 also replaces an event handler attach function reference 608 and an event handler detach function reference 610 in an element (e.g., event generator) 612 , with a reference to a wrapper attach function 614 and a reference to a wrapper detach function 616 .
[0035] In FIG. 7 when an event 702 is invoked on an element 704 the reference to the wrapper attach function 706 calls to the wrapper attach function 710 . An event handler monitoring wrapper function generator 712 creates and injects an event handler monitoring wrapper function 724 , injects a reference to an event handler monitoring wrapper function 718 in an event handler 720 at a 1 st location 722 and at a 2 nd location 732 , and sends both the reference to an event handler monitoring wrapper function 718 and the reference to the event handler function 726 to a reference storer 714 . The event handler monitoring wrapper function 724 records a 1 st state of the element 704 , prior to an event handler function being called upon it. The event handler monitoring wrapper function 724 calls to the event handler 720 to invoke the event function 726 upon the element 704 . A 2 nd monitoring wrapper function reference 724 calls to the monitoring wrapper function 724 , which records a 2 nd state of the element 704 . The monitoring wrapper function 724 sends a 1 st and 2 nd state of the element 704 as event information 730 to a recording engine 728 . The event handler function 726 calls back to the element 704 for deregistration of the event handler 720 . The reference to a wrapper detach function 708 calls to a wrapper detach function 716 , which calls to the reference storer 714 to retrieve the reference to event handler function 726 stored there. The wrapper detach function 716 calls to the event handler 720 to deregister from the element 704 .
[0036] Another embodiment (which may include one or more of the variations described above) involves a computer-readable medium comprising processor-executable instructions configured to apply one or more of the techniques presented herein. An exemplary computer-readable medium that may be devised in these ways is illustrated in FIG. 8 , wherein the implementation 800 comprises a computer-readable medium 808 (e.g., a CD-R, DVD-R, or a platter of a hard disk drive), on which is encoded computer-readable data 806 . This computer-readable data 806 in turn comprises a set of computer instructions 804 configured to operate according to the principles set forth herein. In one such embodiment, the processor-executable instructions 804 may be configured to perform a method 802 for recording events from user interfaces by registering event handlers with references to wrappers and creating wrappers for event handlers, such as the method 100 of FIG. 1 , for example. Many such computer-readable media may be devised by those of ordinary skill in the art that are configured to operate in accordance with the techniques presented herein.
[0037] Although the subject matter has been described in language specific to structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as example forms of implementing the claims.
[0038] As used in this application, the terms “component,” “module,” “system”, “interface”, and the like are generally intended to refer to a computer-related entity, either hardware, a combination of hardware and software, software, or software in execution. For example, a component may be, but is not limited to being, a process running on a processor, a processor, an object, an executable, a thread of execution, a program, and/or a computer. By way of illustration, both an application running on a controller and the controller can be a component. One or more components may reside within a process and/or thread of execution and a component may be localized on one computer and/or distributed between two or more computers.
[0039] Furthermore, the claimed subject matter may be implemented as a method, apparatus, or article of manufacture using standard programming and/or engineering techniques to produce software, firmware, hardware, or any combination thereof to control a computer to implement the disclosed subject matter. The term “article of manufacture” as used herein is intended to encompass a computer program accessible from any computer-readable device, carrier, or media. Of course, those skilled in the art will recognize many modifications may be made to this configuration without departing from the scope or spirit of the claimed subject matter.
[0040] FIG. 9 and the following discussion provide a brief, general description of a suitable computing environment to implement embodiments of one or more of the provisions set forth herein. The operating environment of FIG. 9 is only one example of a suitable operating environment and is not intended to suggest any limitation as to the scope of use or functionality of the operating environment. Example computing devices include, but are not limited to, personal computers, server computers, hand-held or laptop devices, mobile devices (such as mobile phones, Personal Digital Assistants (PDAs), media players, and the like), multiprocessor systems, consumer electronics, mini computers, mainframe computers, distributed computing environments that include any of the above systems or devices, and the like.
[0041] Although not required, embodiments are described in the general context of “computer readable instructions” being executed by one or more computing devices. Computer readable instructions may be distributed via computer readable media (discussed below). Computer readable instructions may be implemented as program modules, such as functions, objects, Application Programming Interfaces (APIs), data structures, and the like, that perform particular tasks or implement particular abstract data types. Typically, the functionality of the computer readable instructions may be combined or distributed as desired in various environments.
[0042] FIG. 9 illustrates an example of a system 910 comprising a computing device 912 configured to implement one or more embodiments provided herein. In one configuration, computing device 912 includes at least one processing unit 916 and memory 918 . Depending on the exact configuration and type of computing device, memory 918 may be volatile (such as RAM, for example), non-volatile (such as ROM, flash memory, etc., for example) or some combination of the two. This configuration is illustrated in FIG. 9 by dashed line 914 .
[0043] In other embodiments, device 912 may include additional features and/or functionality. For example, device 912 may also include additional storage (e.g., removable and/or non-removable) including, but not limited to, magnetic storage, optical storage, and the like. Such additional storage is illustrated in FIG. 9 by storage 920 . In one embodiment, computer readable instructions to implement one or more embodiments provided herein may be in storage 920 . Storage 920 may also store other computer readable instructions to implement an operating system, an application program, and the like. Computer readable instructions may be loaded in memory 918 for execution by processing unit 916 , for example.
[0044] The term “computer readable media” as used herein includes computer storage media. Computer storage media includes volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions or other data. Memory 918 and storage 920 are examples of computer storage media. Computer storage media includes, but is not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, Digital Versatile Disks (DVDs) or other optical storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can be accessed by device 912 . Any such computer storage media may be part of device 912 .
[0045] Device 912 may also include communication connection(s) 926 that allows device 912 to communicate with other devices. Communication connection(s) 926 may include, but is not limited to, a modem, a Network Interface Card (NIC), an integrated network interface, a radio frequency transmitter/receiver, an infrared port, a USB connection, or other interfaces for connecting computing device 912 to other computing devices. Communication connection(s) 926 may include a wired connection or a wireless connection. Communication connection(s) 926 may transmit and/or receive communication media.
[0046] The term “computer readable media” may include communication media. Communication media typically embodies computer readable instructions or other data in a “modulated data signal” such as a carrier wave or other transport mechanism and includes any information delivery media. The term “modulated data signal” may include a signal that has one or more of its characteristics set or changed in such a manner as to encode information in the signal.
[0047] Device 912 may include input device(s) 924 such as keyboard, mouse, pen, voice input device, touch input device, infrared cameras, video input devices, and/or any other input device. Output device(s) 922 such as one or more displays, speakers, printers, and/or any other output device may also be included in device 912 . Input device(s) 924 and output device(s) 922 may be connected to device 912 via a wired connection, wireless connection, or any combination thereof. In one embodiment, an input device or an output device from another computing device may be used as input device(s) 924 or output device(s) 922 for computing device 912 .
[0048] Components of computing device 912 may be connected by various interconnects, such as a bus. Such interconnects may include a Peripheral Component Interconnect (PCI), such as PCI Express, a Universal Serial Bus (USB), firewire (IEEE 8394), an optical bus structure, and the like. In another embodiment, components of computing device 912 may be interconnected by a network. For example, memory 918 may be comprised of multiple physical memory units located in different physical locations interconnected by a network.
[0049] Those skilled in the art will realize that storage devices utilized to store computer readable instructions may be distributed across a network. For example, a computing device 930 accessible via network 928 may store computer readable instructions to implement one or more embodiments provided herein. Computing device 912 may access computing device 930 and download a part or all of the computer readable instructions for execution. Alternatively, computing device 912 may download pieces of the computer readable instructions, as needed, or some instructions may be executed at computing device 912 and some at computing device 930 .
[0050] Various operations of embodiments are provided herein. In one embodiment, one or more of the operations described may constitute computer readable instructions stored on one or more computer readable media, which if executed by a computing device, will cause the computing device to perform the operations described. The order in which some or all of the operations are described should not be construed as to imply that these operations are necessarily order dependent. Alternative ordering will be appreciated by one skilled in the art having the benefit of this description. Further, it will be understood that not all operations are necessarily present in each embodiment provided herein.
[0051] Moreover, 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 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. In addition, the articles “a” and “an” as used in this application and the appended claims may generally be construed to mean “one or more” unless specified otherwise or clear from context to be directed to a singular form.
[0052] Also, although the disclosure has been shown and described with respect to one or more implementations, equivalent alterations and modifications will occur to others skilled in the art based upon a reading and understanding of this specification and the annexed drawings. The disclosure includes all such modifications and alterations and is limited only by the scope of the following claims. In particular regard to the various functions performed by the above described components (e.g., elements, resources, etc.), the terms used to describe such components are intended to correspond, unless otherwise indicated, to any component which performs the specified function of the described component (e.g., that is functionally equivalent), even though not structurally equivalent to the disclosed structure which performs the function in the herein illustrated exemplary implementations of the disclosure. In addition, while a particular feature of the disclosure may have been disclosed with respect to only one of several implementations, such feature may be combined with one or more other features of the other implementations as may be desired and advantageous for any given or particular application. Furthermore, to the extent that the terms “includes”, “having”, “has”, “with”, or variants thereof are used in either the detailed description or the claims, such terms are intended to be inclusive in a manner similar to the term “comprising.” | Recording of functional steps resulting from actions in an application is desirable for performing functional testing or user interface automation of an application. However, certain events that may result from actions occurring in an application are often difficult to record, which may lead to playback failure. Further, a user's intent when performing an action is difficult to determine. In order to obtain effective playback, a reliable and efficient recording of an application's functional steps needs to occur. Injecting wrapper functions into an application and monitoring an event generator's state before and after an action has occurred may yield more reliable and effective results. | 6 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to systems for producing one or more gases from a liquid compound by way of electrolysis. The present invention relates more specifically to a system for generating pressurized gases from polar molecular liquids. The system anticipates its preferred use in conjunction with liquid water, although other polar molecular liquids may be used to produce other gases based upon the same principles.
[0003] 2. Description of the Related Art
[0004] Electrolysis involving water is the decomposition of water ( ) into oxygen gas ( ) and hydrogen gas ( ) as the result of the establishment of an electric potential that results in the flow of an electric current through the water. The principle behind electrolysis involves reactions that occur on two electrodes placed within the water. In the basic arrangement, an electrical power source is connected to the two electrodes, or two plates (typically made from some inert metal, such as platinum or stainless steel) which are placed in the water. Hydrogen gas ( ) bubbles will appear at the cathode (the negatively charged electrode where electrons enter the water) and oxygen gas ( ) bubbles will appear at the anode (the positively charged electrode). The amount of hydrogen gas generated is typically twice that of the amount of oxygen gas and both are proportional to the total electrical charge conducted by the solution.
[0005] Electrolysis of pure water requires excess energy to overcome various activation barriers. Without the excess energy, the electrolysis of pure water occurs very slowly or not at all. This is in part due to the limited self-ionization of water. Pure water has an electrical conductivity of about one millionth of that of sea water. Many electrolytic cells may also lack the requisite electrocatalyst. The efficiency of electrolysis is increased through the natural presence or the addition of an electrolyte (such as salt, an acid, or a base) and the use of an electrocatalyst. The present invention takes advantage of the greater concentration of naturally occurring electrolytes in deeper water.
[0006] In water, at the negatively charged cathode, a reduction reaction takes place with electrons from the cathode being given to hydrogen cations to form hydrogen gas. At the positively charged anode, an oxidation reaction occurs generating oxygen gas and giving electrons to the anode to complete the circuit. The overall reaction involves the decomposition of water into oxygen and hydrogen according to the following equation [=+]. The number of hydrogen molecules produced is therefore (on average) twice the number of oxygen molecules. Assuming equal temperature and pressure for both gases, the produced hydrogen gas therefore has twice the volume of the produced oxygen gas. The number of electrons pushed through the water is twice the number of generated hydrogen molecules and four times the number of generated oxygen molecules.
[0007] It would be desirable to utilize the above described principle of electrolysis to generate one or more gases from a liquid and to do so in a manner that produces the gases at an elevated pressure. It would be desirable if the ability to produce gases at an elevated pressure did not require the addition of significant amounts of energy to compress the gases once they have been produced. It would be useful to have a system that generated pressurized gas or gases in a manner that allowed for the storage of the gas or gases, or the immediate use of the gas or gases to release energy associated with either the pressure (through mechanical means) or with the chemical compounds (through chemical reaction means).
[0008] Efforts to produce usable gases through electrolysis, especially at elevated pressures, have generally met with little success. Most such systems require the use of complex and expensive equipment to pressurize the gas once it is produced. This process of compressing the gas once produced is energy intensive and generally makes the production of gases from the electrolysis of a liquid highly impractical. It would be desirable to have a system that made the production of pressurized gases from electrolysis a practical alternative to other known means for producing such gases.
SUMMARY OF THE INVENTION
[0009] The present invention therefore provides systems for generating and producing pressurized gases from polar molecular liquids without the need to compress the gases through the addition of outside mechanical force driven through the use of electrical energy or otherwise. The system of the present invention incorporates an electrolysis cell positioned at depth (16 feet or greater). The electrolysis cell includes a bell shaped enclosure defining a gas generating assembly that is positioned at depth within the polar molecular fluid, such as water. The gas generating assembly includes first and second electrodes positioned in spaced relationship and the bell shaped collection vessel arranged above the electrodes. The collection vessel or vessels include at least one gas port configured on an upward oriented closed end of the vessel from which may extend one or more gas conduits to carry the generated pressurized gas to the surface. At least one electrical conductor extends from a power source (a voltage potential source) at the surface down to the electrodes positioned within the gas generating assembly. Positioned at the surface are the necessary structural assemblies for deploying, supporting, and retracting a gas conduit bundle assembly and the attached gas generating assembly. In the preferred embodiment, at least one gas collection and storage tank is positioned at the surface to receive and store the produced pressurized gas. Positioning the gas generating assembly at depth immerses the electrodes within the polar molecular fluid, and operation of the electrical power supply effects an electrical potential between the electrodes resulting in an electrolytic breakdown of the polar molecular fluid into its constituent components. The gas components generated at a pressure above atmospheric pressure (dependent upon the depth) are then conducted up toward the surface and used below the water surface (bubbler, water pump) or brought to the surface and collected in one or more gas collection and storage tanks. The pressurized gas thus collected at the surface may be stored and used in a number of different applications at a later date or may be immediately used.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a cross sectional view of the electrode bell pressurized gas generator apparatus of the present invention.
[0011] FIG. 2 is a schematic block diagram of the overall system for generating pressurized gas of the present invention.
[0012] FIG. 3 is a partially schematic elevational view of a first implementation (first preferred embodiment) of the overall system of the pressurized gas generating system of the present invention (open water).
[0013] FIG. 4 is a partially schematic side plan view of the surface level components of the pressurized gas generating system of the present invention.
[0014] FIG. 5 is a detailed cross sectional view of the gas collection hose bundle of the first preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0015] Reference is made first to FIG. 1 for a detailed description of a partially schematic cross-sectional diagram of the basic apparatus of the present invention. The diagram shown in FIG. 1 is intended to describe the functionality of the system as well as its basic geometry and structure. Deep water electrolysis system 10 comprises a long outer tube 12 concentrically surrounding a long inner tube 14 . At the upper end of the electrolysis system 10 , outer tube 12 and inner tube 14 are terminated and partially closed by way of cap 16 . At the opposite end of outer tube 12 and inner tube 14 is positioned collection bell 18 . In a preferred embodiment, each of these components might be constructed of stainless steel pipe, PVC pipe, aluminum pipe, or the like.
[0016] Positioned within collection bell 18 are two dome-shaped wire mesh electrodes 20 and 22 . Electrode 20 comprises a dome-shaped screen having a central aperture 24 positioned at the peak of the dome. Electrode 22 comprises a dome-shaped screen smaller in diameter than electrode 20 and forming a complete dome or pyramid-shaped shell. Each of electrodes 20 and 22 includes a conductive ring 26 and 28 respectively, to which are electrically attached conductive wires 30 and 32 . These conductive wires 30 and 32 extend to the surface to a DC power source (not shown) oriented in the manner indicated in the figure. This configuration preferably establishes electrode 20 as the cathode (negatively charged electrode) on which are formed hydrogen molecules. Electrode 22 is thereby established as the anode (positive electrode) on which are formed the oxygen molecules.
[0017] As oxygen molecules are formed on the anode (electrode 22 ) the bubbles of oxygen gas collect below the screen (as far from the opposing electrode as possible) and migrate to the dome of the screen electrode where they pass through the screen, through central aperture 24 of electrode 20 , and are collected at the opening of inner tube 14 . Oxygen gas bubbles 36 then pass up through inner tube 14 to a point where the gas collects inside inner tube 14 at volume 40 . Oxygen gases may then be controllably conducted through valve 44 to the surface where the oxygen gas may be stored.
[0018] In a similar manner, hydrogen gas is generated on the cathode (negative electrode 20 ) where the bubbles pass over the screen of the electrode and are collected on the inside surface of bell 18 where they pass up into the circumferential structure of outer tube 12 . Hydrogen gas 38 then bubbles up through outer tube 12 into the enclosed volume 42 . Hydrogen gases then may be drawn out of the system through valve 46 as shown.
[0019] Because the electrolysis in the present system occurs at great depths in salt water (in the example shown), the efficiency of the reaction is higher than that as might occur at the surface. The gases thus generated also maintain the higher pressure established at depth in the salt water and will therefore arrive at the surface in either a greater volume or under higher pressure.
[0020] Reference is next made to FIG. 2 which is a schematic block diagram of the overall system of the present invention designed to generate pressurized gas for storage and use. The diagram in FIG. 2 is intended to represent the functional connections between the various components in the system and not the specific geometry or even arrangement of these components.
[0021] The entire system is preferably operated and controlled by data acquisition and control systems 50 which include various microprocessors, displays, and other analog and digital controllers that operate the electrical and gas flow components of the system. Data acquisition and control systems 50 are connected to the various other components within the system through electrical conductors and gas flow conduits. The vertically oriented components of the system are generally supported and maintained in position by support structure 52 . Below, or in conjunction with support structure 52 , are the necessary lifting and lowering mechanisms 58 . These various support structures are generally positioned at or near the surface of the water, or at a position of approximately one atmospheric pressure.
[0022] Also included at or near the surface are gas conditioning systems 62 described in more detail below, as well as the gas storage tanks, here indicated as gas tanks 54 and gas tanks 56 . Finally at the surface, power supply 60 is preferably positioned to direct the necessary voltage potential down to the electrolysis cell. It is possible, however, that the power supply necessary to generate the electrical potential across the electrodes in the electrolytical cell could also be positioned at depth. In general, however, it is more efficient and easier to simply direct electrical conductors down with the gas conduits to provide the necessary voltage potential across the electrodes.
[0023] The balance of the system shown in FIG. 2 is supported below the surface of the liquid (water) in a vertical column generally as indicated in an environment in excess of one atmosphere. The lifting/lowering mechanism 58 supports one or more gas conduits 66 as well as additional intermediate components that facilitate the transport of the pressurized gas to the surface. These intermediate components are generally identified as pressurized gas surge tank 64 , whose function is described in more detail below, as well as further gas conditioning systems 65 .
[0024] The gas conduits 66 extend to the surface from a pressurized gas column 68 which is positioned above, and in association with, the electrode bell enclosure 70 . Electrode bell enclosure 70 incorporates the two electrodes necessary to carry out the electrolytic reaction of the liquid compound. Power supply 60 is therefore electrically connected to electrode bell enclosure 70 as shown. A further optional component, inlet filtration system 72 may be positioned below electrode bell enclosure 70 so as to mediate the intrusion of debris and other material that might jeopardize the efficiency of the operation of the electrolytic cell.
[0025] Reference is next made to FIG. 3 for a broader view of a first implementation of the system of the present invention as might be made in conjunction with operation of the system in open water (an ocean, for example) at some significant depth. FIG. 3 is a partially schematic elevational view of a first implementation (first preferred embodiment) of the overall system of the pressurized gas generating components of the present invention. In this view, watercraft 80 is shown positioned at the surface of the water wherein the support collection and storage components of the system would be retained. Also positioned on watercraft 80 is deployment/take-up reel 82 . Extending from deployment/take-up reel 82 is one or more variations on a combination gas tube, wireline bundle, and support cable 84 . Positioned at an intermediate spot along combination gas tube and wireline bundle 84 is pressurized gas surge tank 86 . The function of this surge tank is also described in more detail below. The electrolysis gas generator 90 is positioned at the terminal of combination gas tube and wireline bundle 84 and may be held in place by one or more deployment anchors/weights 92 .
[0026] Those skilled in the art will recognize that operation of the system of the present invention involves the balancing of pressures between the gas generating assembly at depth and the surface level assemblies. To achieve the transport of a quantity of pressurized gas(es) to the surface there must be a flow of the gas(es), at least initially from a volume at higher pressure (at depth) to a volume at lower pressure (at the surface). In the initial phases of the process it may be necessary to establish a buffer or surge tank (such as surge tanks 86 in FIGS. 3 and 64 in FIG. 2 ) to help prevent the movement of liquid with the flow of gas up the gas conduits. Other methods for regulating the rate at which the gases are generated could also contribute to the mitigation of entrained fluids within the gas flows, especially on startup when the pressure differentials between the gas generating assembly at depth and the surface are greatest.
[0027] FIG. 3 is not intended to be drawn to scale, and the actual depth at which the electrolysis gas generator 90 would be positioned would more typically be on the order of 160′ to 320′ to over 5,000′. Operation of the system at such depths achieves the desired gas pressurization and yet does not incur material costs that exceed the benefits associated with collecting and storing the pressurized gases. It is preferable that electrolysis gas generator 90 not be positioned in close proximity to the ocean or lake bottom so as to avoid the induction of silt and debris into the system. Those skilled in the art will recognize that the “depth” referred to in the present invention is primarily a pressure differential established by a quantity of atmosphere and a quantity of water positioned above the gas generator assembly. This differential “depth” is determined by the distance between the gas generator assembly and the point of use and/or storage.
[0028] Reference is next made to FIG. 4 which is a partially schematic side plan view of the surface level components of the gas generating system of the present invention. In this view, various components are shown schematically placed and positioned around the movable gas collection hose bundle 128 that extends up from the gas generating cell described and shown above. The surface components are shown to include an array of surface level control and collection assemblies 100 . Centrally located among these components is control and data display instrumentation 102 which is connected to various other components within the system through control and data signal wires 136 . Also positioned at the surface is electric power supply 104 which, in the preferred embodiment, may simply be a rechargeable DC battery. Various alternate arrangements of the power supply system may include the use of an electrical ground located at depth.
[0029] Also included at the surface level are active first gas collection tank 106 and active second gas collection tank 108 . In addition to these active gas collection tanks, there are preferably reserve first gas storage tank(s) 110 and reserve second gas storage tank(s) 112 . Various tank valve and pressure gauge assemblies 114 are positioned on each of these tanks. In addition, a first gas flow dryer (entrained fluid removal) device 116 is associated with active first gas collection tank 106 and a second gas flow dryer (entrained fluid removal) 120 is associated with active second gas collection tank 108 . There is also a gas venting valve 118 associated with each side of the gas collection and storage system shown.
[0030] Extending from a collection manifold centrally positioned within the assembly of components at the surface is fixed gas collection hose bundle 122 . This length of multi conduit hose extends from the central manifold to a non-rotating axial position on hose bundle reel support and drive 126 . The reel support and drive 126 holds gas collection hose bundle 124 which is used to deploy and alternately to retract moveable gas collection hose bundle 128 .
[0031] Also positioned and utilized at the surface are grounded support platforms 130 and 132 . As indicated, the necessary control and data signal wires 136 extend from control and data display instrumentation 102 down into movable gas collection hose bundle 128 in a manner described in more detail below. Also incorporated into hose bundle 128 are electrical power supply wires 134 (shown as 30 and 32 in FIG. 1 ). Variations on the actual structure of the hose bundle are anticipated.
[0032] Additional and optional components represented by 138 and 140 , may be positioned at or near the water surface and may include bubble distribution systems, a combustion chamber with ancillary fuel supply, rapid compression or decompression chambers, or the like. These components may be connected through conduits 137 and 139 to active first gas collection tank 106 and active second gas collection tank 108 in a manner that allows for the immediate use of each or both the collected gases for purposes such as generating energy from combustion or otherwise operating systems that benefit from the pressurized condition of the gases, such as therapeutic uses of oxygen gases in pressure chambers or bubbling waters. Rapid decompression of the pressurized gases may be used in thermal exchange systems as well.
[0033] FIG. 5 is a detailed cross-sectional view of the gas collection hose bundle of the first preferred embodiment of the present invention shown generally as 128 in FIG. 4 and as 84 in FIG. 3 . A wide variety of different configurations for this hose bundle are anticipated and the components shown in FIG. 5 are intended to be inclusive of such components even though a more practical implementation may omit one or more of the components shown. Gas collection hose bundle 128 primarily incorporates first gas conduit lumen 150 and second gas conduit lumen 152 . In some applications of the present system, it may only be necessary to utilize a single gas conduit lumen collecting only one gas, and venting the other, or collecting both gases for immediate use when there is no concern for reverse electrolysis occurring. In the preferred embodiment, however, one where two gases are being generated and utilized separately at the surface, gas collection hose bundle 128 should incorporate at least two gas conduit lumens.
[0034] Also incorporated into hose bundle 128 is integrated support cable 154 which, in the preferred embodiment, may simply be a bundled wire cable that extends the length of hose bundle 128 and is utilized to relieve any weight forces on the gas conduit lumens. Further included in hose bundle 128 are electrical power supply wires 134 a and 134 b . In the preferred embodiment, these represent the DC positive and negative conductors that establish the electrical potential between the two electrodes associated with the electrolysis cell positioned at depth. Once again, however, an alternate embodiment wherein the ground electrical potential may be established at depth, a single conductor may provide the necessary positive potential (with respect to a negative ground) to one of the two electrodes while the remaining electrode is connected to ground.
[0035] Finally contained within the preferred embodiment of gas collection hose bundle 128 are control and data signal wire bundle 136 . In the preferred embodiment, this would be a coaxial signal cable that would allow for the multiplexing of data and/or the transmission of signal control data from the surface to the gas generating cell located at depth. Various mechanisms that might be incorporated into the electrolysis cell collection enclosure may be directed and controlled by way of this signal cable. In a like manner, various sensors that might be positioned at depth may direct signal data up to the surface for use in the control and data display instrumentation described above.
[0036] Although the present invention has been described in terms of the foregoing preferred embodiments, this description has been provided by way of explanation only, and is not intended to be construed as a limitation of the invention. Those skilled in the art will recognize modifications in the present invention that might accommodate specific “liquid at depth” environments. Such modifications as to structure, method, and even the specific arrangement of components, where such modifications are coincidental to the environment or the specific type of liquid compound being utilized, do not necessarily depart from the spirit and scope of the invention. Although the invention has been described in conjunction with what is essentially an “open water” environment, the principles involved may be just as easily applied to a “confined well” environment, where the depth is achieved by lowing the gas generating assembly to depth within a drilled well or the like. The same surface structural components may be utilized and the same basic “downhole” components would be utilized. In a like manner, the same hose bundle structures and geometries may be used. | A system for producing pressurized gas(es) from polar molecular liquids without the need to compress the gas(es) through outside mechanical forces or through the use of electrical energy or otherwise. The system incorporates an electrolysis cell positioned at depth (greater than 16 feet) within the liquid. The electrolysis cell includes a bell shaped enclosure defining a gas generating assembly that is positioned at depth within a fluid such as water. The gas generating assembly includes first and second electrodes positioned in spaced relationship and a bell shaped collection vessel arranged above the electrodes. At least one collection vessel includes at least one gas port configured to connect to gas conduits to carry the pressurized gas(es) to the point of use or storage. At least one electrical conductor extends from a power source to at least one of two electrodes positioned within the gas generating assembly. At least one gas collection and storage tank is preferably positioned at the surface to receive and store the produced pressurized gas. Positioning the gas generating assembly at depth immerses the electrodes within the polar molecular fluid, and operation of the electrical power supply establishes an electrical potential between the electrodes resulting in an electrolytic breakdown of the polar molecular fluid into its constituent components. The gas thus collected at the surface may be stored or used immediately in a number of different applications. | 8 |
BACKGROUND OF THE INVENTION
By virtue of its high level of crystallinity, trans-1,4-polybutadiene (TPBD) is a thermoplastic resin. Because it contains many double bonds in its polymeric backbone, TPBD can be blended and cocured with rubber. TPBD is similar to syndiotactic-1,2-polybutadiene in this respect. Even though the trans-1,4-polybutadiene of this invention is a thermoplastic resin, it becomes elastomeric when cured alone or when cocured with one or more rubbers.
Good molecular weight control can normally be achieved by utilizing an anionic polymerization system to produce TPBD. There is typically an inverse relationship between the catalyst level utilized and the molecular weight attained when anionic polymerization systems are used. Such an anionic polymerization system is disclosed in U.S. Pat. No. 4,225,690. The catalyst system disclosed therein is based on a dialkylmagnesium compound which is activated with a potassium alkoxide. However, such catalyst systems have not proven to be commercially successful.
TPBD is normally prepared utilizing transition metal catalysts or rare earth catalysts. The synthesis of TPBD with transition metal catalysts is described by J. Boor Jr., "Ziegler-Natta Catalysts and Polymerizations," Academic Press, New York, 1979, Chapters 5-6. The synthesis of TPBD with rare earth catalysts is described by D. K. Jenkins, Polymer, 26, 147 (1985). However, molecular weight control is difficult to achieve with such transition metal or rare earth catalysts and monomer conversions are often very modest.
Japanese Patent Application No. 67187-1967 discloses a catalyst system and technique for synthesizing TPBD consisting of 75 to 80 percent trans-1,4-structure and 20 to 25 percent 1,2-structure. The catalyst system described by this reference consists of a cobalt compound having a cobalt organic acid salt or organic ligand, an organoaluminum compound and phenol or naphthol. Gel formation is a serious problem which is frequently encountered when this three-component catalyst system is utilized in the synthesis of TPBD. Gelation is a particularly serious problem in continuous polymerizations. By utilizing the catalyst system and techniques of this invention, TPBD can be synthesized in a continuous process with only minimal amounts of gel formation.
U.S. Pat. No. 5,089,574 is based upon the finding that carbon disulfide will act as a gel inhibitor in conjunction with three component catalyst systems which contain an organocobalt compound, an organoaluminum compound and a para-alkyl-substituted phenol. U.S. Pat. No. 5,089,574 also indicates that conversions can be substantially improved by utilizing para-alkyl-substituted phenols which contain from about 12 to about 26 carbon atoms and which preferably contain from about 6 to about 20 carbon atoms.
U.S. Pat. No. 5,089,574 more specifically reveals a process for synthesizing trans-1,4-polybutadiene in a continuous process which comprises continuously charging 1,3-butadiene monomer, an organocobalt compound, an organoaluminum compound, a para-substituted phenol, carbon disulfide and an organic solvent into a reaction zone; allowing the 1,3-butadiene monomer to polymerize in said reaction zone to form the trans-1,4-polybutadiene; and continuously withdrawing the trans-1,4-polybutadiene from said reaction zone.
The techniques described in U.S. Pat. No. 5,089,574 are very useful in improving conversions and reducing gel formation. However, its teachings do not describe a technique for controlling the molecular weight of the TPBD being synthesized. In many applications, it would be desirable for the TPBD produced to have a lower molecular weight. There is, accordingly, a need to control the molecular weight of the TPBD produced with such Ziegler-Natta catalyst systems.
U.S. Pat. No. 5,448,002 discloses that dialkyl sulfoxides, diaryl sulfoxides and dialkaryl sulfoxides act as molecular weight regulators when utilized in conjunction with cobalt-based catalyst systems in the polymerization of 1,3-butadiene monomer into TPBD. U.S. Pat. No. 5,448,002 reports that the molecular weight of the TPBD produced decreases with increasing levels of the dialkyl sulfoxide, diaryl sulfoxide or dialkaryl sulfoxide present as a molecular weight regulator.
U.S. Pat. No. 5,448,002 specifically discloses a process for the synthesis of trans-1,4-polybutadiene which comprises polymerizing 1,3-butadiene monomer under solution polymerization conditions in the presence of at least one sulfoxide compound selected from the group consisting of dialkyl sulfoxides, diaryl sulfoxides and dialkaryl sulfoxides as a molecular weight regulator and in the presence of a catalyst system which includes an organocobalt compound, an organoaluminum compound and a para-alkyl-substituted phenol.
The presence of residual cobalt in TPBD made with cobalt-based catalyst systems is not desirable. This is because the residual cobalt can lead to polymer instability during storage. This is a particular problem in cases where the TPBD is stored in a "hot-house" prior to usage which is a standard procedure in many industries, such as the tire industry. In any case, higher levels of residual cobalt in the TPBD lead to worse problems with polymer instability. For this reason, it would be highly desirable to reduce the level of cobalt needed in catalyst systems which are used in the synthesis of TPBD. Reducing the level of cobalt needed is, of course, also desirable from a cost standpoint since cobalt compounds are relatively expensive.
Unfortunately, carbon disulfide is typically required as a gel-reducing agent in the synthesis of TPBD with cobalt-based catalyst systems. This is particularly true in the case of continuous polymerization systems. However, the presence of carbon disulfide in such systems reduces the level of catalyst activity and generally makes it necessary to increase the level of cobalt in the catalyst system. Thus, in cases where carbon disulfide is required for gel control, the level of cobalt needed is further increased.
SUMMARY OF THE INVENTION
By utilizing the techniques of this invention, trans-1,4-polybutadiene having a trans-isomer content within the range of about 82 percent to about 87 percent can be synthesized continuously to a high level of conversion utilizing a low level of a highly active cobalt-based catalyst system. The trans-1,4-polybutadiene made with the cobalt-based catalyst system of this invention also typically has a molecular weight which is acceptable for use in tire applications without the need for employing a molecular weight regulator. More specifically, the TPBD made utilizing the catalyst system of this invention typically has a dilute solution viscosity which is within the range of about 1.4 to about 2.4.
It is not typically necessary to utilize a gel inhibitor, such as carbon disulfide, in the polymerizations of this invention. This is because the TPBD made with the catalyst system of this invention produces an essentially gel-free polymer without the need for a gel inhibitor. Since a low level of residual cobalt is present in the trans-1,4-polybutadiene which is made utilizing the catalyst system of this invention, it is much more stable than trans-1,4-polybutadiene made with standard cobalt-based catalyst systems.
The present invention more specifically reveals a process for synthesizing trans-1,4-polybutadiene by polymerizing 1,3-butadiene monomer in the presence of a catalyst system which is comprised of cobalt (III) acetylacetonate, an organoaluminum compound and a para-alkyl-substituted phenol, wherein the cobalt (III) acetylacetonate is mixed with the para-alkyl-substituted phenol prior to the polymerization.
The subject invention also reveals a process for synthesizing trans-1,4-polybutadiene in a continuous process which comprises continuously charging 1,3-butadiene monomer, cobalt (III) acetylacetonate, an organoaluminum compound, a para-alkyl-substituted phenol and an organic solvent into a reaction zone, wherein the cobalt (III) acetylacetonate is mixed with the para-alkyl-substituted phenol prior to being charged into the reaction zone; allowing the 1,3-butadiene monomer to polymerize in said reaction zone to form the trans-1,4-polybutadiene; and continuously withdrawing the trans-1,4-polybutadiene from said reaction zone. In practicing the process of this invention, it is preferred for the molar ratio of the para-substituted phenol to the cobalt (III) acetylacetonate to be within the range of about 12:1 to about 16:1 and for the molar ratio of the organoaluminum compound to the cobalt (III) acetylacetonate to be within the range of about 16:1 to about 24:1.
DETAILED DESCRIPTION OF THE INVENTION
The polymerizations of the present invention will normally be carried out in a hydrocarbon solvent which can be one or more aromatic, paraffinic or cycloparaffinic compounds. These solvents will normally contain from 4 to 10 carbon atoms per molecule and will be liquids under the conditions of the polymerization. Some representative examples of suitable organic solvents include pentane, isooctane, cyclohexane, methylcyclohexane, isohexane, n-heptane, n-octane, n-hexane, benzene, toluene, xylene, ethylbenzene, diethylbenzene, isobutylbenzene, petroleum ether, kerosene, petroleum spirits, petroleum naphtha, and the like, alone or in admixture.
In the solution polymerizations of this invention, there will normally be from 5 to 30 weight percent 1,3-butadiene monomer in the polymerization medium. Such polymerization media are, of course, comprised of the organic solvent and 1,3-butadiene monomer. In most cases, it will be preferred for the polymerization medium to contain from 10 to 25 weight percent monomer. It is generally more preferred for the polymerization medium to contain 15 to 20 weight percent 1,3-butadiene monomer.
The microstructure of the TPBD varies with the monomer concentration utilized in its synthesis. Lower monomer concentrations in the polymerization medium result in higher trans contents. As the concentration of 1,3-butadiene monomer in the polymerization medium is increased, the level of trans-1,4 structure decreases. For instance, at a 1,3-butadiene monomer concentration of 5 weight percent, trans contents of about 84 percent are typical. In cases where the polymerization medium contains about 30 weight percent monomer, TPBD having a trans content of only about 68 percent is generally produced.
Such polymerizations can be carried out utilizing batch, semi-continuous or continuous techniques. In a continuous process, additional 1,3-butadiene monomer, catalyst and solvent are continuously added to the reaction zone (reaction vessel). The polymerization temperature utilized will typically be within the range of about 20° C. to about 125° C. It is normally preferred for the polymerization medium to be maintained at a temperature which is within the range of about 65° C. to about 95° C. throughout the polymerization. It is typically most preferred for the polymerization temperature to be within the range of about 70° C. to about 90° C. The pressure used will normally be sufficient to maintain a substantially liquid phase under the conditions of the polymerization reaction.
The polymerization is conducted for a length of time sufficient to permit substantially complete polymerization of the 1,3-butadiene monomer. In other words, the polymerization is normally carried out until high conversions are realized. In a continuous two-reactor system, the residence time in the first reactor will typically be from about 0.5 hours to about 1 hour with the residence time in the second reactor being about 1 hour to about 2 hours. In commercial operations, conversions in excess of about 80 percent will normally be attained. The polymerization can then be terminated using a standard procedure.
The organoaluminum compounds that can be utilized typically have the structural formula: ##STR1## in which R 1 is selected from the group consisting of alkyl groups (including cycloalkyl), aryl groups, alkaryl groups, arylalkyl groups, alkoxy groups and hydrogen; R 2 and R 3 being selected from the group consisting of alkyl groups (including cycloalkyl), aryl groups, alkaryl groups and arylalkyl groups. Some representative examples of organoaluminum compounds that can be utilized are diethyl aluminum hydride, di-n-propyl aluminum hydride, di-n-butyl aluminum hydride, diisobutyl aluminum hydride, diphenyl aluminum hydride, di-p-tolyl aluminum hydride, dibenzyl aluminum hydride, phenyl ethyl aluminum hydride, phenyl-n-propyl aluminum hydride, p-tolyl ethyl aluminum hydride, p-tolyl n-propyl aluminum hydride, p-tolyl isopropyl aluminum hydride, benzyl ethyl aluminum hydride, benzyl n-propyl aluminum hydride, and benzyl isopropyl aluminum hydride, diethylaluminum ethoxide, diisobutylaluminum ethoxide, dipropylaluminum methoxide, trimethyl aluminum, triethyl aluminum, tri-n-propyl aluminum, triisopropyl aluminum, tri-n-butyl aluminum, triisobutyl aluminum, tripentyl aluminum, trihexyl aluminum, tricyclohexyl aluminum, trioctyl aluminum, triphenyl aluminum, tri-p-tolyl aluminum, tribenzyl aluminum, ethyl diphenyl aluminum, ethyl di-p-tolyl aluminum, ethyl dibenzyl aluminum, diethyl phenyl aluminum, diethyl p-tolyl aluminum, diethyl benzyl aluminum and other triorganoaluminum compounds. The preferred organoaluminum compounds include triethyl aluminum (TEAL), tri-n-propyl aluminum, triisobutyl aluminum (TIBAL), trihexyl aluminum and diisobutyl aluminum hydride (DIBA-H).
Halogens, such as fluorine, chlorine, bromine and iodine, and halogen containing compounds have been found to be poisons and are detrimental to the polymerizations of this invention. The polymerizations of this invention will accordingly be conducted in the absence of significant quantities of halogens and halogen containing compounds.
The para-alkyl-substituted phenols which can be utilized generally have the structural formula: ##STR2## wherein R is an alkyl group which contains from about 6 to about 20 carbon atoms. Such para-alkyl-substituted phenols accordingly contain from about 12 to about 26 carbon atoms. In most cases, the alkyl group in the para-alkyl-substituted phenol will contain from about 8 to about 18 carbon atoms. Such para-alkyl-substituted phenols contain from about 14 to about 24 carbon atoms. It is typically preferred for the alkyl group in the para-alkyl-substituted phenol to contain from about 9 to about 14 carbon atoms. Such para-alkyl-substituted phenols contain from about 15 to about 20 carbon atoms. Exceptionally good results can be attained utilizing para-alkyl-substituted phenols having alkyl groups which contain 12 carbon atoms. These highly preferred para-alkyl-substituted phenols contain 18 carbon atoms. The polymerizations of this invention are initiated by charging the catalyst components into the polymerization medium.
The amount of cobalt (III) acetylacetonate utilized will typically be within the range of about 0.020 phm to about 0.075 phm (parts per hundred parts of 1,3-butadiene monomer). It is generally preferred for the cobalt (III) acetylacetonate to be employed at a level which is within the range of about 0.030 phm to about 0.065 phm. It is generally more preferred for the cobalt (III) acetylacetonate to be utilized in an amount within the range of about 0.045 phm to about 0.055 phm. In order to attain the level of solubility which is desired, it is important to utilize cobalt (III) acetylacetonate.
The organoaluminum compound will be employed in an amount sufficient to attain a molar ratio of the organoaluminum compound to the cobalt (III) acetylacetonate to be within the range of about 10:1 to about 50:1. It is typically preferred for the molar ratio of the organoaluminum compound to the cobalt (III) acetylacetonate to be within the range of about 12:1 to about 30:1. It is more preferred for the ratio of the organoaluminum compound to the cobalt (III) acetylacetonate to be within the range of about 16:1 to about 24:1.
It is critical in attaining the benefits of this invention for a portion of the para-alkyl-substituted phenol to be "premixed" with the cobalt (III) acetylacetonate prior to charging it into the polymerization medium. Normally, at least about 1 mole of the para-alkyl-substituted phenol will be premixed per mole of the cobalt (III) acetylacetonate. It is generally preferred for the molar ratio of para-substituted phenol to cobalt (III) acetylacetonate in the premix to be within the range of 2:1 to 37:1 with molar ratios within the range of 3:1 to 16:1 being most preferred. This can be accomplished by simply mixing the para-alkyl-substituted phenol with the cobalt (III) acetylacetonate prior to their introduction into the reaction zone. This will typically be accomplished by mixing the phenol with the cobalt (III) acetylacetonate in the presence of an organic solvent. This is because the organic solvent will reduce the viscosity of the mixture which makes it much easier to handle. Hexane is a highly preferred organic solvent for this purpose. In most cases, a sufficient amount of hexane will be added to make a solution which contains from about 1 weight percent to about 95 weight percent hexane, based upon the total weight of the para-alkyl-substituted phenol/cobalt (III) acetylacetonate/hexane solution. It is generally preferred for such solutions to contain from about 2 weight percent to about 20 weight percent hexane with it being most preferred for such solutions to contain from about 4 weight percent to about 10 weight percent hexane.
It is also critical to "prereact" a portion of the para-alkyl-substituted phenol with the organoaluminum compound prior to charging it into the polymerization medium. The balance of the para-alkyl-substituted phenol is prereacted with the cobalt (III) acetylacetonate. In other words, the portion of the para-substituted phenol which is not premixed with the cobalt (III) acetylacetonate is prereacted with the organoaluminum compound. The total molar ratio of para-alkyl-substituted phenol to the organoaluminum compound in the polymerization medium will be within the range of 2:1 to 3:1. It is preferred for a molar ratio of the para-alkyl-substituted phenol to the organoaluminum compound to be within the range of 2.3:1 to 2.8:1 with molar ratios within the range of about 2.5:1 to 2.6:1 being most preferred.
The molar ratio of the para-alkyl-substituted phenol to the cobalt (III) acetylacetonate will typically be within the range of about 1:1 to about 37:1. It is generally preferred for the molar ratio of the para-alkyl-substituted phenol to the cobalt (III) acetylacetonate to be within the range of about 1:1 to about 24:1. It is generally most preferred for the ratio of the para-alkyl-substituted phenol to the cobalt (III) acetylacetonate to be within the range of about 12:1 to about 16:1.
Carbon disulfide can be introduced into the polymerization medium as a separate component in cases where it is employed as a gel inhibitor or it can be premixed with the monomer and solvent prior to initiating the polymerization. In such cases, the molar ratio of the carbon disulfide to the cobalt will generally be within the range of about 0.05 to about 1. In any case, the carbon disulfide can be added "in situ" to the reaction zone by charging it separately from the other components. However, as has been explained, in most cases, it will not be necessary to add carbon disulfide to the polymerization as a gel inhibitor. In other words, the polymerizations of this invention will typically be carried out in the absence of carbon disulfide.
In the practice of this invention, it will not ordinarily be necessary to utilize a molecular weight regulator. Thus, the polymerizations of this invention will normally be conducted in the absence of molecular weight regulators. However, a dialkyl sulfoxide, a diaryl sulfoxide or a dialkaryl sulfoxide can optionally be included in the polymerization medium as a molecular weight regulator. The molecular weight of the TPBD produced naturally decreases with increasing levels of the sulfoxide molecular weight regulator present during the polymerization. In cases where a molecular weight regulator is utilized, the molar ratio of the sulfoxide molecular weight regulator to the cobalt compound will normally be within the range of about 0.05:1 to about 10:1.
The sulfoxides which can optionally be employed as molecular weight regulators can be dialkyl sulfoxides, diaryl sulfoxides or dialkaryl sulfoxides. These compounds have the general structural formula: ##STR3## wherein R 1 and R 2 can be the same or different and are selected from alkyl groups, aryl groups and alkaryl groups. R 1 and R 2 generally contain from 1 to about 12 carbon atoms. R 1 and R 2 will more typically contain from 1 to about 6 carbon atoms.
Some representative examples of dialkyl sulfoxides which can be used include dimethyl sulfoxide (DMSO), diethyl sulfoxide, dipropyl sulfoxide and dibutyl sulfoxide. Diphenyl sulfoxide is an example of a diaryl sulfoxide which can be employed as the molecular weight regulator. Some representative examples of dialkaryl sulfoxides which can be utilized include di-3-phenylpropyl sulfoxide, di-phenylmethyl sulfoxide and di-para-methylphenyl sulfoxide.
In the TPBD produced by the process of this invention, at least about 65 percent of the butadiene repeat units in the polymer are of the trans-1,4-isomeric structure. The TPBD made utilizing the catalyst system of this invention typically has a trans-isomer content of at least about 70 percent. In most cases, the TPBD made by the process of this invention will have a trans-isomer content which is within the range of about 75 percent to about 87 percent.
The polymerizations of this invention result in the formation of solutions containing the TPBD. Standard techniques can be utilized to recover the TPBD from the solution in which it is dissolved. Coagulation techniques will typically be employed to recover the TPBD from the organic solvent. Such coagulation procedures typically involve the addition of an alcohol or ketone to the TPBD solution to induce coagulation. However, the TPBD can also be recovered from the organic solvent by evaporation procedures, such as steam-stripping. Such evaporation procedures typically involve heating the polymer solution to a slightly elevated temperature in conjunction with the application of vacuum.
The TPBD made utilizing the techniques of this invention is a thermoplastic resin. It can be molded into various useful articles. Because the TPBD contains many double bonds in its backbone, it can also be blended and cocured with rubbers. Despite the fact that TPBD of this invention is a thermoplastic resin, it becomes elastomeric when cured alone or when cocured with one or more rubbers. TPBD has the ability to strain crystallize which improves properties, such as tensile strength, tear strength and flex fatigue. It can accordingly be used in manufacturing rubber articles such as hoses, belts and tires which have improved performance characteristics. By virtue of the fact that a low level of cobalt is present in the catalyst systems of this invention, the level of residual cobalt in the TPBD made by the process of this invention is greatly reduced. This significantly improves the thermal stability of the TPBD.
This invention is illustrated by the following examples which are merely for the purpose of illustration and are not to be regarded as limiting the scope of the invention or the manner in which it can be practiced. Unless specifically indicated otherwise, all parts and percentages are given by weight.
EXAMPLES 1-20
In this series of experiments, TPBD was synthesized utilizing the techniques of this invention. In the procedure used, a cobalt catalyst solution was made by first adding cobalt (III) acetylacetonate (cobaltic acetylacetonate) to a make-up vessel followed by the addition of p-dodecylphenol (DP). The cobalt (III) acetylacetonate was obtained from The Shepherd Chemical Company and the p-dodecylphenol was obtained from Schenectady Chemicals. Then, about 30 percent of the hexanes was added and the make-up bottle was placed on a shaker. Dissolution was complete within a few minutes. Then, more hexanes was added to provide a final concentration of 0.05M cobalt.
Aluminum catalyst solutions were also made by mixing triethylaluminum with p-dodecylphenol in hexanes. Various ratios were used in the make-up, depending on the amount of p-dodecylphenol used in making up the cobalt salt solution.
Polymerizations were carried out by charging solutions containing 14.5 percent 1,3-butadiene in hexanes into 4-ounce (118 ml) polymerization bottles followed by the addition of the aluminum catalyst solution and the cobalt catalyst solution. In this series of experiments, the molar ratio of aluminum to cobalt was held constant at 24:1 and the cobalt level was held constant at 0.054 phm. The molar ratio of the p-dodecylphenol to the cobalt is reported in Table I. It should be noted that p-dodecylphenol was not included in the polymerizations of Examples 1-5.
During the polymerizations, the polymerization bottles were rotated end-over-end in a water bath which was maintained at a temperature of 65° C. After the desired polymerization time, a shortstop solution was added to give 1.0 phm of 2-propanol and 1.0 phm of an antioxidant. The TPBD was then isolated by air drying followed by drying in a vacuum oven. The polymer yields and dilute solution viscosities of the TPBD polymers made is reported in Table I.
TABLE I______________________________________Example DP:Co ratio Yield DSV (dl/g)______________________________________1 -- 23% 2.882 -- 52% 4.073 -- 68% 4.354 -- 81% 4.595 -- 97% 4.756 3:1 34% 2.757 3:1 57% 3.238 3:1 68% 3.309 3:1 79% 3.6410 3:1 96% 3.6211 14:1 32% 1.7912 14:1 48% 1.9813 14:1 59% 2.1514 14:1 64% 2.2415 14:1 84% 2.3416 37:1 32% 1.617 37:1 46% 1.7718 37:1 51% 1.8419 37:1 68% 2.1820 37:1 89% 2.32______________________________________
COMPARATIVE EXAMPLES 21-25
In this series of experiments, the same procedure which was utilized in Examples 1-20 was repeated except for the fact that cobalt octanoate was substituted for the cobalt (III) acetylacetonate. The results of this series of experiments is reported in Table II.
TABLE II______________________________________Example DP:Co ratio Yield DSV (dl/g)______________________________________21 -- 31% 4.7722 -- 56% 5.8023 -- 72% 6.3124 -- 81% 6.5225 -- 95% 7.01______________________________________
As can be seen by reviewing the data in Table II, the molecular weights of TPBD synthesized in this series of experiments was much higher than the molecular weights of the TPBD made utilizing cobalt (III) acetylacetonate. This is exemplified by the fact that the dilute solution viscosities of the TPBD polymers made in this series of experiments is much higher. This series of experiments accordingly shows the criticality of employing cobalt (III) acetylacetonate in the catalyst system.
COMPARATIVE EXAMPLE 26
In this experiment, TPBD was synthesized utilizing a catalyst system like the one employed in Examples 1-20 except for the fact that cobalt octanoate was substituted for the cobalt (III) acetylacetonate and that the cobalt octanoate was not premixed with the p-dodecylphenol. Additionally, the level of cobalt octanoate was increased to 0.25 phm. Thus, the level of cobalt employed was about 5 times higher than the level of cobalt employed in Examples 1-20.
The polymer yield attained in this experiment was about 85 percent and the TPBD made was determined to have a dilute solution viscosity of 2.32 dl/g. Thus, the TPBD made in Example 20 had the same dilute solution viscosity as the polymer made in this experiment. However, it was synthesized using only about 22 percent as much cobalt in the catalyst system. Nevertheless, the polymer yield attained in Example 20, using the technique of this invention, was higher than the yield realized in this comparative experiment. Thus, this comparative experiment shows the enormous benefit which can be realized by utilizing the technique of this invention in the synthesis of TPBD.
While certain representative embodiments and details have been shown for the purpose of illustrating the present invention, it will be apparent to those skilled in this art that various changes and modifications can be made therein without departing from the scope of the present invention. | By utilizing the techniques of this invention, trans-1,4-polybutadiene can be synthesized continuously to a high level of conversion utilizing a low level of a highly active cobalt-based catalyst system. The trans-1,4-polybutadiene made with the cobalt-based catalyst system of this invention also typically has a molecular weight which is acceptable for use in tire applications without the need for employing a molecular weight regulator. It is also not typically necessary to utilize a gel inhibitor, such as carbon disulfide, in the polymerizations of this invention. Since a low level of residual cobalt is present in the trans-1,4-polybutadiene which is made utilizing the catalyst system of this invention, it is much more stable than trans-1,4-polybutadiene made with standard cobalt-based catalyst systems. This invention specifically relates to a process for synthesizing trans-1,4-polybutadiene by polymerizing 1,3-butadiene monomer in the presence of a catalyst system which is comprised of cobalt (III) acetylacetonate, an organoaluminum compound and a para-alkyl-substituted phenol, wherein the cobalt (III) acetylacetonate is mixed with the para-substituted phenol prior to the polymerization. Such polymerizations can be conducted on a batch or a continuous basis. | 8 |
BACKGROUND
[0001] 1. Technical Field
[0002] The development relates to providing cooling for electric motors.
[0003] 2. Background Art
[0004] Electric motors can be used as a power source in vehicles. It is known that the motor can overheat depending on the severity of the operating condition to which it is subjected.
[0005] Most automotive vehicle manufacturers offer a variety of electric and hybrid electric vehicles for sale. The offerings differ in their weight, hauling capacity, and duty cycle. For vehicles that include an electric traction motor or a motor generator, or other high-power motor, the maximum power demands on the motor differ greatly depending on the application. The maximum power affects the cooling needs of the motor. Cooling, by circulating a liquid within an electric motor, is known in the prior art. However, cooling systems are designed for a particular motor used in a particular vehicle configuration with a particular cooling demand. For an alternate vehicle configuration that, for example, uses the same motor system but has a higher power level, greater cooling is needed. Such a system designed for a particular cooling demand must be redesigned for each cooling demand level to ensure proper heat transfer, volumetric coolant flow, and directional flow control, among other considerations.
SUMMARY
[0006] To overcome the difficulty of redesigning the entire motor system for each application, an electric motor is disclosed, which has an end cap attached to the motor, with the end cap having many of the components directed toward providing the desired cooling for the motor. For example, the end cap can contain: the heat exchanger having a high-temperature coolant passage, a low-temperature coolant passage, a pump to circulate the high-temperature coolant through the high-temperature coolant passage, and related components for hydraulic and thermal control, such as electronic valves, temperature and pressure sensors, and an electronic control unit. In one embodiment, a mechanical thermostatic valve is provided to control flow through the high temperature coolant loop. In another embodiment, an electrically-controlled valve is provided in the high temperature coolant loop, with the valve controlled by an electronic control unit ECU. In one embodiment, the ECU is provided in the end cap with the ECU controlling the valve's position based on signals from temperature and/or pressure sensors electronically coupled to the ECU. In one embodiment, the motor's output shaft passes through the end cap. In this embodiment, the end cap contains a shaft seal and bearing. The end cap can also have a hydraulic accumulator, fill and drain ports, and fasteners, to attach the cap to the motor. Based on the intended application, an end cap including: the desired level of cooling, appropriate control components for the cooling system, bosses for the fluid and electrical inputs/outputs, etc., is attached to the motor. By including these components in the end cap, the motor can be standard for all applications with all necessary changes to accommodate the cooling and hydraulic rates required by various applications contained in the end cap.
[0007] According to an embodiment of the disclosure, an electric motor is disclosed which has a high-temperature coolant within. The motor has an end cap attached to the motor with an integral heat exchanger. The heat exchanger has a high-temperature coolant passage, a pump to circulate the high-temperature coolant through the high-temperature coolant passage, and related components for hydraulic and thermal control, for example, electronic valves, sensors, and electronic control unit. The end cap and the motor are separately assembled. In one embodiment, the high-temperature coolant is oil.
[0008] In a liquid-to-air heat exchanger embodiment, the exterior surface of the end cap has fins. In a liquid-to-liquid heat exchanger embodiment, the heat exchanger has a low-temperature coolant passage coupled to a low-temperature coolant loop external to the end cap. In one embodiment, the low-temperature coolant loop has a thermostat, which typically contains a thermally actuated valve. The high temperature and low-temperature coolant passages form interlaced spirals in the end cap, in one example.
[0009] In one example, there is a low-temperature coolant passage in the heat exchanger with the low-temperature coolant passage being part of a low-temperature coolant loop. Also, an external heat exchanger and a pump are disposed in the loop. The external heat exchanger transfers heat from the low-temperature coolant to another medium, such as air.
[0010] In another embodiment, the end cap of the electric motor contains hydraulic and thermal management components, including, for example, electronic valves, electronics control unit, a pump for the low-temperature coolant, electronic sensors, and a hydraulic accumulator. These components are used to modify cooling of the motor. For example, it may be desirable to partially close a valve in the high-temperature coolant passage to allow faster motor warm-up. By allowing faster warm-up, parasitic drag caused by the motor lubricant may be reduced.
[0011] In yet another embodiment, the electric motor is disposed in an automotive vehicle. There is a heat-generating unit separate from the electric motor already described. This heat-generating unit can be an internal combustion engine, a power-steering pump, or a transaxle. The heat-generating unit has a cooling loop adapted to circulate a liquid coolant, a pump in the heat-generating unit cooling loop, a heat exchanger in the heat-generating unit cooling loop; and a branch of the heat-generating unit cooling loop coupled to the motor's low-temperature coolant loop. The low-temperature coolant may be, for example, a water-based coolant, power steering fluid, hydraulic fluid, dielectric fluid, transmission fluid, or lubricating oil.
[0012] In one embodiment, the low temperature passage is coupled to a branch off of an air-conditioning loop coupled to an air-conditioning unit or any refrigeration unit. Refrigerant is the working fluid in this embodiment.
[0013] Also disclosed is a hybrid electric vehicle including an internal combustion engine with an internal cooling path, a cooling circuit coupled to the internal cooling path in the engine, an external heat exchanger, e.g. a radiator, disposed in the cooling circuit, and a water pump disposed in the cooling circuit. The vehicle also has an electric motor with a heat exchanger disposed in an end cap of the electric motor. The motor's heat exchanger includes a high-temperature cooling passage with the high-temperature passage's inlet connected to a circulating pump and the high-temperature passage's outlet coupled to the motor's interior. The heat exchanger in the motor's end cap also has a low-temperature cooling passage adapted to circulate a water-based coolant. The low-temperature cooling passage is coupled to the engine cooling circuit. The end cap may also contain thermal management components, for example, electronic valves and thermal sensors. The end cap assembly of the electric motor is a separate component from the electric motor. Non-limiting embodiments show the electric motor functioning as a motor-generator, a traction motor, or both.
[0014] Also disclosed is a method to provide a cooling system for an electric motor. An end cap with an integral heat exchanger is selected, which has predetermined heat transfer characteristics. The end cap with these characteristics is attached to the electric motor housing. The method also includes determining the cooling requirement of the electric motor at its most demanding operating condition for its design duty cycle. Based on that cooling requirement the predetermined heat transfer characteristics which provide the required cooling are computed. The heat exchanger in the end cap has a low-temperature coolant passage and a high-temperature coolant passage. The predetermined heat transfer characteristics take into account the following factors: material of the end cap, the effective surface area for heat transfer between the high-temperature and low-temperature coolants, the expected coolant flow rates, the expected temperatures, the properties of the low-temperature coolant, and the properties of the high-temperature coolant.
[0015] An advantage of the present disclosure is that having the heat exchanger and hydraulic components for cooling the motor placed in the end cap, the cooling level required for the motor's application can be met by selecting an end cap assembly with the desired cooling capacity, while little or no change is made to the motor itself. In this way, a single motor design can be used in many vehicle applications with various end caps that can be coupled to the motor to satisfy the cooling requirements of the particular vehicle configuration.
[0016] The coolant passages are described above as high-temperature and low-temperature. However, according to an embodiment of the present disclosure, the motor can be warmed when the coolant within the motor is at a lower temperature than the external coolant. In such a situation, energy is supplied to the motor, thereby providing yet another advantage by bringing the motor to its desired operating temperature more quickly. The passages can be referred to as first coolant passage and second coolant passage with the understanding that in some situations these are high-temperature coolant passage and low-temperature coolant passage, respectively, when the motor is being cooled and in other situations these are low-temperature coolant passage and high-temperature coolant passage, respectively, when the motor is being warmed up.
[0017] The above advantages and other advantages and features of the present disclosure will be apparent from the following detailed description when taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 is a side view of a cross section of an electric motor;
[0019] FIG. 2 is an end view of the end cap shown in cross-section to show the internal cooling passages;
[0020] FIG. 3 is an end view of the end cap shown in cross-section to show the internal cooling passages;
[0021] FIG. 4 is a side view of a cross section of a portion of the electric motor;
[0022] FIG. 5 is an end view of the end cap shown in cross-section to show the internal cooling passages;
[0023] FIG. 6 is a side view of a cross section of a portion of the electric motor;
[0024] FIG. 7 is an exterior view of the end of the end cap with cooling fins on the exterior surface;
[0025] FIG. 8 is a diagrammatic view of the cooling system for an electric motor coupled to the cooling system of an internal combustion engine cooling system;
[0026] FIG. 9 is a diagrammatic view of the cooling system for an electric motor;
[0027] FIG. 10 is a side view of a cross section of a portion of the electric motor for an embodiment which includes a gear set within the housing of the electric motor;
[0028] FIG. 11 is a side view of a portion of a dry electric motor in which the stator is cooled by a fluid circulating within an enclosure;
[0029] FIG. 12 is an isometric view of an end cap according to one embodiment of the disclosure;
[0030] FIGS. 13-15 are diagrammatic views of the motor assembly with end cap per three embodiments of the disclosure.
DETAILED DESCRIPTION
[0031] A motor 10 is shown in FIG. 1 which has an end cap 12 . Motor 10 has a stator 20 with a rotor 22 inserted into stator 20 . Output shaft 24 is connected to rotor 22 . An end of output shaft 24 goes through end cap 12 . Output shaft 24 can extend out at one end of motor 10 only or at both ends depending on the desired configuration. The end cap has a seal and bearing 26 , which can be integrated or separate components. Motor 10 has a liquid coolant circulating within, contacting both the stator and rotor, or the stator only. In one embodiment, the liquid is oil. Thermal energy is extracted from motor 10 via coolant circulation. Coolant enters the end cap 12 at 30 and exits at 32 , being pumped by pump 34 which is driven by shaft 24 . Pump 34 has a coolant pickup 31 at the bottom of motor 10 . Within end cap 12 is a liquid-to-liquid heat exchanger being supplied a second liquid coolant at 36 and removed at 38 . The second liquid can be a water-based coolant, in one embodiment. In another alternative, pump 34 is located on the shaft at the other end of rotor 22 and is contained in the end cap assembly. In yet another alternative, pump 34 is an electric pump which is not coupled to shaft 24 . In the configuration shown in FIG. 1 , shaft 24 goes through end cap 12 , with seal and bearing assembly 26 preventing fluid leakage out of motor 10 and supporting shaft 24 .
[0032] In FIG. 2 , an end view of end cap 12 is shown. The high temperature fluid, which circulates in the motor, is shown entering at 30 and exiting at 32 . The low temperature fluid enters at 36 and exits at 38 . The channels for the two fluids are concentric spirals. The effective heat transfer surface area of the channels depends on the length of the spirals in FIG. 2 and the cross-sectional shape of the channels, as seen from the side view in FIG. 1 . By varying the length of end cap 12 , dimension L of end cap 12 as shown in FIG. 1 , the cooling capacity is affected.
[0033] An alternate embodiment of end cap 12 ′ is shown in FIGS. 3 and 4 in which the low- and high-temperature fluids are conducted through channels which zig zag between each other. The flow shown in FIG. 3 has a parallel-flow configuration where both high- and low-temperature fluids enter at the same end ( 30 ′ and 36 ′) and travel parallel to each other, exiting at 32 ′ and 38 ′, respectively. Alternatively, a counter flow configuration is possible in which the exit of the low-temperature fluid is close to the entrance of the high-temperature fluid. Such a configuration would have the flow direction of either the low- or high-temperature fluid (not both) in FIG. 3 reversed.
[0034] Another alternative for end cap 12 ″ is shown in FIGS. 5 and 6 in which low-temperature fluid enters into a cavity in end cap 12 ″. A tube 39 for high-temperature fluid is placed through the center of the cavity such that the tube carrying the high-temperature fluid is surrounded by low-temperature fluid. A counter-flow configuration is shown in FIG. 5 . However, both counter-flow and parallel-flow configuration embodiments are contemplated for any of the embodiments shown in FIGS. 2 , 3 , and 5 . Tube 39 is shown as one continuous loop in the plane of the cross-section. However, it is desirable to affect the contact surface area between the low- and high-temperature fluids to allow a variety of cooling levels. Thus, tube 39 can be bent, multiply, in the direction along the length of end cap 12 ″ to provide more cooling than a smooth bend as shown in FIG. 5 . Alternatively, tube 39 can include multiple loops within the cavity formed in end cap 12 ″. In FIG. 5 , tube 39 contains the high-temperature fluid circulating within and low-temperature fluid is circulating in the cavity on the outside of tube 39 . Alternatively, the cold fluid is circulated through tube 39 and the hot fluid is circulated within the cavity in end cap 12 ″.
[0035] FIGS. 2 , 3 and 5 show end cap 12 , 12 ′, and 12 ″ having a liquid-to-liquid heat exchanger. An alternative is shown in FIG. 7 in which the outside surface of end cap 12 ′″ is an air-to-liquid heat exchanger with rows of fins 40 placed on the outside of end cap 12 ′″.
[0036] An example configuration in which the low-temperature fluid is engine coolant is shown in FIG. 8 . An internal combustion engine 50 has coolant that circulates through engine 50 and radiator 52 with a thermostat 54 regulating the flow. Engine 50 has a water pump 56 and pulleys 58 . A branch off of the engine's cooling system is supplied to end cap 12 of motor 10 . The branch supplying engine coolant to motor 10 , in one embodiment, has a thermostatic valve 60 to control flow to end cap 12 . As shown in FIG. 8 , the thermostat 60 is external to end cap 12 . Alternatively, thermostatic valve 60 and accompanying hydraulic control components are integrated with end cap 12 .
[0037] In another example embodiment in FIG. 9 , motor 10 has its own low-temperature coolant circulating system with its own pump (not shown) and external heat exchanger 62 . In one embodiment, the low-temperature coolant pump is integrated with end cap 12 . The low-temperature fluid is water-based in one embodiment or oil in another embodiment.
[0038] The embodiment of end cap 12 shown in FIG. 7 obviates the low-temperature-fluid cooling loop. A cooling fan (not shown) can be provided to force flow past fins 40 . The cooling fan may be driven, for example, by motor 10 via shaft 24 , by a separate electric motor (not shown), or by another source. In one embodiment, the cooling fan and drive are integrated with end cap 12 .
[0039] Referring to FIG. 10 , an electric motor 10 ′ accommodates installation of an element within. The element can be a gear set or any other element which augments motor functionality and would benefit from lubrication and cooling available within electric motor 10 ′.
[0040] The embodiments shown in FIGS. 1 and 10 envision coolant sloshing and spraying about within motor 10 . In these embodiments, the coolant may be a lubricating hydraulic oil that provides both lubrication and cooling to the rotor, stator, gear box (element 64 of FIG. 10 ), and any other components with motor 10 . An alternative configuration is shown in FIG. 11 in which assembly 66 comprises rotor 22 ′ and stator 20 ′. Stator 20 ′ is provided lubricant within an enclosure 68 . In FIG. 11 , coolant is provided by inlet 70 and returned by outlet 72 . In this embodiment, the motor is dry inside with coolant provided only to stator 20 ′.
[0041] An isometric drawing of an end cap, according to an embodiment of the present disclosure, in FIG. 12 , shows inlet port 36 and outlet port 38 for low temperature coolant. Seal and bearing 26 are provided for sealing and supporting, respectively, a shaft ( 24 of FIG. 1 ). An electronic control unit (ECU) 80 is provided in end cap 12 . In an embodiment in which the motor assembly is installed in a vehicle, an ECU mounted elsewhere in the vehicle can be used, in which case element 80 is a connector for the electrical connections between a remotely mounted ECU and electrical components within end cap 12 . An electrically driven pump 78 is mounted on end cap 12 . End cap 12 is coupled to motor 12 by fasteners 76 . End cap 12 can be mounted to motor 12 by any known method.
[0042] A circuit diagram of end cap 12 is shown in FIG. 13 . End cap 12 is coupled to electric motor 10 . Electric motor 10 , in one embodiment, is a traction motor coupled to an automobile axle. Electric motor 10 , in some embodiments, has a reservoir and vent 88 and a drain port 90 . End cap 12 has a high temperature coolant loop, which supplies coolant to motor 10 at 32 with the return at 30 . The coolant is circulated via pump 34 which is shaft driven by electric motor 10 . In the coolant circuit is a filter 92 , a temperature sensor 102 , and a valve 94 . ECU 80 is electronically coupled to valve 94 to control the fraction of coolant flow passing through air-to-liquid heat exchanger 96 and the fraction of flow bypassing heat exchanger 96 through bypass 86 . Note that electrical lines are denoted by thicker lines than hydraulic lines in FIGS. 13-15 . ECU 80 determines the position at which to control valve 94 based on temperature information from temperature sensors 100 and 102 . Alternatively, valve 94 is a mechanical valve, such as a wax-motor driven thermostat, the position of which is based on the fluid temperature in communication with the wax motor.
[0043] An alternative embodiment is shown in FIG. 14 , in which end cap 12 has both a high-temperature and a low-temperature fluid circulating within. The high-temperature fluid coolant loop provides cooling for electric motor 10 . Such circuit has an internal filter 92 , temperature sensors 100 and 102 and an internal heat exchanger 104 . Circulation of coolant through the high-temperature fluid loop is provided by pump 34 which is shaft driven by electric motor 10 . Energy from the high-temperature fluid is extracted within heat exchanger 104 by virtue of a lower-temperature fluid circulating through the cold fluid loop. The amount of flow through the low-temperature fluid loop is determined by the position of valve 94 which controls the flow to: heat exchanger 108 , bypass 86 , or a combination of the two by pulse width modulation control of valve 94 or by valve 94 being controlled to an intermediate position. Flow through the low-temperature fluid loop is provided by an electric motor 110 . Alternatively, if the low temperature fluid is part of another cooling system, such as an engine cooling system in an automotive vehicle, flow to through the low-temperature fluid loop may be provided by a pump provided for the other cooling system, which obviates pump 110 . Valve 94 is electronically coupled to ECU 80 . ECU 80 controls the position of valve 94 , based on inputs received by ECU 80 from temperature sensors 100 , 102 , and 106 , to maintain the desired level of cooling and/or component temperatures.
[0044] In yet another embodiment shown in FIG. 15 , an electric pump 112 driven by electric motor 78 is provided to circulate coolant through the high-temperature fluid loop. Electric pump 112 is coupled to pump 110 , which circulates fluid through the low-temperature fluid loop. Thus, electric motor 78 drives both pumps 110 and 112 in this embodiment. The rest of the circuit is similar to FIG. 14 .
[0045] For the embodiments described to this point, the heat exchanger is used to transfer energy out of the motor assembly. Alternatively, the heat exchanger can be used to transfer energy into the motor assembly. This may be done to decrease parasitic drag losses when the motor and internal fluids are cold. This implementation is achievable with the same hardware, except that the external fluid is at a higher temperature than the motor coolant, allowing an energy transfer from the external fluid to the motor coolant to provide faster warm-up. The coolant loops are described below as first and second coolant loops and the coolant passageways are referred to as first and second coolant passageways. When the motor is being cooled, first coolant loop may be called high-temperature coolant loop and second coolant loop may be called low-temperature coolant loop. In the less common condition in which the motor is being warmed, first coolant loop may be called low-temperature coolant loop and second coolant loop may be called high-temperature coolant low. The same nomenclature applies to the coolant passageways and depends on whether the energy flow is into the motor for warming up or out of the motor for cooling down.
[0046] While particular embodiments of the disclosure have been shown and described, numerous variations and alternate embodiments will occur to those skilled in the art. All such variations and alternate embodiments and equivalents thereof are intended to be defined by the appended claims. | An electric motor which has a separate end cap heat exchanger, through which a liquid coolant is passed, is disclosed. In one example embodiment, the electric motor is a traction motor or motor-generator in a hybrid electric vehicle having an internal combustion engine. Additionally, in one embodiment, the heat exchanger has a low-temperature coolant loop configured to extract energy from the motor coolant. The electric motor may be installed in a variety of vehicles or other applications having greatly differing cooling requirements. By placing the heat exchanger and control componentry in the end cap, the cooling capability of the electric motor can be changed by selecting an end cap with the appropriate heat transfer characteristics and control componentry to provide the desired cooling. Consequently, a single electric motor, with a variety of end cap choices, can be used in a variety of applications. | 8 |
FIELD OF THE INVENTION
The present invention relates to a display apparatus including a CRT.
BACKGROUND OF THE INVENTION
FIG. 4 shows a structure of a conventional CRT display apparatus. In this figure, there is shown a CRT 14 , a cathode 2 , a G1 electrode 3 , a G2 electrode 4 , a G3 electrode 6 , an anode 7 , a video circuit 9 , a flyback transformer (FBT) 15 , and a variable resistor 16 . The G1, G2, and G3 electrodes are cylindrical-shaped electrodes disposed within the electron gun to draw electrons from the cathode and prefocus them. Another focusing electrode and the like disposed after the G3 electrode are omitted from the drawing to simplify explanation.
The operation of the apparatus of FIG. 4 will be explained below. A video signal is amplified by the video circuit 9 , and is supplied to the cathode 2 . A high voltage of about 25 KV, which the FBT 15 produces by stepping up and rectifying horizontal flyback pulses generated in a not-illustrated horizontal-deflection-signal output circuit, is applied to the anode 7 . The G2 electrode 4 is applied with a voltage of 700V to 1000V which the variable resistor 16 produces by dividing the high voltage. The current flowing through the G2 electrode 4 is very small, and therefore the variable resistor 16 has resistance as much as 100 MΩ. By adjusting the voltage applied to the G2 electrode 4 , a coarse adjustment to a threshold point at which electrons start to flow towards a screen and the screen starts to illuminate, which is called a screen adjustment, can be carried out.
Generally, a CRT display apparatus is provided with a facility of adjusting brightness and a facility of adjusting contrast. The brightness adjusting facility enables a user to tune a black level of a picture and the threshold point at which the screen starts to illuminate to his liking. Generally, this brightness adjusting facility is obtained by changing a black bias voltage of a video signal supplied to the cathode. The contrast adjusting facility enables a user to tune the ratio of a brightness of the darkest part to that of the brightest part in the picture to his liking. Generally, this contrast adjusting facility is obtained by changing the amplitude of a video signal supplied to the cathode.
On the other hand, the demand for improving intensity and resolution of a CRT display apparatuses is growing in recent years. Japanese Unexamined Patent Publication No. 11-224618 discloses a high intensity/resolution CRT (referred to as a “Hi-Gm tube” hereinafter) that addresses such a demand. This Hi-Gm tube features a novel electron gun that has, in addition to the G1, G2 and G3 electrodes, a modulating electrode called “Gm electrode” disposed between the G2 electrode and the G3 electrode.
FIG. 5 shows a structure of such an electron gun used for the Hi-Gm tube. In this figure, 17 denotes a G1 electrode, 18 denotes a G2 electrode, 19 denotes a G3 electrode, 20 denotes a cathode, 21 denotes an electron-emitting substance formed on the surface of the cathode, and 22 denotes a Gm electrode. This electron gun has, for the part following the G3 electrode where another focusing electrode and the like are disposed, the same structure as the conventional electron gun.
FIG. 6 is a graph showing potential distribution in the vicinity of the cathode within the electron gun of the Hi-Gm tube.
In this graph, the horizontal axis represents the distance (mm) from the cathode surface, the vertical axis represents the potential (V), and the curve 23 shows the potential distribution symmetrical with the axis of revolution in the vicinity of the cathode. Furthermore, the arrow 24 shows a range within which the Gm electrode 22 exists, which is about 0.5 mm from the cathode surface. The graph of FIG. 6 holds while the G1 electrode is applied with 0V, the G2 electrode is applied with 500V, the G3 electrode is applied with 5.5 KV, the Gm electrode is applied with 80V, and the anode is applied with the high voltage of 25 KV for example.
The potential of the Gm electrode 22 is set to about 80 VDC, so there is a position 25 within the range 24 at which the potential curve 23 is minimum. If the potential of the cathode 20 shown by the broken line is lower than the potential at this position 25 , electrons pass through the position 25 and flow towards the screen. If not, electrons do not flow towards the screen since they cannot pass through the position 25 .
As seen from this graph, between the cathode 20 and the position 25 , electrons always exist abundantly, and the potential slope after the position 25 is of the order of 10 6 (V/m). Compared with the potential slope between the cathode and the G1 electrode, it is greater by an order of magnitude. Accordingly, after electrons pass through the Gm electrode 22 , most of them can move towards the screen without being affected by spatial charges, so the intensity of the electron beam flowing to the screen is determined by the quantity of the electrons that pass through the position 25 at which the spatial potential is minimum.
For this reason, variation of the intensity of the electron beam when the cathode potential is varied by a certain value in the Hi-Gm tube is about twice as much as that in the conventional CRT. That is, the variation of the cathode potential required to vary the intensity of the electron beam by a certain value in the Hi-Gm tube is less than half the variation required in the conventional CRT. In other words, with the Hi-Gm tube, the variation of the intensity of the electron beam can be doubled for the same variation of the cathode potential. Consequently, with the Hi-Gm tube, it is possible to easily adapt to video signals of high frequency, and therefore to provide a display apparatus of high intensity and high resolution.
OBJECT AND SUMMARY OF THE INVENTION
Although it has been described that, in a conventional CRT display apparatus, brightness of a picture is adjusted by changing the value of a black bias voltage supplied to the cathode, it is necessary in reality, to change each of three bias voltages of the three channels of R, G, and B. Furthermore, in the case of adjusting contrast of a picture by changing the amplitude of a video signal supplied to the cathode, to obtain high contrast, expensive amplifiers having a high gain and an expensive power supply outputting a high voltage are required.
An object of the present invention is to provide a display apparatus in which brightness is adjusted by a simple circuit utilizing the above-described characteristics of the Hi-Gm tube. Another object of the present invention is to provide a display apparatus capable of displaying a picture in high contrast at a low cost.
The above-described object is achieved by a CRT display apparatus comprising:
a CRT including an electron gun,
the electron gun having a cathode, a G1 electrode, a G2 electrode and a G3 electrode disposed in that order to draw electrons from the cathode, the electron gun further having a modulating Gm electrode disposed between the G2 and G3 electrodes; and
a controller for controlling a value of a voltage applied to the Gm electrode to adjust brightness of a picture on a screen of the CRT.
The controller may be a voltage source which produces a voltage having a value corresponding to a value of a brightness adjustment signal input to the voltage source, and applies the produced voltage to the Gm electrode.
The above-described another object is achieved by a CRT display apparatus comprising:
a CRT including an electron gun,
the electron gun having a cathode, a G1 electrode, a G2 electrode and a G3 electrode disposed in that order to draw electrons from the cathode, the electron gun further having a modulating Gm electrode disposed between the G2 and G3 electrodes; and
a controller for controlling a value of a voltage applied to the G2 electrode to adjust contrast of a picture on a screen of the CRT.
The controller may be a voltage source which produces a voltage having a value corresponding to a value of a contrast adjustment signal input to the voltage source, and applies the produced voltage to the G2 electrode.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will now be described by way of example and with reference to the accompanying drawings in which:
FIG. 1 is a block diagram showing a structure of a first example of the CRT display apparatus according to the invention;
FIG. 2 is a graph showing a cathode voltage-beam current characteristic of a CRT;
FIG. 3 is a block diagram showing a structure of a second example of the CRT display apparatus according to the invention;
FIG. 4 is a block diagram showing a structure of a conventional CRT display apparatus;
FIG. 5 is an explanatory view of a structure of an electron gun in the vicinity of a cathode of a Hi-Gm tube; and
FIG. 6 is a graph showing potential distribution in the vicinity of the cathode within the electron gun of the Hi-Gm tube.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a block diagram showing the structure of a first example of the CRT display apparatus according to the present invention. Here, the “CRT display apparatus” means a display apparatus using a CRT, such as a television set or a monitor display for a personal computer. In this figure, reference numerals identical to those in FIG. 4 represent the same or equivalent elements.
In FIG. 1, there is shown a Hi-Gm tube 1 , a cathode 2 , a G1 electrode 3 , a G2 electrode 4 , a Gm electrode 5 , a G3 electrode 6 , an anode 7 , a video circuit 10 , and a Gm electrode power source 10 . Another focusing electrode and the like disposed after the G3 electrode are omitted from the drawing to simplify explanation.
A video signal is inverted and amplified by the video circuit 9 , and is supplied to the cathode 2 . The Gm electrode voltage source 10 produces a voltage to be applied to the Gm electrode 5 . This voltage source 10 is configured to produce a voltage having a value in accordance with a value of an after-described control signal which is input to this voltage source 10 . In this first example, the G1 electrode 3 is applied with 0V, the G2 electrode 4 is applied with 500V, the G3 electrode 6 is applied with 5.5 KV, the Gm electrode 5 is applied with 80V, and the anode 7 is applied with the high voltage of 25 KV.
The voltage applied to the Gm electrode 5 defines a threshold point at which electrons start to flow towards the screen causing the screen to illuminate. When the cathode voltage falls below the voltage of the Gm electrode 5 , an electron beam starts to flow, and thereby electrons hit the fluorescent substance of the screen causing the screen to illuminate. In the Hi-Gm tube, it is possible to match the point at which the screen starts to illuminate to the black level of a picture by equalizing the black bias voltage supplied to the cathode to the voltage of the Gm electrode.
In a case where black sinks too much and therefore the picture is dark as a whole and is not easy to see, a control signal input into the Gm electrode voltage source 10 is increased to raise the voltage applied to the Gm electrode 5 . As a result, the voltage corresponding to the point at which the screen starts to illuminate increases, and thereby the picture brightens, or brightness is increased. On the other hand, in a case where black is elevated too high and therefore the picture is lax, the control signal is reduced to lower the voltage applied to the Gm electrode 5 . This control signal may be a voltage signal output from an output port of a microcomputer when a user presses a key to adjust brightness, viewing a user-adjustment menu which is generated by a character generator or the like and displayed on the monitor screen. This control signal may be generated by other means such as a hardware including a microcomputer and switches, or software-based processing.
In the conventional CRT display apparatus, brightness adjustment is achieved by varying the three cathode bias voltages of the three channels of R, G, B in a like manner, whereas in this example, brightness adjustment is achieved by just varying the voltage applied to the Gm electrode, which simplifies its circuit structure.
FIG. 2 is a graph showing typical cathode voltage-beam current characteristics of CRTs. In this graph, the solid line represents a characteristic of a Hi-Gm tube and the dotted line represents a characteristic of a conventional CRT.
As shown in this graph, in the case of the Hi-Gm tube, if the voltage applied to the Gm electrode is set to A, no beam current flows while the cathode voltage is above A, and when the cathode voltage falls below A, a beam current starts to flow, and increases approaching the characteristic of the conventional CRT as the cathode voltage lowers.
Here, if the voltage applied to the Gm electrode is lowered from A to B, a point at which the screen starts to illuminate, or a black level goes down for the same video signal supplied to the cathode. At this moment, the beam current curve is steepened at its rising part. In consequence, a feeling of contrast having been enhanced in a mid-brightness range is obtained. On the other hand, if the voltage applied to the Gm electrode is raised from A to C, the black level goes up for the same video signal supplied to the cathode. In this case, the beam current curve is made gentle at its rising part. In consequence, a feeling of contrast having been declined in a mid-brightness range is obtained.
As described above, lowering the Gm electrode voltage brings about the effect of contrast enhancement. In this case, however, since the black level goes down, black sinks or a picture is darkened. To cope with this, it is possible to readjust the black level by lowering the cathode bias voltage as conventional brightness adjustment. Likewise, in the case of raising the Gm electrode voltage to obtain the effect of contrast decline, it is possible to readjust the black level by raising the cathode bias voltage.
As described above, the brightness adjustment through the control over the Gm electrode presents a novel image-quality-adjustment effect since brightness variation by this brightness adjustment involves contrast variation in a mid-brightness range.
FIG. 3 is a block diagram showing a structure of a second example of the CRT display apparatus according to the present invention. Here, the “CRT display apparatus” means a display apparatus using a CRT, such as a television set or a monitor display for a personal computer. In this figure, reference numerals identical to those in FIG. 1 represent the same elements. The second example differs from the first example in that the control signal is input into a G2 electrode voltage source 12 and not into the Gm electrode voltage source 10 . The G2 electrode voltage source 12 is configured to produce a voltage having a value in accordance with a value of the control signal input thereto.
As previously described, in a display apparatus having a conventional CRT, a coarse adjustment to a threshold point (cutoff point) with respect to the cathode voltage at which the screen starts to illuminate, which is called a screen adjustment, is carried out by adjusting a voltage applied to the G2 electrode. And, a fine adjustment to the cutoff point is carried out by adjusting a black bias voltage supplied to the cathode.
In a conventional CRT, when the voltage of the G2 electrode is raised, the potential difference between the cathode and the G2 electrode increases and thereby the beam current increases, but the black level as well goes up at this moment. As distinct from this, in the Hi-Gm tube, when the voltage of the G2 electrode is raised, the potential difference between the cathode and the G2 electrode increases and thereby the beam current increases as in the case of the conventional CRT. However, since the threshold point at which the electron beam starts to flow towards the screen causing the screen to illuminate is determined by the voltage applied to the Gm electrode, the black level remains unchanged as long as the rise of the G2 electrode voltage is not so large. As a result, in the Hi-Gm tube, when the voltage of the G2 electrode is increased, the beam current increases accordingly with the black level being kept constant, and therefore, the effect of contrast enhancement can be obtained.
Accordingly, in the display apparatus of the second example including the Hi-Gm tube having the above-described characteristics, contrast can be increased by increasing a dc voltage input as the control signal into the G2 electrode voltage source 12 to increase the voltage applied to the G2 electrode 4 . Likewise, it is possible to reduce contrast by reducing this dc voltage to reduce the voltage applied to the G2 electrode 4 . This control signal may be a voltage signal output from an output port of a microcomputer when a user presses a key to adjust brightness, viewing a user-adjustment menu which is generated by a character generator or the like and displayed on the monitor screen. This control signal may be generated by other means such as a hardware including a microcomputer and switches, or software-based processing.
In the display apparatus of the second example, it is also possible to increase brightness of a picture in part by inputting a rectangular-wave signal which increases in amplitude for a certain period of time as the control signal into the G2 electrode voltage source 12 . For example, it is possible to detect a low-brightness span from a video signal, and to increase the voltage applied to the G2 electrode for a period of time corresponding to this detected span, thereby increasing the brightness for that span. As described above, it is possible to boost a low-brightness span by controlling the G2 electrode voltage, which brings about an effect similar to gamma correction. Furthermore, when a picture includes a part to be displayed in high brightness such as a moving-image window, it is possible to superimpose a rectangular-wave signal on the G2 electrode voltage so that the G2 electrode voltage increases for that part and thereby the moving-image window is displayed in high brightness.
As previously described, in a conventional display apparatus, to adjust contrast, the gains of the three amplifiers for the three channels of R, G, and B have to be respectively controlled. As distinct from this, in the display apparatus of the second example, it is possible to adjust contrast by just controlling the voltage applied to the G2 electrode to control three electron beams of the three channels at once. Furthermore, in a conventional display apparatus, to achieve high-contrast display, expensive high-gain amplifiers and an expensive high-output-voltage power supply are required, whereas, in the second example, high-contrast display is achieved by a simple circuit without using such expensive amplifiers and an expensive power supply.
The above explained preferred embodiments are exemplary of the invention of the present application which is described solely by the claims appended below. It should be understood that modifications of the preferred embodiments may be made as would occur to one of skill in the art. | A display apparatus includes a CRT, the CRT including an electron gun having a cathode, a G1 electrode, a G2 electrode, and a G3 electrode disposed in that order to draw electrons from the cathode. The electron gun further has a modulating Gm electrode disposed between the G2 and G3 electrodes. The display apparatus is provided with a controller for controlling a value of a voltage applied to the Gm electrode to adjust brightness of a picture on a screen of the CRT. | 7 |
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation of PCT International Patent Application No. PCT/NL/02/00572, filed on Sep. 2, 2002, designating the United States of America, and published, in English, as PCT International Publication No. WO 03/017845 A1 on Mar. 6, 2003, the contents of the entirety of which is incorporated by this reference.
TECHNICAL FIELD
This invention relates to a method for generating hardness information of tissue subject to a varying pressure. In particular, the method relates to a method for generating hardness information of the wall of a blood vessel or body cavity.
BACKGROUND
Such a method is known from European patent application EP-A 0 908 137. In this application, the strain (deformation) of vessel walls is derived with ultrasound from the relative displacement of a more inward layer and a more outward layer of the vessel wall as a result of the pressure varying through the heartbeat. These relative displacements are (at an assumed equal speed of sound in the medium) equal to the difference of relative time delays of the ultrasound beam, measured at two times.
The relative time delay can be measured by correlating with each other sound signals obtained consecutively over time from one specific direction and deriving the relevant time delay from a correlation optimum. At this optimum, therefore, two signals consecutive over time are maximally correlated when the time difference between the respective signals is equal to the relevant time delay. By taking the difference of time delays measured at two different times and relating this to the time difference between the measuring times, it is possible to derive the degree of strain of the vessel wall in the direction of the sound beam as a result of pressure changes induced by the heartbeat.
By measuring the local relative displacements with a measuring beam in a specific direction and performing this measurement in a measuring plane oriented transversely to the vessel wall, it is possible to display elasticity information about respective measuring positions in the measuring plane. Furthermore, by measuring an average relative displacement along the above directions, a so-called palpogram can be composed, which is indicative of the hardness of the vessel wall in the plane in which the vessel wall cuts the measuring plane. The information derivable from such an elastogram/palpogram is important to identify and characterize plaques on the vessel walls. The composition of plaques can be important to the assessment of their injuriousness to health.
Such information is often not derivable from a conventional echogram, since the image of high-risk cannot be distinguished from less high-risk plaques.
Moreover, practical and theoretical studies show that the degree of strain of the vessel wall is indicative of the stresses that can occur in such plaques. If the stresses become too high, a plaque can tear open, so that a life-threatening thrombosis can arise.
Although for a two-dimensional cross-section, satisfactory measuring results can be obtained, in practice there appears to be a need for a three-dimensional display of the hardness information of the wall, so that the elasticity/hardness of at least one surface part of the vessel wall can be measured. With the present technique, it is practically very difficult to reproducibly analyze a blood vessel in such a manner. Furthermore, on the basis of conventional echographic data it is very hard to localize a suspect spot in a blood vessel. In fact, the performance of a single transverse scan at selected positions in a blood vessel provides insufficient information to enable determination of the presence or absence of plaques in the blood vessel as a whole.
DISCLOSURE OF THE INVENTION
The invention meets such needs and provides a method with which 3D information about the elasticity and/or hardness of a wall of a body cavity, in particular a blood vessel, can be obtained in a consistent and reproducible manner. In this regard, it is observed that with the present conventional technique the correlation between consecutive images is optimized by positioning the sensor as stably as possible, because movement of the sensor in general has a negative effect on the correlation. The invention is based on the insight that precisely by performing a motion transverse to the measuring plane a sufficient correlation between consecutive images can be maintained to enable detection of hardness and/or elasticity properties.
Accordingly, the method comprises the following steps of:
receiving signals from the tissue with a sensor for measuring the deformation of the tissue in a measuring plane defined by the sensor, which sensor, during a varying pressure exerted on the tissue, is moved along the tissue in a direction transverse to the measuring plane; identifying strain of the tissue from the resulting signals; and relating the strain to elasticity and/or hardness parameters of the tissue.
According to the invention, signals are received from, e.g., a vessel wall in a preferably almost continuous motion, consecutive (groups of) frames still having a sufficient correlation to enable distillation of the relevant information. This can be determined by means of a probability function indicating the relation between consecutive images. By controlling the motion (or feeding back feedback position) related to this probability function, an optimum palpogram quality is obtained, which can even be more favorable than in a stationary arrangement.
The method preferably comprises the step of displaying elasticity and/or hardness parameters of the tissue surface or tissue volume part extending practically parallel to the direction of motion of the sensor, if required, combined with position information of the sensor and/or the tissue. The deformation can be determined with an acoustic or optical sensor detecting echographic or optical data.
In a further preferred embodiment, signals possessing an optimum overlap are received. An optimum overlap can be determined by means of a probability function displaying the similarity between consecutive signals.
In the alternative or in addition thereto, at an assumed cyclic pressure change, signals can be received at predetermined time intervals in the period of the motion. In a preferred embodiment, these are signals of a blood vessel wall, the data being received only during a specific time interval of the period of the heartbeat. An advantage thereof is that signals that are not or less suitable for the determination of elasticity and/or hardness information of the tissue need not be stored, as a result of which data storage capacity can be performed to a limited extent, and the data processing can be significantly simplified.
The invention has a special use in case the tissue is an artery moving through the heartbeat in the longitudinal direction. In that case, the sensor can be moved practically parallel to this direction, so that during at least one detection period, the sensor is in a practically fixed position relative to the tissue. Practice shows that in particular in or near the heart, where relatively strong longitudinal motions of the artery occur, a strongly improved recording of hardness and/or elasticity properties, compared to the conventional recording technique, is obtained in a measuring plane transverse to the vessel wall.
The invention further relates to an apparatus for using the method according to the invention, comprising:
a sensor movable through a blood vessel or body cavity for recording signals from the tissue; a processor device for collecting and processing signals from the sensor to identify strain of the tissue and to relate the strain to elasticity and/or hardness parameters of a tissue surface or tissue volume part extending practically parallel to the direction of motion of the sensor; and a display device for displaying elasticity and/or hardness parameters of the tissue surface or tissue volume part.
In a preferred embodiment, the apparatus further comprises a position recording means coupled with the processor device to record sensor positions. The position recording means can display the 3D coordinates of the sensor relative to a fixed reference, e.g., by means of (electromagnetic) bearings, or in a simpler embodiment it may be a relative linear measure from, e.g., the point where a catheter is inserted or from a specific fixed location in a blood vessel.
In a mechanized use, the apparatus may be provided with an actuator for moving the sensor. Preferably, the actuator has an adjustable speed of motion. Position recording may thereby occur by means of measuring and/or adjusting the speed of motion of the sensor and/or the actuator.
In a further preferred embodiment, activating means are provided to activate data storage means for recording signals. Further activating means may be provided to activate the actuator. The activating means may be connected with an ECG recording device. In this manner, signals can be received from a blood vessel, the data being received only during a specific time interval of the period of the heartbeat. In the alternative or in addition thereto, the activating means may detect the correlation between consecutive echographic images and activate the data storage means at a the predetermined correlation.
In another further preferred embodiment, the sensor is arranged in a catheter, which can be inserted into a blood vessel, which sensor can record signals under controlled pullback of the catheter.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will further be explained on the basis of the description of the drawings, in which:
FIG. 1 is a diagrammatic representation of the apparatus according to the invention;
FIG. 2 a is a 3D palpogram of a phantom with a soft plaque part;
FIG. 2 b is a longitudinal section of the 3D palpogram of FIG. 2 a , combined with conventional echographic information;
FIG. 3 is a series of six 3D palpograms of a similar aorta part of a rabbit, obtained in six different measurements; and
FIG. 4 is a 3D palpogram of a human coronary artery, obtained in vivo.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is a diagrammatic representation of the apparatus 1 according to the invention. This apparatus comprises a movable catheter 2 provided with an acoustic sensor 3 . A processor 4 is present to collect and process echographic data; the processor 4 is connected with a display device 5 . The processor 4 is further in contact with a position recording means 6 for recording the position of the sensor 3 .
The catheter 2 can be moved through a blood vessel 7 , which blood vessel 7 has a vessel wall 8 deformed by the heartbeat. The deformation can be derived by the processor 4 from the echographic data of the catheter 2 and related to elasticity and/or hardness parameters of the wall 8 .
In explanation, a plaque 9 is shown in the blood vessel 7 . This plaque comprises a fat core 10 closed by a harder cap 11 . The motion of the catheter 2 is controlled by an actuator 12 . The actuator 12 has an adjustable speed of motion, such that the catheter can be moved at a speed of 0.1-2 mm/s. The preferred direction is a so-called pullback direction, i.e. the catheter 2 is inserted until a maximum insertion depth and is then pulled back by the actuator 12 . The actuator can pull the catheter 2 back in a practically continuous motion. The actuator 12 can be activated by the activating means 13 .
In the alternative, the activating means 13 can be controlled by data from an ECG device 14 , so that a favorable moment of the heartbeat can be selected to perform a measurement. This will be explained below in more detail. During the performance of the measurement, the motion can be interrupted, so that an intermittent pullback motion can be performed. The activating means 13 can also be coupled with a data storage means 15 for storing echographic data. This ensures that the extensive amount of echographic data is received only during a relevant part of the heartbeat, which results in a favorable capacity saving and significantly simplifies the data processing.
Besides through selection of a relevant part of the heartbeat for the performance of the palpographic measurement, the activating means can be connected, additionally or alternatively, with correlation-detection means 16 detecting the correlation between consecutive echographic images to become active at a predetermined correlation.
The method according to the invention will be explained below. At a varying pressure as a result of the heartbeat, echographic data are received by the acoustic sensor 3 , while the sensor 3 is moved along the vessel wall 8 . The echographic data can be analyzed by a processor 4 , strain of the vessel wall 8 being identified from the resulting echographic data; and the strain being related to elasticity and/or hardness parameters of the vessel wall 8 . In this manner, it is possible to display elasticity and/or hardness parameters of a tissue surface or tissue volume part extending practically parallel to the direction of motion of the sensor. In a preferred embodiment, in such a display, i.e., a palpogram or an elastogram of the vessel wall, the position information of the sensor and/or the tissue is displayed as well. The motion can be a practically continuous motion; in the alternative, an intermittent motion can be performed. The motion and/or the analysis of echographic data can be controlled, so that the echographic data are received at predetermined time intervals in the period of the heartbeat, at which time interval the motion may be interrupted.
In the alternative, only those signals possessing an overlap can be received. An optimum overlap can be determined by means of a probability function displaying the similarity between consecutive signals.
The palpogram of FIG. 2 a has been obtained by scanning a phantom with a soft inclusion, shown in cross-section by the echogram of FIG. 2 b . The phantom has the shape of a hollow tube and is made of polyvinyl alcohol cryogel. The inclusion comprises a harder cap, which may also be present in a naturally formed plaque. The thickness of the cap varies from 2 mm to 800 μm.
The inclusion thus has mechanical properties corresponding to those of a plaque that may be present in a natural blood vessel.
The phantom was kept under water and subjected to a pulsatile pressure. A catheter provided with an acoustic converter was moved through the phantom at a speed of 1.0 mm/s. The number of acquired frames was about 30 per second, i.e., an axial displacement of 0.03 mm per image. At a beam width of about 0.6 mm, this proved to be an acceptable amount.
In the soft part, a strain until 1% was observed. The strain increases with a decreasing thickness of the cap.
The palpograms of FIG. 3 have been obtained by scanning an artherosclerotic aorta of a New Zealand White rabbit at a pullback speed of 0.5 and 1 mm/s, respectively. In this Figure, a) is a first scan; b) is a second scan obtained after the catheter was positioned again; and c) is a scan obtained some time after, with the catheter again being inserted into the animal.
The palpograms have been obtained at a speed of motion of the catheter of 1.0 mm/s. In the palpograms, the plaque is always clearly visible as a lighter region.
In all cases, the following measuring method was used:
1. contour detection;
2. selection of frames with a minimum mutual motion;
3. estimating the displacement of the wall between two frames;
4. deriving the strain;
5. averaging the strain per angle;
6. (color) coding the strain at the contour.
Of three patients a palpogram was obtained; FIG. 4 shows an example thereof. The hatched regions do not represent available measuring values, as a result of the presence of a side branch of the aorta. As appears from the figure, the largest strain occurs in the regions around the side branch (light regions). It turned out that the motion of the catheter was slight enough to determine a reliable palpogram during a heartbeat. The degree of overlap between consecutive frames always remained at least about 70%.
In an experiment, a palpogram was obtained in which the data were divided into heart cycles, using the R-wave of the ECG signal. Because of the natural motion of the catheter through the varying speed of flow of the blood and the contraction of the heart, the catheter moves deeper into the coronary artery during the diastolic phase. Therefore, measurement is performed during this phase (i.e., a decreasing pressure of the heart and an increasing speed of flow), and the catheter is pulled out against the natural motion. This was done at a speed between 0.5 and 1.0 mm/s, by means of a mechanical actuator (Trakback, JoMed Imaging, Rancho Cordova, Calif., USA).
It turned out that through this motion the sensor, during the detection period, has a practically fixed position relative to the wall of the artery. It was found that the motion from the measuring plane is minimized, so that the quality of the palpogram is improved.
Although the invention has been discussed on the basis of the above-mentioned exemplary embodiment, in which the presence of plaques in a blood vessel was checked, it is clear that the invention can also be used when detecting and analyzing other tissues, such as (for cancer research of) the prostate, the esophagus etc. Instead of measuring deformations as a result of a naturally varying pressure, the apparatus can be provided with means for artificially exerting a pressure variation on the tissue.
Furthermore, all kinds of variations and modifications may be used without departing from the spirit of the invention. Such variations may, e.g., comprise the display of a 3D palpogram as a stack of 2D palpograms; the display of the angle at which measurement is performed; or a combination display of a palpogram and an angiogram.
Such and other variations are deemed to be within reach and the scope of protection of the appended claims. | A method for generating hardness information of tissue subject to a varying pressure. The method comprises receiving signals from the tissue from a sensor for measuring the deformation of the tissue in a measuring plane defined by the sensor, which sensor, during a varying pressure exerted on the tissue, is moved along the tissue in a direction transverse to the measuring plane; identifying strain of the tissue from the resulting signals; and relating the strain to elasticity and/or hardness parameters of the tissue. The method may comprise the step of displaying elasticity and/or hardness parameters of a tissue surface or tissue volume part extending practically parallel to the direction of motion of the sensor. | 0 |
BACKGROUND OF THE INVENTION
[0001] (1) Field of the Invention
[0002] The present invention relates to an image forming apparatus and an image forming method using it, and in particular relates to an image forming apparatus such as a copier, printer, facsimile machine and the like, which can be used with a limited, commercial power supply for small facilities, in an energy saving operation.
[0003] (2) Description of the Prior Art
[0004] Recently image forming apparatus equipped with a fuel cell using hydrogen and air have been proposed. Among these, there is a proposal of a configuration in which electric energy generated from a fuel cell is supplied to the drives and controller of the image forming apparatus and thermal energy arising from the fuel cell is used to heat the heating portion of the fixing unit (c.f. Japanese Patent Application Laid-open No. 2003-270980).
[0005] Typically, an image forming apparatus such as a copier, printer, facsimile machine and the like, includes drives for a photoreceptor, developing roller and the like, a controller for them and a thermal fixing unit for fixing the toner image onto plain paper, OHP sheets and the like. These drives, controller, fixing unit and the like should receive power supply from a commercial power supply to operate. Particularly, for heating the fixing unit its halogen heater and/or ceramic heater should be directly heated by commercial power supply; the commercial power supply is required to provide high electric power at a maximum of some thousand watt. For this reason, there have been cases that electromagnetic wave noise arises on the commercial power supply line, which often causes adverse influence on the controller and others.
[0006] Accordingly, as stated above it has been contemplated that electric energy obtained from a fuel cell is supplied to the drives and controller of the image forming apparatus so as to achieve stable operation as well as to lessen influences from noise arising on the power supply line and voltage drop, flickering and the like on the power supply line. It is also proposed that thermal energy arising at the fuel cell is supplied to the heating portion of the fixing unit (c.f. Japanese Patent Application Laid-open No. 2003-270980).
[0007] Incidentally, because of the surge of energy saving restraints, the system of the image forming apparatus itself has come to be reconsidered. For example, reduction of the consumption energy during periods of standby, which take up a high ratio of the operation of the image forming apparatus produces a large energy saving effect. For this reason, it is preferred that no power is supplied to the heating portion of the fixing unit when the image forming apparatus is unused. However, if no heating is effected to the heating portion of the fixing unit during periods of standby, it takes a long time while waiting for temperature rise of the heating portion when the apparatus is used again, resulting in poor user friendliness. On the other hand, in some recent configurations that support high-speed and high-volume continuous printing, there are cases where a safety control system is activated when insufficiency of power supply occurs at the fixing unit, and this interrupts printing halfway for the purpose of temperature recovery of the fixing unit.
[0008] In order to shorten the time for elevation in temperature of the heating portion, it is believed to be effective that the heat capacity of, not the heat roller as a heating portion of the fixing unit, but the whole fixing unit inclusive of the pressure roller should be reduced. It is also necessary to enlarge the input energy per unit time for heating the heating portion, that is, the electric power of the commercial power supply at the start. The former solution has a physical limitation. As the latter solution there has been a proposal that the time for elevating the temperature of the heating portion such as a heat roller etc., is shortened by using a power supply voltage of 200V.
[0009] In the typical offices in Japan, however the 200 V power supply is not, as yet, widespread, and a commercial power supply of 100 V with its upper current limit no higher than 15 A exists as the status quo. To deal with this situation, for the purpose of quick temperature rise of the heating portion, there has been a proposal of an image forming apparatus which employs two separate lines of commercial power supply of 100 V, 15 A, so as to increase the total power input to the heating portion of the fixing unit. However, this image forming apparatus needs to have more than one separate power outlet nearby. Whether the power supply is of a 100 V line or a 200 V line, the apparatus will be limited by power source capacity. In reference to the above conventional image forming apparatus equipped with a fuel cell, since electric energy from the fuel cell is not directly supplied to the fixing unit, it is not efficient enough to heat the fixing unit when it should be elevated in temperature. Accordingly, there has been demand for a configuration which can shorten the time for temperature rise of the heating portion in the fixing unit without the necessity of increase of usage wattage or amperage of the commercial power source to be used.
[0010] Conventionally, when a fuel cell equipped image forming apparatus is used, fuel (hydrogen, methanol, ethanol, dimethyl ether or the like) has been needed for the fuel cell, hence it has been necessary to provide a fuel storage tank in the image forming apparatus. In addition, maintenance for charging hydrogen or the like to the storage has also been needed. Further, use of a fuel cell involves formation of water or the like; these products, even though they are assumed to be discharged to the outside of the machine may increase the humidity around the image forming apparatus and degrade the environment.
SUMMARY OF THE INVENTION
[0011] In view of the above circumstances, it is an object of the present invention to provide an image forming apparatus which needs little consumption of energy during periods of standby and uses a fuel cell but does not need refueling. It is another object of the present invention to provide an image forming apparatus which, by making efficient use of commercial power supply, can shorten the time for temperature rise of the fixing unit without the necessity of enlarging the wattage of the commercial power supply and will not cause any power insufficiency and the like even in high-speed and high-volume printing.
[0012] In order to solve the above problems, the present inventors hereof constructed an image forming apparatus including a fuel cell and a fuel producing device for forming (producing) fuel for the fuel cell, and found that, by actuating the fuel producing device while the commercial power supply is not used for the electrophotographic process, it is possible to effect quick temperature rise of the fixing unit without increase of the wattage of commercial power source and supplying little consumption energy to the fixing unit during periods of standby, that it is possible to make refueling of the fuel cell or the like, maintenance free and that it is possible to obtain a further efficient combination of commercial power supply and a fuel cell, and thus has completed the present invention.
[0013] Illustratively, the present invention is characterized by the means or configuration described by the following features (1) to (13).
[0014] (1) An image forming apparatus, supplied from a commercial power supply and including a fuel cell, comprising: a fuel producing device for producing fuel for the fuel cell, characterized in that the fuel producing device produces fuel for the fuel cell making use of the commercial power supply.
[0015] (2) The image forming apparatus defined in the above (1), wherein the energy generated from the fuel cell is supplied as an auxiliary energy source for increase of the temperature or warmup of the fixing unit of the image forming apparatus and/or for high-speed printing.
[0016] (3) The image forming apparatus defined in the above (2), wherein the fuel of the fuel cell is hydrogen and the fuel producing device is made of a water electrolysis.
[0017] (4) The image forming apparatus defined in the above (2), wherein, in addition to the electric energy generated by the fuel cell, thermal energy arising from the fuel cell is used as the auxiliary energy source by way of a heat exchanger.
[0018] (5) The image forming apparatus defined in the above (3), wherein, in addition to the electric energy generated by the fuel cell, thermal energy arising from the fuel cell is used as the auxiliary energy source by way of a heat exchanger.
[0019] (6) The image forming apparatus defined in the above (3), wherein fuel transport lines between the fuel cell and the fuel producing device are constructed by an enclosed system.
[0020] (7) The image forming apparatus defined in the above (5), wherein the fuel cell, the fuel producing device and the lines between these are constructed by an enclosed circulating system.
[0021] (8) The image forming apparatus defined in the above (6), wherein the circulating system includes a pressure detecting means.
[0022] (9) The image forming apparatus defined in the above (3), wherein water arising at the fuel cell is collected by the fuel producing device and electrolyzed.
[0023] (10) The image forming apparatus defined in any one of the above (1) to (9), wherein the fuel cell is a solid polymer fuel cell using a polymer electrolyte membrane.
[0024] (11) An image forming method using an image forming apparatus comprising: a fuel cell; and a fuel producing device for producing fuel of the fuel cell, the fuel producing device producing fuel of the fuel cell by making use of a commercial power supply, characterized in that the fuel producing device produces fuel by utilizing the commercial power supply during periods other than that for heating the fixing unit of the image forming apparatus.
[0025] (12) The image forming method defined in the above (11), wherein energy generated from the fuel cell is supplied as an auxiliary energy source for increase of the temperature or warmup of the fixing unit of the image forming apparatus and/or for high-speed printing.
[0026] (13) The image forming method defined in the above (12), wherein, in addition to the electric energy generated by the fuel cell, thermal energy arising from the fuel cell is used as the auxiliary energy source by way of a heat exchanger.
[0027] According to the image forming apparatus and the method for using it, the image forming apparatus includes a fuel cell and a fuel producing device for it, so that it is no longer necessary to periodically recharge fuel for the fuel cell, such as hydrogen, methanol, ethanol, diethyl ether or the like. This simplifies maintenance. Water vapor is generally produced as a by-product from a fuel cell; there is a fear that production of water vapor might degrade the surrounding environment of the image forming apparatus. However, since an enclosed line that integrates the fuel cell and the fuel producing device can be created, it is possible to prevent degradation of the surrounding environment of the image forming apparatus. Further, application of electric energy from the fuel cell to the fixing unit in the electrophotographic process when the fixing unit is raised in temperature, makes it possible to quickly raise the temperature of the fixing unit without increase of the wattage of commercial power supply and without wasting power consumption during periods of standby. Further, there is no fear of printing stopping during high-speed printing due to temperature reduction of the fixing unit and for its recovery of temperature at a halfway point.
[0028] Moreover, when the fuel producing device is supplied with electric power from commercial power source while the electrophotographic process is not actuated or driven, it is possible to refuel the fuel cell during periods of standby.
BRIEF DESCRIPTION OF THE DRAWINGS
[0029] FIG. 1 is an illustrative schematic view showing an image forming apparatus according to the present invention.
[0030] FIG. 2 is a schematic view showing the relationship of lines between a fuel cell and a fuel producing device provided for an image forming apparatus according to the present invention.
[0031] FIG. 3 is a flowchart showing control timing at a fuel electric power supply controller.
DESCRIPTION OF THE INVENTION
[0032] The embodiment of the present invention will hereinafter be described in detail.
[0033] The image forming apparatus according to the present invention and the image forming method using it should not be limited to the embodied forms shown hereinbelow.
[0034] As shown in FIG. 1 , an image forming apparatus 1 includes a fuel cell 3 and a fuel producing device 4 other than an electrophotographic process unit 2 . Electrophotographic process unit 2 has a heat fixing unit 5 for fixing toner images to plain paper, OHP sheets and the like, further including, though unillustrated, a document reader, a photoreceptor, a developing roller, drives for these, a paper feeder, a printing portion, a discharge portion and the like. These drives, controller, fixing unit and the like are power supplied from a commercial power supply. Particularly, for heating fixing unit 5 , a halogen lamp and a ceramic heater are directly heated using the commercial power supply.
[0035] Fuel cell 3 has a hydrogen transport line 7 for letting in fuel and an oxygen transport line 8 for letting in oxygen (or air), and also has a discharge line (or water collection line) 9 for discharging water vapor. Discharge line 9 may be directly connected to a water storage 22 , or may be connected to water storage 22 by way of a heat exchanger 10 as in the present embodiment.
[0036] Heat exchanger 10 condenses water vapor from discharge line 9 and collects it and supplies the obtained thermal energy to heat fixing unit 5 . In this case, the heat medium is raised in temperature to 180 deg. C. or higher and is fed to fixing unit 5 .
[0037] Electric energy generated by fuel cell 3 is directly supplied to fixing unit 5 to heat it.
[0038] As shown in FIG. 2 , fuel producing device 4 is essentially an water electrolysis, which is housed by a casing 21 including water storage 22 and hydrogen storage 24 and oxygen storage 25 , defined by respective electrode caps 23 . The interior of casing 21 is adapted to communicate with discharge line 9 via a circulation pump 29 . Hydrogen transport line 7 and oxygen transport line 8 are inserted into casing 21 ; the hydrogen transport line is put in communication with hydrogen storage 24 in electrode cap 23 and oxygen line 8 is put in communication with oxygen storage 25 in the electrode cap.
[0039] In each electrode cap 23 , a hydrogen producing electrode (negative electrode) 26 or an oxygen producing electrode (positive electrode) 27 is arranged, and these electrodes are connected to a d.c. power source 11 shown in FIG. 1 . D.C. power source 11 is transferred from the commercial power supply and is controlled by a fuel electric power supply controller 14 . A pressure sensor (or pressure detector) 13 is arranged inside casing 21 ; pressure sensor 13 detects the pressure inside casing 21 or the pressure of oxygen and hydrogen produced therein and transmits the detected signal to fuel electric power supply controller 14 . A control valve 15 is arranged in each of the aforementioned hydrogen transport line 7 and oxygen transport line 8 . These control valves 15 are controlled by fuel electric power supply controller 14 .
[0040] Fuel cell 3 herein is a solid polymer fuel cell, and its anode pole 31 and cathode pole 33 are arranged opposing each other with an electrolyte membrane 32 in between. Anode pole 31 is formed of a conductive material that permits the fuel or hydrogen to spread therethrough, having a hydrogen diffusible layer 35 . Cathode pole 33 is formed of a conductive material that permits the oxidizer, or oxygen or air to spread therethrough, having an oxygen diffusible layer 36 . Polymer electrolyte membrane 32 is a proton conducting, or ion permeable, electrolyte membrane. A solid polymer electrolyte membrane or the like may be used; other than this, a solid electrolyte of a hetropoly acid such as molybdophosphoric acid, phosphotungstic acid or the like, being formed in a membrane structure, a matrix that is made up of an acid-resistant fine ceramic powder bounded by Teflon® and impregnated with an acid, and others may be used.
[0041] Hydrogen diffusible layer 35 is connected to hydrogen transport line 7 , and oxygen diffusible layer 36 is connected to oxygen transport line 8 . Water vapor is produced as a by-product from oxygen diffusible layer 36 and is collected by discharge line 9 . Accordingly, fuel cell 3 and fuel producing device 4 constitute a closed circulating line including circulating pump 29 , lines 7 , 8 and 9 .
[0042] Anode electrode 31 and cathode electrode 33 of fuel cell 3 are connected to a heat roller 37 of fixing unit 5 so that heat roller 37 can be quickly raised in temperature by electric energy from fuel cell 3 . The water vapor produced at fuel cell 3 is condensed by heat exchanger 10 (including a heat absorber 38 , compressor 39 and a heat discharger 40 ) as yielding and discharging thermal energy. The thermal energy arising at fuel cell 3 is transferred by the adjoining heat discharger 40 to heat the heat roller 37 .
[0043] In the thus constructed image forming apparatus 1 , as soon as image forming apparatus 1 is energized by power supply the switch of fuel electric power supply controller 14 is turned on, and fuel electric power supply controller 14 judges whether fuel cell 3 and fuel producing device 4 are ready to start warming up safely.
[0044] A shown in FIG. 3 , upon start, pressure sensor 13 measures the pressure in hydrogen storage 24 and oxygen storage 25 .
[0045] The pressure measurement data is input to fuel electric power supply controller 14 , which judges whether the pressure value is greater than the predetermined upper limit.
[0046] If the judgment is affirmative, or if the pressure value exceeds the predetermined upper limit, a warning indication is given.
[0047] In order to cancel the warning, control valves 15 of hydrogen transport line 7 and oxygen transport line 8 are released and compressor 39 and circulating pump 29 are turned on. Warning indication or the like is repeated until the pressure value from pressure sensor 13 is reduced to the predetermined upper limit or lower than the upper limit. When the pressure value becomes equal to or lower than the upper limit, warning is canceled and control valves 15 , compressor 39 and circulating pump 29 are turned off, then the operation returns to the main sequence.
[0048] Next, it is judged whether the pressure value is lower than the predetermined lower limit.
[0049] If the judgement is affirmative, it is judged whether fixing unit 5 is turned on or not. If the judgement is affirmative, the same loop of judgement is repeated until fixing unit 5 is off. When it is confirmed that fixing unit 5 is off and the judgement shows negative, electrolysis is started in fuel producing device 4 . Electrolysis is continued by repeating this loop during the state where the pressure value is lower than the predetermined lower limit. When the pressure value becomes equal to or greater than the lower limit, the operation returns to the main sequence.
[0050] It is judged whether warm-up can be started or not; if the judgment is negative, the operation is started again from the pressure measurement.
[0051] If it is determined that warm-up can be started, control valves 15 of hydrogen transport line 7 and oxygen transport line 8 are released, and compressor 39 and circulating pump 29 are turned on so as to make fuel cell 3 active. It is judged whether the predetermined period, n seconds, has elapsed from the start of generation of electricity at fuel cell 3 . After a lapse of n seconds, control valves 15 of hydrogen transport line 7 and oxygen transport line 8 are closed, and compressor 39 and circulating pump 29 are turned off so as to make fuel cell 3 inactive. Next, it is judged by pressure sensor 13 whether the pressure is normal. If the pressure is not normal, the operation returns to the start and repeats the above process until the pressure is normalized. When the pressure is normal, the apparatus is set into standby, and the operation is ended by turning off image forming apparatus 1 .
[0052] In this case, after the safety of fuel producing device 4 and fuel cell 3 is verified, electric energy from both the commercial power supply and fuel cell 3 is supplied to fixing unit 5 from the start of warm-up. Heat roller 37 of fixing unit 5 is able to reach the predetermined temperature for fusing and fixing after a lapse of the predetermined period or n seconds.
[0053] When, in standby of fuel producing device 4 and fuel cell 3 , a high-speed, high-volume continuous printing is started and heat roller 37 lowers in temperature, resulting in shortage of electric power for fixing unit 5 , fuel electric power supply controller 14 makes a call for canceling the standby mode and the operation returns to the start position. After the condition of the warm-up start of fuel cell 3 is checked, fuel cell 3 is reactivated; in this case, thermal energy from heat exchanger 10 provided for fuel cell 3 is also used, as required, to heat the heat roller 37 .
[0054] In the thus constructed image forming apparatus 1 , for increase of the temperature or warmup of heat roller 37 of fixing unit 5 for the electrophotographic process, it is possible to use not only commercial power supply but also the electric energy from fuel cell 3 . It is therefore possible to reduce the time for temperature rise of fixing unit 5 with a minimized wattage value of the commercial power supply. In addition, since electric energy from fuel cell 3 is also supplied to fixing unit 5 when a high-speed high-volume printing is implemented, it is possible to make stable control for heating fixing unit 5 . Therefore, printing can be done without break.
[0055] In the thus constructed image forming apparatus 1 , since fuel producing device 4 is provided together with fuel cell 3 , it is no longer necessary to periodically refill fuel to fuel cell 3 . Further, electrolysis for producing fuel to the full is effected during periods of standby. In standby, consumption of commercial power supply is inhibited to as low as possible. Execution of this electrolysis during the periods other than that for heating fixing unit 5 allows a margin for the electric power of commercial power supply, hence contributing to the operation of electrophotographic process 2 without hindrance.
[0056] Additionally, fuel cell 3 and fuel producing device 4 are constructed to form an enclosed circulating system. Limitation of an enclosed system is not a must, and it is also possible to conduct water and air other than the produced oxygen from the outside. However, formation of an enclosed circulating system made up of fuel cell 3 and fuel producing device 4 as in this embodiment makes it possible to collect resultant water vapor etc., as liquid water by way of the heat exchanger. Thus, this configuration prevents degradation of the environment inside and around the machine, i.e., increase in humidity, which would cause changes in the process conditions, image degradation, paper feed failure, paper jamming, water condensation in the optical system and the like, or environmental degradation in the office and other possible degradation. This also prevents oxygen concentration drop with no feed of air and hence can prevent discharge of unburned gas.
[0057] Further, provision of pressure sensor 13 allows for detection of abnormal increase in the pressure of the circulating system so as to stop generation of electricity by the fuel cell or electrolysis, whereby it is possible to prevent the fuel cell and fuel producing device from being accidentally broken due to excessive electrolysis, an abnormal temperature rise and others.
[0058] In the present embodiment, a solid poly fuel cell using a polymer electrolyte membrane is used for fuel cell 3 , but the present invention should not be limited to this kind of fuel cell. However, use of a solid polymer fuel cell for fuel cell 3 allows for its operation at normal temperature without the necessity of preheating over 100 deg. C., which would be needed for phosphoric acid fuel cells having an operational temperature of 150 to 300 deg. C. and other fuel cells, hence the solid polymer fuel cell is effective to provide auxiliary energy to the fixing unit.
[0059] Since the image forming apparatus and image forming method according to the present invention can be used with a commercial power supply for small facilities, in an energy saving operation, and since it is possible to deal sufficiently with high-speed high-volume printing, the present invention presents high industrial applicability. | The present invention provides an image forming apparatus, supplied from a commercial power supply and including a fuel cell, comprising: a fuel producing device for the fuel cell, in which the fuel producing device produces fuel for the fuel cell making use of the commercial power supply. This image forming apparatus needs little consumption of energy during periods of standby and does not need refueling even though it includes a fuel cell. Further, efficient use of commercial power supply makes it possible to shorten the time for temperature rise of the fixing unit without the necessity of increasing the wattage of the commercial power supply and avoid insufficient power supply even upon high-speed high-volume printing. | 8 |
TECHNICAL FIELD OF THE INVENTION
[0001] The present invention generally relates to vacuum pumps, and more specifically to the kind of device in which a plurality of vanes are fitted to slide substantially radially in a respective slot of a rotor eccentrically mounted within a casing.
DESCRIPTION OF RELATED ART AND BACKGROUND OF THE INVENTION
[0002] A previously known vacuum pump of such kind is illustrated in FIGS. 1 a - e. The pump includes a cylindrical-shaped casing or housing 10 which has an inner cylindrical wall surface 12 and is closed at its opposite ends by end walls 14 , 16 such as by means of machine screws 18 or the like. As shown, the pump includes circumferentially spaced fluid input 20 and output 22 ports intercommunicating the interior cavity. Output 22 is preferably held at atmospheric pressure, while input 20 is held at a vacuum of about 50 kPa during operation.
[0003] The rotor 24 of the pump is provided with a number of elongated vane slots 26 cut therein from the circumference thereof; and wherein a plurality of vanes 28 are mounted in freely slidable relation within these slots. A pump drive shaft 30 , provided with an axle spindle 32 for coupling, is keyed to the rotor 24 and is rotatably mounted in the end walls 14 , 16 as by means of bearings 32 , 34 . The rotor 24 is eccentrically mounted relative to the cylindrical inner wall 12 of the casing 10 . Accordingly, for efficient operation of a pump of this type, as the rotor turns within the casing it is required for the outboard edges of the vanes 28 to be in pressure-sealing contact with the inner surface 12 of the casing 10 while sliding in slots 26 back and forth; and that pressure losses around the longitudinal ends of vanes 28 and rotor 24 permitting escape of fluid to the exhaust, must also be prevented.
[0004] To such end, the pump comprises radial seals 35 , 36 between the rotor 24 and the end walls 14 , 16 , respectively, and also between the vanes 28 and the end walls 14 , 16 . The rotor is not axially locked, but is freely movable between the end walls, in order not to exhibit unacceptable losses caused by e.g. axial slackness of the ball bearings and manufacturing tolerances of the pump components. Due to such freely movable mounting, however, the pump is very sensitive to axial forces and in unfortunate situations such forces may lead to seizing of the pump. Additionally, such radial seals need large amounts of evenly distributed lubrication in order to work satisfactorily and very precise clearances 38 , 40 of the seals 35 and 36 , respectively, have to be provided and maintained irrespective of variations in the temperature of the pump. This may be hard to fulfill due to different length expansions of casing 10 and rotor 24 .
[0005] The latter problem has been addressed in the art. For instance, U.S. Pat. No. 2,312,655 issued to LAUCK discloses a rotary impeller type of vacuum pump, which provides for a precise clearance between the walls and the adjacent impeller assembly irrespective of the materials of the housing and of the impeller assembly. The pump includes the main housing of a light weight material, the impeller assembly of a heavier material, and an intermediate housing assembly, being composed of a thin sleeve member of a material having substantially the same characteristic temperature expansion as the heavier material of the impeller assembly, an axially adjustable end plate, and a plurality of coil springs. The thin sleeve member is arranged between the main housing and the impeller assembly and has a length slightly greater than the overall coaxial dimension of the impeller assembly by an amount exactly equal to the desired total clearance to be provided. The end plate is arranged to engage at the periphery thereof with the end of the sleeve member and urging the same into such engagement by means of the plurality of coil springs. In such manner the initially provided clearance is maintained irrespective of the differential temperature expansion between the housing and the impeller assembly.
[0006] U.S. Pat. No. 2,098,652 issued to BUCKBE discloses a similar type of vacuum pump provided with annular members arranged in spaces provided between the rotor-vane combination and the casing heads of the pump. These annular members are maintained pressed against the end surfaces of the rotor-vane combination by means of directing a suitable pressure fluid against the annular members, preferably between annular recesses of the annular members and the casing heads, such that they are forced to rotate with the rotating rotor-vane combination. The longitudinal dimensions are set such that there will always be a clearance between the rotating parts and the casing heads. Further, the annular members and the casing heads are provided with a number of interengaging annular ribs as a further means of preventing internal leakage.
[0007] However, such vacuum pumps comprise additional parts, which make them more complicated and costly to fabricate. Further, the former pump needs provision of a plurality of coil springs, and it does not provide for maintenance of the radial clearance if there are spatial temperature gradients, such as if the impeller was to be more heated than the sleeve member. The latter pump needs the provision of a pressure fluid and seals to prevent such pressurized fluid from leaking into the low pressure pump chamber. Additionally, there are extensive frictional movements between the vanes and the annular members, as these members are pressed against the vanes, while the vanes are sliding substantially radially within their respective slots continuously.
[0008] Further, U.S. Pat. No. 4,397,620 issued to INAGAKI et al. discloses a rotary compressor including disc-shaped members having a diameter slightly smaller than that of a rotor each disposed on opposite ends of the rotor and supported on the same rotary shaft as the rotor for rotation, and two disc-shaped recesses each formed on one of inner opposite end surfaces of a housing for receiving therein one of the rotary disc-shaped members. A small gap is formed between the inner end surfaces of the housing and the end surfaces of the rotor, and small gaps are formed between surfaces of the rotary disc-shaped members and surfaces of the disc-shaped recesses.
[0009] However, such pump is not suitable to be used with a coupling, which generates axial forces since the pump then may seize. Further, the pump may be noisy and the bearings used may be exposed to stress, and thus have a short lifetime. Also, it is doubtful if the pump may withstand its own weight, and maintain the radial gaps if mounted on a support which is not horizontal.
SUMMARY OF THE INVENTION
[0010] It is an object of the present invention to provide a vacuum pump of the rotary vane type, which is in lack of the problems discussed above in connection with vacuum pumps of the prior art.
[0011] It is yet a further object of the invention to provide such a vacuum pump that is efficient, simple, reliable, of low cost, and easy to manufacture.
[0012] It is still a further object of the invention to provide such a vacuum pump that allows for axial biasing of the rotor.
[0013] These objects among others are, according to the present invention, attained by vacuum pumps as claimed in the appended claims.
[0014] By providing the rotor and the end walls at oppositely facing surfaces, by annular recesses and annular ribs, respectively, wherein the ribs and the recesses are interengaging so as to define radial clearances and axial seals, respectively, between the end walls and the rotor, a pump is obtained, which provides for a clearance between the rotor and end walls irrespective of the materials thereof or any temperature gradients, while the pump is simple and reliable and has very few movable parts. Very same end walls may be used in a large variety of pumps having different pump capacities.
[0015] The rotor and the end walls may be provided with a plurality of annular recesses and ribs, respectively, such that axial labyrinth seals between the end walls the said rotor are obtained. In such manner any leakages occurring, are further reduced.
[0016] By axially biasing the rotor/drive shaft combination of the vacuum pump, preferably by means of axial stops provided in the end walls and a loaded spring, e.g. a cup spring, mounted between the rotor and the axial stops, a vacuum pump, which is insensitive to axial forces is obtained. In such instance, a plurality of different transmission systems or gearboxes may be used with the vacuum pump. Further, an axially biased pump is easier to manufacture, and the pump may be mounted upon a support, which is not horizontal.
[0017] Bearings, such as ball bearings, in which the rotor/drive shaft combination may be mounted at the end walls would have a longer lifetime, be less noisy and cause less vibrations, when being axially biased. Further, the radial and axial plays of the bearings would not affect the sealing properties of the inventive vacuum pump.
[0018] Further, by providing the end walls with a respective inner annular rib for axially guiding the vanes when sliding substantially radially within the slots of the rotor, it is prevented that vanes may move sideways and get stuck at the inner corners of the end walls. Additionally, each of the inner annular ribs may be provided with a respective through hole for lubrication of the vanes.
[0019] By providing a rotor wherein the longitudinally extending radial slots are at least partly, or completely, radially sealed at the longitudinal ends thereof, the internal leakage is even further reduced. Hereby, the casing and the end wall located at the motor side, may be an integrated single part.
[0020] Further characteristics of the invention and advantages thereof will be evident from the following detailed description of embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The present invention will become more fully understood from the detailed description of embodiments of the present invention given hereinbelow and the accompanying FIGS. 1 - 3 , which are given by way of illustration only, and thus are not limitative of the present invention.
[0022] [0022]FIG. 1 a is a front elevation view of a vacuum pump of the rotary vane type according to prior art.
[0023] [0023]FIG. 1 b is a sectional view along the line A-A of FIG. 1 a.
[0024] [0024]FIG. 1 c is a radial cross sectional view of the vacuum pump of FIG. 1 a.
[0025] [0025]FIG. 1 d displays, in a perspective view, a rotor as being comprised in the vacuum pump of FIG. 1 a.
[0026] [0026]FIG. 1 e displays, in a perspective view, a casing end wall as being comprised in the vacuum pump of FIG. 1 a.
[0027] [0027]FIG. 2 a is a front elevation view of a vacuum pump of the rotary vane type when its front-end wall is demounted according to a first embodiment of the present invention.
[0028] [0028]FIG. 2 b is a sectional view along the line B-B of FIG. 2 a.
[0029] [0029]FIG. 2 c is a radial cross sectional view of the vacuum pump embodiment of FIG. 2 a.
[0030] [0030]FIG. 2 d displays, in a perspective view, an inventive rotor as being comprised in the vacuum pump embodiment of FIG. 2 a.
[0031] [0031]FIG. 2 e displays, in a perspective view, an inventive casing end wall as being comprised in the vacuum pump embodiment of FIG. 2 a.
[0032] [0032]FIG. 3 a is a front elevation view of a vacuum pump of the rotary vane type when its front-end wall is demounted according to a second embodiment of the present invention.
[0033] [0033]FIG. 3 b is a sectional view along the line C-C of FIG. 3 a, in which also fragmentary enlarged scale views of encircled portions are shown.
[0034] [0034]FIG. 3 c is a radial cross sectional view of the vacuum pump embodiment of FIG. 3 a.
[0035] [0035]FIG. 3 d displays, in a perspective view, an inventive rotor as being comprised in the vacuum pump embodiment of FIG. 3 a.
[0036] [0036]FIG. 3 e displays, in a perspective view, an inventive casing end wall, and also a fragmentary enlarged scale view of an encircled portion thereof, as being comprised in the vacuum pump embodiment of FIG. 3 a.
DETAILED DESCRIPTION OF EMBODIMENTS
[0037] In the following description, for purposes of explanation and not limitation, specific details are set forth, such as particular techniques and applications in order to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known methods and apparatuses are omitted so as not to obscure the description of the present invention with unnecessary details.
[0038] The vacuum pump of the present invention is primarily intended to be used with equipment such as an automatic milking machine and other equipment present at a dairy farm. Nevertheless, the pump may be suitable for use in other fields, and as far as the present invention concerns there is no limitation whatsoever as to where the pump may find applications.
[0039] With reference to FIGS. 2 a - e a first exemplary embodiment of the vacuum pump of the present invention will be described.
[0040] The pump includes a cylindrical-shaped casing or casing 50 , which has an inner cylindrical wall surface 52 and is closed at its opposite ends by end walls 54 , 56 such as by means of machine screws 58 or the like, being received in holes 59 of end wall 54 and similar holes in the longitudinal end of casing 50 . Similarly, end wall 56 is mounted to the opposite end of casing 50 . As shown, end wall 56 is integrated in a larger detail 57 referred to as a motor axle casing to be mounted to a motor casing housing a motor for driving the pump. Further, casing 50 includes circumferentially spaced apart fluid inlet 60 and outlet 62 ports intercommunicating the interior cavity of the pump.
[0041] The rotor 64 of the machine is provided with a number of elongated vane slots 66 cut therein on the radius thereof, and within these slots are mounted in freely slidable relation therein a plurality of vanes 68 . The pump drive shaft 70 is press-fitted into the rotor 64 (or otherwise keyed thereto) and is rotatably mounted in the end walls 54 , 56 as by means of bearings 72 , 74 . In an alternative version the rotor and the pump drive shaft are fabricated as a single unit. The bearings are preferably slide fitted to the end walls 54 , 56 , and interference fitted to the rotor/drive shaft combination 64 , 70 .
[0042] The rotor 64 is concentrically mounted and positioned with respect to the axis of the drive shaft 70 as shown in FIG. 2d, but the shaft 70 is eccentrically mounted relative to the cylindrical inner wall 52 of the casing 50 . Accordingly, it will be understood that for efficient operation of a machine of this type, as the rotor turns within the casing it is required for the outboard edges of the vanes 68 to be at all times in pressure-sealing contact with the inner surface 52 of the casing 50 while reciprocatively sliding in the slots 66 ; and that pressure losses around the ends of the vanes permitting escape of fluid to the exhaust, has also to be prevented.
[0043] To attain the aforesaid objectives, end walls 54 , 56 are provided with annular recesses 84 , 86 and the rotor 64 is provided with annular ribs 88 , 90 at its respective end faces. Recess 84 and rib 88 are interengaging so as to define a radial clearance 92 and an axial seal 94 , respectively, between end wall 54 and rotor 64 . Similarly, recess 86 and rib 90 are interengaging so as to define a radial clearance 96 and an axial seal 98 , respectively, between end wall 56 and rotor 64 . It shall be appreciated in this respect that a radial clearance signifies a play between the rotor and the end walls, said play extending in the radial direction. Correspondingly, an axial seal signifies a thin slit or a gap between the rotor and the end walls, said thin slit or gap extending in the axial direction and operating as a seal between said parts.
[0044] The rotor/drive shaft combination 64 , 70 (joined in fixed relation or fabricated as a single piece) is axially biased by means of axial stops 110 , 102 , respectively, provided in the end walls 54 , 56 and a loaded spring, preferably a cup spring 104 , mounted between rotor 64 , or more precisely one of the bearings 74 , and the axial stop 102 of end wall 56 . In such manner the thermal expansion of rotor 64 is balanced by means of spring 104 in the direction of end wall 56 (i.e. on the motor side). Such axial biasing is very advantageous since it allows for the use of a coupling (not illustrated), which generates axial forces. Preferably then, the drive shaft 70 is provided with an axle spindle, to which the coupling is mounted, and via which the motor can drive the rotor/drive shaft combination 64 , 70 . Further, the use of axial biasing of the rotor/drive shaft combination 64 , 70 provides for a more silent-running pump with a longer lifetime.
[0045] End walls 54 , 56 comprise a respective inner annular rib or ring 106 , 108 for axially guiding the vanes 68 when sliding substantially radially within said slots. This guiding rib guides the vanes from their innermost position (e.g. at startup) towards their outermost position without allowing them to move sideways and thus to possibly get stuck in the end walls 54 , 56 . Annular ribs or rings 106 , 108 may further be provided with a respective through hole (not illustrated) for lubrication of the vanes.
[0046] The longitudinally extending radial slots 66 are in this embodiment preferably extending along the complete longitudinal extension of said rotor. The vanes 68 extend along the entire casing 50 and in this respect, an essentially radial sealing between vanes 68 and end walls 54 , 56 is provided as in the prior art device of FIG. 1. However, vanes 68 are preferably made of a plastic or other low friction material, such that very small clearances between vanes 68 and end walls 54 , 56 can be employed. The need of lubrication of the vanes may in such instances be dispensed with. Further, the material of vanes 68 is preferably chosen such that the thermal expansion of vanes 68 and of casing 50 , respectively, are comparable. Further, vanes 68 are easily exchangeable simply by demounting end wall 54 , drawing the vanes axially out of their respective slots, inserting new vanes, and finally remounting end wall 54 .
[0047] Further notably, slots 66 are arranged not entirely radially, but parallelly translated therefrom, to be oriented in a radial-tangential direction. Such design is intended to be included in the expression “substantially radially” as used within the present patent application. Accordingly, vanes 68 are sliding in a substantially radial direction.
[0048] Advantages of this particular embodiment of the invention comprise:
[0049] An axial sealing is not working as a sliding bearing, which indicates that no lubrication is needed between rotor and end walls.
[0050] The location for lubrication of the vanes may be freely selected. Hence, the material of the vanes as well as the type of lubrication may be more freely selected. Possibly, the pump may be driven entirely without lubrication.
[0051] The critical thermal expansion is now related to the diameter of the rotor and not to the length thereof. Thus, there are possibilities to manufacture pumps of longer lengths. Further, very same end walls may be used for both short and long vacuum pumps. Different material combinations for the casing, rotor, and end walls may be used with the risk of seizing reduced to a minimum.
[0052] The axial biasing of the rotor/drive shaft combination enables the use of a coupling, which generates axial forces.
[0053] The manufacturing will be easier due to less stringent tolerances.
[0054] The pump may be located on a surface, which is inclined with respect to the horizontal plane.
[0055] The axial biasing of the rotor/drive shaft combination will result in longer lifetimes of the ball bearings.
[0056] Further, the bearings will cause less noise and less vibrations. The kind of bearings is more freely chosable and any radial and/or axial play of the bearings does not affect the sealing between the rotor and the end walls.
[0057] In FIGS. 3 a - e a second exemplary embodiment of the present invention is shown. This second embodiment is similar to said second embodiment and all identical parts and features of the two embodiments are given identical reference numerals in the Figures. However, the second embodiment is differing from the first embodiment as regards the following.
[0058] End walls 54 ′ and 56 ′ are provided with respective first and second annular recesses 84 ′, 84 ″ and 86 ′, 86 ″, and rotor 64 ′ is provided with respective first and second annular ribs 88 ′, 88 ″ and 90 ′, 90 ″ at each of its longitudinal end faces. Thus, annular recesses 84 ′, 84 ″ and 86 ′, 86 ″ and ribs 88 ′, 88 ″ and 90 ′, 90 ″ are interengaging so as to define radial clearances 92 ′, 96 ′ and a plurality of axial seals 94 ′ 98 ′, respectively, between end walls 54 ′, 56 ′ and rotor 64 ′. Thus, axial labyrinth seals are provided, which may further reduce the internal leakages of the pump.
[0059] End wall 56 ′ is as in previous embodiment integrated in a motor axle casing 57 ′.
[0060] Annular ribs or rings 106 ′, 108 ′ as defined between respective annular recesses 84 ′, 84 ″ and 86 ′, 86 ″ are adapted to guide the vanes 68 axially when sliding substantially radially within the slots. Annular ribs or rings 106 ′, 108 ′ are further provided with a respective through hole (only through hole 110 in rib 106 ′ is illustrated, FIG. 3 e ) for lubrication of the vanes. Preferably, vanes 68 , fluid inlet port 60 , and through hole 110 for lubrication, are arranged circumferentially such that there are, at all times during operation, at least one of the vanes 68 located between fluid inlet port 60 and the through hole 110 for lubrication. Thus, as through hole 110 never will be in open communication with inlet port 60 the internal leakages are further reduced.
[0061] Furthermore, the longitudinally extending radial slots 66 are at least partly, but preferably completely, radially sealed 112 at the longitudinal ends thereof, e.g. by means of sealing rings 114 , 116 attached to the body of rotor 64 ′ by means of screws 118 or other fastening means. Such sealing rings may extend along the entire radial extension of slots 66 as illustrated, or they may extend only partly along the radial extension of slots 66 . Alternatively, the rotor 64 ′ is made as a single piece with integrated radial seals.
[0062] Particular advantages of this latter embodiment comprise:
[0063] The internal leakage is further reduced.
[0064] A larger play between end walls and vanes may thus be acceptable, which facilitates the choice of vane material.
[0065] A larger “smallest distance” between the eccentrically arranged rotor 64 ′ and the inner surface 52 of casing 50 may be acceptable. This would make it possible to manufacture end wall/motor axle casing 56 ′, 57 ′ and casing 50 integrated in a single piece.
[0066] Simpler manufacturing and logistics if tolerances are higher, fewer pieces are to be manufactured.
[0067] Simpler mounting if fewer pieces (integrated casing/end wall) are to be mounted.
[0068] No need of uniquely fastening end walls to casing by pins; the end walls are thus exchangeable.
[0069] Simple and even lubrication of the vanes, if at all necessary, through holes 110 provided in annular end wall ribs 106 ′, 108 ′.
[0070] It will be obvious that the invention may be varied in a plurality of ways. Such variations are not to be regarded as a departure from the scope of the invention. All such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the appended claims. | A vacuum pump of the rotary vane type, comprises a casing ( 50 ) having a cylindrical inner wall surface ( 52 ), a first ( 54; 54′ ) and a second ( 56; 56′ ) end wall at opposite sides of said casing defining a fluid cavity therein, fluid inlet ( 60 ) and outlet ( 62 ) ports in open communication with said fluid cavity, and a rotor ( 64; 64′ ) extending between said end walls carried by a drive shaft ( 70 ) for rotation about an axis eccentric to said casing inner wall surface, said rotor being provided with a plurality of longitudinally extending radial slots ( 66 ) about the periphery thereof. Further, there are provided a plurality of vanes ( 68 ), each being radially slidably carried within a respective of said slots. The invention comprises that at least one of said end walls and said rotor comprise, at oppositely facing surfaces, an annular recess ( 84, 86; 84′, 84″, 86′, 86″ ) and an annular rib ( 88, 90; 88′, 88″, 90′, 90″ ), respectively, said rib and recess being interengaging so as to define a radial clearance ( 92, 96; 92′, 96′ ) and an axial seal ( 94, 98; 94′, 98′ ), respectively, between said at least one of said end walls and said rotor, and that the rotor/drive shaft combination is axially biased. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a divisional of U.S. patent application Ser. No. 14/409,031 filed on Dec. 18, 2014, titled “II-VI BASED LIGHT EMITTING SEMICONDUCTOR DEVICE”, which is a §371 application of International Application No. PCT/IB2013/055235 filed on Jun. 28, 2013, which claims priority to U.S. Provisional Patent Application No. 61/739,165 filed on Dec. 19, 2012 and U.S. Provisional Patent Application No. 61/665,968 filed on Jun. 29, 2012. U.S. patent application Ser. No. 14/409,031, International Application No. PCT/IB2013/055325, U.S. Provisional Patent Application No. 61/739,165, and U.S. Provisional Patent Application No. 61/665,968 are incorporated herein.
FIELD OF THE INVENTION
[0002] The invention relates to a II-VI based light emitting semiconductor device, a luminescent material, a method for the production of such luminescent material, as well as to a method for the production of a II-VI semiconductor layer for such semiconductor device.
BACKGROUND OF THE INVENTION
[0003] Wide-band gap II-VI compounds are expected to be one of the most vital materials for high-performance optoelectronics devices such as light-emitting diodes (LEDs) and laser diodes (LDs) operating in the blue or ultraviolet spectral range. Thin films were commonly grown using the conventional vapor-phase epitaxy (VPE) method. With the development of science and technology, new and higher requirements arose for material preparation. For this reason, novel epitaxial growth techniques were developed, including hot-wall epitaxy (HWE), metal organic chemical vapor deposition (MOCVD), molecular-beam epitaxy (MBE), metal organic molecular-beam epitaxy (MOMBE) and atomic layer epitaxy (ALE). Using these growth methods, film thickness can be controlled and quality can be improved. Examples of II-VI semiconductors are ZnS, ZnO, ZnSe, ZnTe, and CdTe.
[0004] Zinc oxide semiconductor materials comprising zinc and oxygen as constituent elements have attracted considerable attention since they can emit not only blue light but also near ultraviolet rays of 400 nanometers or less because of their wide band gap similarly to semiconductor materials such as gallium nitride and the like. Further, their applications to photo detector, piezoelectric device, transparent conductive electrode, active device and the like have also been expected without being limited to light emitting device. To form such a zinc oxide semiconductor material, various methods such as MBE method using ultra-high vacuum, sputtering, vacuum evaporation, sol-gel process, MO-CVD method, and the like have been conventionally examined. With respect to the light emitting device, the MBE method using ultra-high vacuum is widely used from the viewpoint of crystallinity.
[0005] Further, U.S. Pat. No. 4,278,913 describes a zinc oxide-based phosphor emits yellow light of high luminance under excitation of low-velocity electrons: xMIIF2.yMIIIF3.ZnO wherein MII is at least one divalent metal selected from the group consisting of beryllium, magnesium, calcium, strontium, barium, zinc and tin, MIII is at least one trivalent metal selected from the group consisting of aluminum, gallium, indium, thallium, yttrium and antimony, and x and y are numbers satisfying the conditions of 0.0001≦x+y≦0.1, 0≦x and 0<y. The zinc oxide-based phosphor is used as a fluorescent screen of a low-velocity electron excited fluorescent display device.
SUMMARY OF THE INVENTION
[0006] Currently, the lighting world is in the middle of a transition from the incandescent bulbs and (compact) fluorescent lamps towards solid-state lighting, mostly provided by light emitting diodes (LEDs). The majority of the LEDs in market are based on gallium nitride (GaN). While GaN is an excellent emitter, it does suffer from several drawbacks. The main issue is the susceptibility to defects in the crystal lattice that are generally detrimental for the emissive properties of GaN layers. Yet, GaN is the most suitable III-V material for LED fabrication because is actually one of the more defect-tolerant III-V materials. In order to prevent emission loss, the defect concentration has to be kept low by growing the GaN layers epitaxially. Epitaxial growth however prevents fabrication of large area devices. Additionally, the GaN covered wafers are generally cut up into small parts (typically 1×1 mm) to ensure an acceptable yield in functional devices, and to ensure optimum use of materials, because of the fact that gallium is a relatively scarce and expensive element.
[0007] The requirement for small areas has several disadvantages. In order to have enough light output GaN LEDs are generally operated at high power densities leading to heating of the devices which decreases their efficiency and requires the use of heat dissipation mechanisms such as heat sinks. The high light output from a small area effectively makes them point sources, which makes it uncomfortable to look directly into when used for general lighting applications. In fact, high power LEDs are classified on par with lasers with respect to eye safety. Therefore, for lighting applications, some kind of light spreading and glare reduction is generally required. An approach to solve these issues is to have large light emitting surfaces that can be driven at much lower power densities. As mentioned above, a large-area GaN light source is currently impossible and does not exist.
[0008] One of the reasons for the vulnerability for defects in the GaN crystal lattice stems from the low exciton binding energy, which is below kT. This low value means that at room temperature, excitons are likely to split up in separate electrons and holes before they have a chance to radiatively recombine. The separated charge carriers are then trapped at defect sites, leading to non-radiative decay. Obviously, this process intensifies at the elevated temperatures that GaN LEDs are commonly operated at.
[0009] On the other side of the spectrum are organic LEDs (OLEDs) with an exciton binding energy of 0.5 eV, far larger than kT, enabling light emission from an essentially amorphous medium which makes large area lighting applications possible. OLEDs however require (expensive) encapsulation due to the reactive nature of the electrode materials used.
[0010] Zinc oxide has long been studied as a material that may have the best of both worlds. Like GaN, it is a wide band gap semiconductor (˜3.3 eV), but ZnO has a high exciton binding energy of 60 meV (2.4 times kT at room temperature). This value means that defects should be less detrimental to light emission, thereby enabling a switch from epitaxial growth methods towards cheaper, large area deposition techniques like sputtering that generally result in polycrystalline layers. Furthermore, ZnO is cheap, abundant and highly stable making it an attractive choice as a potential light emitting material in large area devices.
[0011] Zinc oxide can be applied using large area deposition techniques like sputtering, which generally results in polycrystalline layers. Furthermore, ZnO is cheap, abundant and highly stable, making it an attractive choice as a potential light emitting material in large area devices. However, despite these promises, ZnO has a few issues as a potential phosphor that have not been solved yet. Firstly, the main (near band gap) emission is in the UV (˜385 nm) and secondly the quantum efficiency of this emission is very low. Up to 3% efficiency has been reported from powder at room temperature, but generally lower values are observed.
[0012] A well-known additive is sulfur, which results in a strong, broad band emission from ZnO centered around 500 nm with a quantum efficiency of ˜50%. Although the preparation of highly luminescent ZnO:S powder is rather straightforward, the deposition of thin films of a similar composition is troublesome.
[0013] Therefore, there is an interest in additives for ZnO that improve the visible emission and quantum efficiency of the material, while being compatible with large area deposition techniques like sputtering. Hence, it is an aspect of the invention to provide an alternative (light emitting) semiconductor device, which preferably further at least partly obviates one or more of above-described drawbacks. It is further an aspect of the invention to provide an alternative luminescent material, which preferably further at least partly obviates one or more of above-described drawbacks. Further, it is an aspect to provide a method for the production of such luminescent material, especially in the form of a layer on a substrate that can be used as active layer in such alternative semiconductor device.
[0014] In a first aspect, the invention provides a light emitting semiconductor device comprising a stack, the stack comprising a cathode (which may especially be a cathode layer), a semiconductor layer comprising an emissive (oxidic) material having an emission in the range of 300-900 nm, an (oxidic) insulating layer, and an anode (which may especially be an anode layer), wherein the cathode is in electrical contact with the semiconductor layer, wherein the anode is in electrical contact with the insulating layer, such as a metal oxide layer, and wherein the insulating layer has a thickness in the range of up to 50 nm (i.e. >0 nm and ≦50 nm).
[0015] This approach is a realization of the diode by incorporation of an insulating layer in the device stack, i.e. metal-insulator-semiconductor-metal (MISM) diode. The cathode or anode can in principle be of any material that is suitable as cathode or anode material, respectively. Especially, at least one of cathode or anode is transmissive. In an embodiment, the cathode comprises ZnO doped with aluminium or indium tin oxide (ITO). Hence, in an embodiment, the cathode is transmissive. Herein, the term “transmissive” indicates that the layer is transmissive for emission of the active layer. In a further embodiment, the anode may be a noble metal, such as gold or platinum, or a combination thereof.
[0016] Suitable materials for the semiconductor layer may especially be an emissive material selected from the group consisting of oxides, sulfides or selenides of zinc or cadmium, such as zinc oxide, zinc magnesium oxide, zinc sulfide, zinc selenide, cadmium oxide, cadmium sulfide, and cadmium selenide, especially ZnO, (Zn,Mg)O, ZnS, ZnSe, CdO, CdS, CdSe. Further, also oxysulfides may be applied, like gadolinium oxy sulfide. Further, also doped version of these materials may be applied, like ZnO:Al, (Zn,Mg)O:Al, ZnO:Mn, (Zn,Mg)O:Mn, etc. Hence, in an embodiment, the emissive material is selected from the group consisting of ZnO, (Zn,Mg)O, ZnS, ZnSe, CdO, CdS, CdSe, and doped variants of any of these, (like ZnO:Al, (Zn,Mg)O:Al, ZnO:Mn, (Zn,Mg)O:Mn, etc.). Also other semi-conducting materials may be applied that show emission in the visible. Optionally, also tellurides, like ZnTe, might be applied.
[0017] Hence, in a specific embodiment, the semiconductor layer comprises an emissive material selected from the group consisting of zinc (magnesium) oxide and cadmium oxide. The semiconductor layer is herein also indicated as “active layer”. In an embodiment, the layer is a non-granular layer, such as a layer obtainable by CVD or sputtering (and annealing), or other techniques known in the art, such as described herein. However, in another embodiment, the layer comprises a particulate layer, such as a layer comprising semiconducting nanoparticles. In another embodiment, the layer comprises (semi conducting) quantum dots. The layer is especially a continuous layer, with a porosity of at maximum 5%.
[0018] The term “(oxidic) emissive material” indicates that the emissive material may be a metal oxide material, such as ZnO. However, the emissive layer may also comprise a sulphide or selenide emissive material, etc., see also above.
[0019] The semiconductor layer comprises an emissive material having an emission in the range of 300-900 nm, such as in the range of 300-800 nm, like 400-700 nm. Especially, the semiconductor layer has at least part of its emission in the visible part of the optical spectrum. Likewise, this may apply to the luminescent material as described below.
[0020] The term white light herein, is known to the person skilled in the art. It especially relates to light having a correlated color temperature (CCT) between about 2000 and 20.000 K, especially 2700-20.000 K, for general lighting especially in the range of about 2700 K and 6500 K, and for backlighting purposes especially in the range of about 7000 K and 20.000 K, and especially within about 15 SDCM (standard deviation of color matching) from the BBL (black body locus), especially within about 10 SDCM from the BBL, even more especially within about 5 SDCM from the BBL. The terms “violet light” or “violet emission” especially relates to light having a wavelength in the range of about 380-440 nm. The terms “blue light” or “blue emission” especially relates to light having a wavelength in the range of about 440-490 nm (including some violet and cyan hues). The terms “green light” or “green emission” especially relate to light having a wavelength in the range of about 490-560 nm. The terms “yellow light” or “yellow emission” especially relate to light having a wavelength in the range of about 560-590 nm. The terms “orange light” or “orange emission” especially relate to light having a wavelength in the range of about 590-620. The terms “red light” or “red emission” especially relate to light having a wavelength in the range of about 620-750 nm. The terms “visible” light or “visible emission” refer to light having a wavelength in the range of about 380-750 nm.
[0021] Specific embodiments of the active layer (material) are elucidated below, but first the insulating layer is discussed.
[0022] As indicated above, especially good results are obtained due to the presence of the (oxidic) insulating layer, which may also be indicated as barrier layer. The term “oxidic insulating layer” indicates that the barrier layer is a metal oxide layer. This layer may also comprise a plurality of layers, optionally of different metal oxides. The term “metal oxide” may also refer to a mixed metal oxide. This insulating layer should preferably not influence the optical properties of the active layer. In other words, the insulating layer should preferably not influence the emission position of the emission band of the active layer. Especially, the insulating layer or barrier layer does not substantially react with the active layer, also not during application of the insulating layer on the active layer or during application of the insulating layer on the active layer (“inverted structure”). Hence, it is highly desirable to have a blocking layer that is stable in air and does not intermix with the underlying active layer, such as ZnO phosphor layer (see below) upon annealing (see also below). A good candidate for such layer is ZrO, which is a stoichiometric oxide with very limited solubility in ZnO. Especially, the oxidic insulating layer is selected from the group consisting of SiO2, MgO, SrTiO3, ZrO2, HfO2, and Y2O3. In a further variant, the insulating layer is a high bandgap dielectrical material, such as with a bandgap of at least 5 eV, especially at least 5.5 eV. The insulating layer may also comprise a non-oxidic material.
[0023] It is further desired that the position of the valence band and conduction band of the insulating layer is positioned such that conduction band of the (material of the) insulating layer is higher than of the conduction band of the (material of the) active layer. Further, the position of the valence band of the (material of the) insulating layer may be in the vicinity of the valence band of the (material of the) active layer.
[0024] Especially, the emissive material has a conduction band at CBp eV and a valence band at VBp eV from the vacuum level, with CBp>VBp, wherein the barrier layer has a conduction band at CBb eV and a valence band at VBb eV from the vacuum level, with CBb>VBb, wherein CBb>CBp, especially wherein CBb≧CBp+0.25 eV. Further, in an embodiment especially VBb≦VBp+1.5 eV, even more especially VBb≦VBp+1 eV. The vacuum level at 0 V is taken as reference.
[0025] Vc and Vb usually have negative values. Therefore, when Vc>Vb this implies that that |Vc| is smaller than |Vb|. Such conditions may give best results in terms of efficiency of the device. For instance, a conduction band of the barrier layer that is too close to, or even below the conduction band of the active layer may lead to an inefficient light emission in comparison with a barrier layers as indicated above, because the barrier required for blocking electron transport in the active layer has been disappeared. Especially, CBb≧CBp+0.35 eV, even more especially, CBb≧CBp+0.5 eV. Further, as indicated above especially VBb≦VBp+1.5 eV, even more especially VBb≦VBp+1 eV.
[0026] To give an example, the emissive material (of the active layer) may have a conduction band at −4 eV and a valence band at −7 eV; hence CBp>VBp. Further, the barrier layer may e.g. have a conduction band at −3 eV and a valence band at e.g. −6 eV, or −8 eV. Hence, CBb>VBb. Further, also CBb≧CBp+0.25 eV and VBb≦VBp+1 eV apply.
[0027] Especially, the thickness of the insulating layer is within the tunneling limit. Hence, the insulating layer has a thickness which is especially equal to or smaller than 50 nm, such as equal to or smaller 30 nm, like especially in the range of 2-30 nm, like at least 4 nm.
[0028] Here, we present also a novel class of zinc oxide based phosphors with enhanced quantum efficiency and emission in the visible part of the spectrum, that are also amenable to robust, large area thin layer deposition techniques such as sputtering, and which may also be used as material for an active layer in above described device. The enhanced emission is achieved by incorporating both magnesium and a trace amount of aluminum, followed by annealing in a non-reducing atmosphere, especially in air. The enhanced emission does not seem to stem from either the Al or Mg themselves, but is attributed to radiating defects in the (modified) ZnO lattice, the nature and number of which are thought to be influenced by the additives. The presence of both Al and Mg seem to have a synergistic effect. These ZnO based materials are prospective candidates for the emissive layer in large area LEDs. The emissive layer is herein also indicated as “active layer”. The term “active layer” indicates that this layer in the semiconductor device will show the desired luminescence (emission), when the semiconductor device is driven under the right conditions. The layer is especially a thin film, such as having a thickness in the range of 50 nm-1000 nm (1 μm). The layer is especially a continuous layer, with a porosity of at maximum 5%.
[0029] In a further aspect, the invention provides a (light emitting) semiconductor device (herein also indicated as “device”) comprising a zinc oxide or zinc magnesium oxide based layer, especially a zinc magnesium oxide based layer, as active layer, wherein the zinc magnesium oxide based layer comprises (or especially consists of) an aluminum doped zinc magnesium oxide layer having 1-350 ppm Al. The zinc magnesium oxide of the aluminum doped zinc magnesium oxide layer is of the type ZnO; thus more precisely (Zn,Mg)O; i.e. especially a (Zn,Mg)O:Al layer is provided. Instead of, or in addition to the Al dopant, also other dopants may be applied, like Mn (manganese).
[0030] Especially, the invention provides a semiconductor device comprising a zinc magnesium oxide based layer as active layer, wherein the zinc magnesium oxide based layer comprises (even more especially consists of) an aluminum doped zinc magnesium oxide layer having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. The phrase “Zn1-xMgxO with 1-350 ppm Al” may also be, as known in the art, indicated as Zn1-xMgxO:Al (1-350 ppm). Here, the term “nominal composition” is applied, as the composition herein indicated relates to the composition as weighed in. Hence, the nominal composition might also be indicated as “(1-x)ZnO*xMgO with 1-350 ppm Al”.
[0031] It appears that a relative highly efficient active layer is provided, that has the desired properties in respect of efficiency and electrical resistance. Further, such layer may be produced relatively easy. Layers without Mg or without Al are less efficient. Further, layers having a higher Al content may have undesired conductive properties.
[0032] It seems that Mg (magnesium) may at least partly be built in the ZnO lattice (alternatively, one may say that MgO dissolves in the ZnO lattice). The amount of Mg in the nominal composition is indicated with x, which is especially in the range of 0<x≦0.3, and even more at maximum 0.2. In the range of 0.02<x≦0.2 best optical properties may be obtained. The intrinsic value for x may especially be 0.1-0.2, like about 0.15 for a layer, whereas for a poly crystalline material, the value for x may especially be 0.04 or lower. The intrinsic value refers to the x-value of the mixed oxide. The presence of Mg in the zinc oxide can be determined from XRD (x-ray diffraction), or SIMS, RBS or ICP/MS, see also below.
[0033] With respect to Al (aluminum), it seems that 1-350 ppm (parts per million) Al, especially 1-200 ppm, even more especially 1-100 ppm, give good optical properties and also does not lead to a high conductivity, which is not desired, and which may occur when high Al amounts are used. An amount of Al in the range of 2-100 ppm, such as 5-100 may be especially suitable, even more a range of 2-80 ppm, such as 2-70, such as 10-60 ppm, like 20-60 ppm, especially like 30-50 ppm can be used. In an embodiment, the aluminum content is at least 10 ppm. Aluminum may partly be present in the zinc magnesium oxide lattice as dopant. Al may replace Zn or Mg lattice positions or may form or occupy interstitial positions in the lattice. The presence of Al can be reflected in SIMS (Secondary Ion Mass Spectrometry) or RBS (Rutherford backscattering) of the material. Optionally also laser ablation with ICP/MS (Inductively Coupled Plasma Mass Spectrometry) can be used to detect the presence of Al. The ppm value of the dopant relates to the total molar amount of the system. Hence, 10 μmol Al in 1 mole Zn1-xMgxO:Al will lead to a value of 10 ppm Al, i.e. Zn1-xMgxO:Al (10 ppm).
[0034] Hence, in a specific embodiment the zinc magnesium oxide contains 5-100 ppm Al, wherein x is in the range of 0.02<x≦0.2 (nominal composition). Further, especially the sulfur content in the zinc magnesium oxide (based layer) is lower than 50 ppm. Higher sulfur contents may lead to systems that cannot easily form the desired composition of the layer. For semiconductor applications, the layer thickness of the aluminum doped zinc magnesium oxide layer may be in the range of 50-1000 nm, such as at least 100 nm. The way in which such active layers may be formed is further elucidated below.
[0035] A semiconductor device, with such aluminum doped zinc magnesium oxide layer active layer can advantageously be used to generate visible light, especially having a dominant wavelength in the wavelength range of 500-650 nm. The term dominant wavelength indicates that the emission intensity maximum is found within the indicated spectral region. Further, it appears that the aluminum doped zinc magnesium oxide layer having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3, can advantageously be used as active layer in a large area LED, the large area LED at least having a die area of at least 1 cm2.
[0036] The premise of ZnO is application in large area lighting due to the exciton binding energy of 60 meV being larger than kT. In III-V LEDs (such as GaN), the binding energy is smaller than kT. Hence, for a high photoluminescence efficiency non-radiative defects have to be avoided. Epitaxially grown thin films are required; the technology cannot be scaled up to large areas. In OLEDs however, the exciton binding energy is about 0.5 eV. Light can be generated in amorphous films that are fabricated by roll-to-roll processing. The challenge for OLEDs is cost price and encapsulation.
[0037] The large binding energy makes ZnO a defect tolerant host material. Epitaxial thin films are not needed; a high efficiency might be obtained with polycrystalline thin films deposited over large area. Numerous papers report light emission from polycrystalline oxide LEDs fabricated by various deposition methods. The present efficiency is low, but there is not necessarily a fundamental limitation. When the efficiency can be optimized it will pave the way for large area solid state lighting. The advantages are low-cost and environmentally stable diodes that can be fabricated over a large area with industrially established deposition techniques.
[0038] As may be known in the art, the ZnO-based layer may be sandwiched between electrodes of the semiconductor device. Further modification of the ZnO-based layer to provide the semiconductor device may also be included. For instance, optionally one or more electron or hole blocking layers may be applied. This may improve efficiency. One or more electron or hole blocking layers may be arranged at different positions within the stack.
[0039] Hence, in an embodiment, the invention provides a light emitting semiconductor device, wherein the semiconductor layer comprises aluminum doped zinc magnesium oxide layer having 1-350 ppm Al. Especially, the semiconductor layer has a nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3.
[0040] The stack especially comprises a cathode, a semiconductor layer comprising an emissive (oxidic) material, an (oxidic) insulating layer, and an anode (and a support). Optionally, between the support and the cathode or anode, one or more other (functional) layers may be present. Further, optionally between the cathode and the semiconductor layer one or more other functional layers may be present. Especially, between the semiconductor layer and the (oxidic) insulating layer (the barrier layer), and between the barrier layer and the anode, no further other layers are present. However, in addition to (or alternative to) the insulating layer between the semiconductor layer and the anode, one or more further (or other) other blocking layers may be present in the device stack that are not necessarily in contact with the anode (or cathode). However, the one at the anode is especially applied, to help and facilitate hole injection.
[0041] The invention also provides the (particulate) luminescent material per se, and thus not only as active (thin) layer in a semiconductor device. Hence, as indicated above, the invention also provides a luminescent material comprising zinc magnesium oxide doped with Al. The zinc magnesium oxide is of the type ZnO; hence, especially (Zn,Mg)O:Al is provided. Hence, the invention also provides a luminescent material comprising zinc magnesium oxide doped with Al having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. This may be a particulate or granular material. Preferred ranges with respect to Mg content and Al content are the same as indicated above for the aluminum doped zinc magnesium oxide layer. For instance, the zinc magnesium oxide (luminescent material) may contain 5-40 ppm Al, wherein x is in the range of 0.02<x≦0.2.
[0042] The fact that the nominal composition “Zn1-xMgxO” is applied does not exclude (small) non-stoichiometric variations, such as in the order of at maximum 5%. Further, this chemical nominal composition does not exclude the presence of other dopants than aluminum (and magnesium). For instance, also sulfur might be present. In an embodiment however, no sulfur is present.
[0043] The invention also provides a method for the production of the light emitting semiconductor device as described herein. Hence, in a further aspect the invention provides a method for producing a light emitting semiconductor device, the method comprising providing a support and forming a stack on the support, wherein the stack comprises a cathode, a semiconductor layer comprising an emissive material having an emission in the range of 300-900 nm, an (oxidic) insulating layer, and an anode, wherein the cathode is in electrical contact with the semiconductor layer, wherein the anode is in electrical contact with the insulating layer, and wherein the insulating layer has a thickness in the range of up to 50 nm. Such device may be made with conventional semiconductor production technologies, though formation of the semiconductor layer, i.e. the active layer, may especially be done via pulsed laser deposition (PLD) and radio frequency (RF) sputtering. Hence, in an embodiment the formation of the layer comprises a deposition technique selected from the group consisting of pulsed laser deposition (PLD) and radio frequency (RF) sputtering. Other techniques that may be used as well are e.g. atomic layer deposition (ALD), chemical vapor deposition (CVD) and its variants of CVD method such as metal-organic CVD (MOCVD) or plasma enhanced CVD (PECVD), hydrothermal growth, spray pyrolysis, etc.; in general, any physical and chemical evaporation technique may be applied. Likewise, this may apply for one or more of the other layers in the stack.
[0044] In an embodiment, the production comprises forming the cathode on the support, the semiconductor layer on the cathode, the (oxidic) insulating layer on the semiconductor layer, and the anode on the (oxidic) insulating layer, followed by annealing the stack, wherein annealing is performed at a temperature in the range of 400-1100° C. However, inverted building is also possible.
[0045] As indicated above, for the conduction band and valence band of the insulating layer especially applies CBb>CBp, especially CBb≧CBp+0.25 and/or VBb≦VBp+1.5 eV, even more especially VBb≦VBp+1 eV. CBb refers to the conduction band of the barrier; CBp refers to the conduction band of the active layer (phosphorescent layer); likewise, VBb refers to the valence band of the barrier and VBp refers to the valence band of the active layer. For instance, the (oxidic) insulating layer is selected from the group consisting of SiO2, MgO, SrTiO3, ZrO2, HfO2, and Y2O3. Suitable emissive materials are also defined above.
[0046] In a specific embodiment, the semiconductor layer (thus formed) has the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. In a further embodiment, the method comprises (a) providing a composition comprising Zn, Mg and Al having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3, optionally heat treating this composition at elevated temperatures, and (b) subsequently annealing the optionally heat treated composition to provide said aluminum doped zinc magnesium oxide.
[0047] As indicated above, the invention also provides a method for the production of an aluminum doped zinc magnesium oxide, such as described above. Hence, in a further aspect, the invention provides a method for the production of an aluminum doped zinc magnesium oxide, the method comprising (a) providing a composition comprising Zn, Mg and Al with having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3, optionally heat treating this composition at elevated temperatures, and (b) subsequently annealing the optionally heat treated composition to provide said aluminum doped zinc magnesium oxide.
[0048] Even more especially, the invention provides a method for the production of an aluminum doped zinc magnesium oxide having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. This may include a method to generate a (particulate) luminescent material, but this may also include a method to produce a thin layer on a substrate. Especially, the method comprises heat treating (especially under oxidative conditions) a composition comprising Zn, Mg and Al with a predetermined nominal composition at elevated temperatures, and subsequently annealing the heat treated composition to provide said aluminum doped zinc magnesium oxide. The phrase “a composition comprising Zn, Mg and Al” may especially refer to one or more compounds comprising Zn, Mg and/or Al, respectively. These may also be indicated as precursor(s), see below.
[0049] The term composition may in an embodiment relate to a combination of one or more precursors of the luminescent material, such as metal oxides, or metal salts, like nitrates, sulfates, chlorides, fluorides, bromides, hydroxides, carboxylates such as oxalates, etc. etc. Optionally also a sulfide (or even optionally a selenide and/or a telluride), such as zinc sulfide might be applied as precursor. Especially, one or more of a metal oxide, a nitrate, a chloride, a hydroxide, and a carboxylate (such as an oxalate) are applied. Combinations of two or more of such precursor types may also be applied. Due to the heat treatment, the aluminum doped zinc magnesium oxide may be formed, but especially the material may be formed during annealing. The heat treatment and annealing may in an embodiment be performed until at least a poly crystalline material is formed.
[0050] In another embodiment, the composition may be formed on a substrate. This may be done at elevated temperatures. For instance, the substrate may be heated. Hence, in a specific embodiment of the method, the method comprises forming an aluminum doped zinc magnesium oxide based layer having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3, the method comprising forming a layer comprising the composition comprising Zn, Mg and Al with the predetermined nominal composition on a substrate at elevated temperatures, and annealing the thus formed layer to provide the aluminum doped zinc magnesium oxide based layer. For such an embodiment, the formation of the layer comprises a deposition technique selected from the group consisting of pulsed laser deposition (PLD) and radio frequency (RF) sputtering. However, also other deposition techniques may be applied (see also above).
[0051] As target material, the oxides may be applied, or mixed oxides may be applied. Especially, as target material (crystalline) aluminum doped zinc magnesium oxide is applied. Hence, the method may especially comprise depositing of the layer of said zinc magnesium oxide on the substrate by pulsed laser deposition or RF sputtering of an aluminum doped zinc magnesium oxide having the nominal composition Zn1-xMgxO with 1-350 ppm Al (i.e. here target material), wherein x is in the range of 0<x≦0.3 (nominal composition). With pulsed laser deposition (PLD) and radio frequency (RF) sputtering, a layer may be deposited on the substrate, having the desired composition. In this way, a II-VI semiconductor layer for a semiconductor device may be produced.
[0052] The term “the predetermined nominal composition” especially relates to the fact that starting components or a composition are composed in such a way, that the ratio of the elements may lead to the desired composition of the end product, i.e. aluminum doped zinc magnesium oxide having the nominal composition Zn1-xMgxO with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. As indicated above, the values that can be derived from the formula “Zn1-xMgxO with 1-350 ppm Al” refers to the nominal composition that is weighed out, and which forms the zinc magnesium oxide. The formed material may in addition to the zinc magnesium oxide, also optionally comprise (remaining) MgO.
[0053] With respect to deposition (of the semiconductor layer; i.e. the active layer), the deposition is especially performed during a deposition time, wherein during at least part of the deposition time the substrate is maintained at a temperature of at least 450 C.° for RF sputtering or at least 500° C. for pulsed laser deposition. With the indicated techniques, layers may be grown at a rate of about 0.3-1 nm/s, such as 04-0.8 nm/s, like about 0.6 nm/s.
[0054] The (first) heat treatment is especially at a temperature of at least 450° C., although for the synthesis of the luminescent material, even a temperature of at least 900° C., such as at least 1100° C. may be chosen. For instance, in the case of the heat treatment to provide the luminescent material, the temperature may be in the range of 1000-1800° C. Thereafter, the material may be cooled down, ground (in case of a particulate material), and be subject to the annealing. In case of making the semiconductor layer, the (first) heat treatment will in general be at least 450° C., but not higher than 800° C. However, in yet another embodiment, deposition is done at a substrate at a lower temperature than 450° C. Optionally, the substrate may even be at room temperature. Especially, however, the substrate is at elevated temperatures, such as indicated above.
[0055] It appears that annealing in a reducing atmosphere does not give entirely desired results. Especially, annealing is performed in a neutral or oxidizing atmosphere. Especially, the method includes annealing in an oxidizing atmosphere. Further, the method may especially comprise annealing at a temperature of at least 900° C. for at least 30 min. For instance, the temperature may be in the range of 900-1800° C. Note that heat treatment and annealing are two different actions, which are in general separated by one or more other steps, such as including a cooling step. For the synthesis of a layer, the temperature maximum for the (first) heat treatment and the annealing may be limited to the temperature stability of the substrate and/or the reactivity of the substrate. In general, the temperature should not be higher than 1200° C., such as not higher than 1100° C. For powder synthesis, the annealing temperature may be above 1000° C., such as at least 1200° C.
[0056] The term “substantially” herein, such as in “substantially all emission” or in “substantially consists”, will be understood by the person skilled in the art. The term “substantially” may also include embodiments with “entirely”, “completely”, “all”, etc. Hence, in embodiments the adjective substantially may also be removed. Where applicable, the term “substantially” may also relate to 90% or higher, such as 95% or higher, especially 99% or higher, even more especially 99.5% or higher, including 100%. The term “comprise” includes also embodiments wherein the term “comprises” means “consists of”.
[0057] Furthermore, the terms first, second, third and the like in the description and in the claims, are used for distinguishing between similar elements and not necessarily for describing a sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances and that the embodiments of the invention described herein are capable of operation in other sequences than described or illustrated herein.
[0058] The devices herein are amongst others described during operation. As will be clear to the person skilled in the art, the invention is not limited to methods of operation or devices in operation. Hence, the phrase “II-VI based light emitting semiconductor device” is also directed to a device which is switched off, and which will in the switched off state not be light emitting. The semiconductor layer comprising an emissive material may especially comprise an n-type emissive material. Hence, the semiconductor layer may be an n-type semiconductor layer, such as n-ZnO or n-CdS, etc.
[0059] It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design many alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. Use of the verb “to comprise” and its conjugations does not exclude the presence of elements or steps other than those stated in a claim. The article “a” or “an” preceding an element does not exclude the presence of a plurality of such elements. The invention may be implemented by means of hardware comprising several distinct elements, and by means of a suitably programmed computer. In the device claim enumerating several means, several of these means may be embodied by one and the same item of hardware. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage.
[0060] The invention further applies to a device comprising one or more of the characterizing features described in the description and/or shown in the attached drawings. The invention further pertains to a method or process comprising one or more of the characterizing features described in the description and/or shown in the attached drawings.
[0061] The various aspects discussed in this patent can be combined in order to provide additional advantages. Furthermore, some of the features can form the basis for one or more divisional applications.
BRIEF DESCRIPTION OF THE DRAWINGS
[0062] Embodiments of the invention will now be described, by way of example only, with reference to the accompanying schematic drawings in which corresponding reference symbols indicate corresponding parts, and in which:
[0063] FIG. 1 depicts emission spectra of a number of luminescent materials; Normalized emission spectra of ZnO (a), ZnO:Al (10 ppm) (b), Zn0.9Mg0.1O (c), and Zn0.9Mg0.1O:Al (10 ppm) (d). All measured as powders sandwiched between quartz plates, excitation at 325 nm;
[0064] FIG. 2 depicts excitation spectra of a number of luminescent materials; Normalized excitation spectra of ZnO:Al (10 ppm) (b), Zn0.9Mg0.1O (c), and Zn0.9Mg0.1O: Al (10 ppm) (d); and
[0065] FIG. 3 a -3 b depict SEM graphs from a sputtered aluminum doped zinc magnesium oxide layer before (a) and after (b) annealing at 1100° C.
[0066] FIGS. 4 a and 4 b show PL (photoluminescence) spectra of sputtered Zn0.85Mg0.15O doped with 40 ppm Al (ZAM-40) deposited on sapphire ( 4 a ) and ITO-coated sapphire ( 4 b ). Films were deposited at room temperature, and were subsequently post annealed; a plurality of annealing temperatures were investigated; some temperatures are indicated to better understand the temperature trends;
[0067] FIG. 5 depicts photoluminescence EQE (external quantum efficiency) measurements as function of post deposition anneal temperature for ZAM-40 deposited on sapphire;
[0068] FIG. 6 shows a comparison of the PL spectra of ZAM-40/sapphire and ZAM-40/ITO/sapphire versus post-deposition anneals temperature;
[0069] FIGS. 7 a (left) and 7 b (right) show PL spectra of ZAM layer on ITO coated sapphire capped with ZrO layer of different thicknesses. FIG. 7 a has on the left axis the absolute irradiance in photons/cm2.nm); FIG. 7 b has on the y-axis the normalize photoluminescence (in arbitrary units); both have a wavelength scale (in nm) as x-axis;
[0070] FIG. 8 shows normalized PL spectra (in arbitrary units on the y-axis) of sapphire/ITO/ZAM layer (dot-dashed) capped with MgO (line) as function of the wavelength (in nm);
[0071] FIGS. 9 a (left), 9 b (right) schematically show an embodiment of the device layout of a (ZnO) diode; References I-VI respectively refer to the anode (I), such as Au and/or Pt, the barrier layer (II), such as a metal oxide, having a layer width of larger than 0 nm and e.g. equal or smaller than 30 nm, the active layer (III), such as (Zn.Mg)O:Al, the cathode (IV), such as ITO, electrode(s) (V), such as Pt electrodes, and a substrate (VI), such as sapphire, quartz or glass;
[0072] FIGS. 10 a (top), 10 b (bottom) show: FIG. 10 a (top) I-V characteristics of ITO/ZAM/MgO/Au diode; FIG. 10 b (bottom) electroluminescent spectra of the diodes driven at 10V and 50 mA. The peak shown with the arrow shows the presence of near-band edge emission (NBE) of ZnO indicating hole injection into ZAM layer; in FIG. 10 b , the curve with two peaks is the 10V/50 mA electroluminescent spectrum; the other curve is the PL spectrum (see e.g. FIG. 8 );
[0073] FIG. 11 shows EL spectra of ITO/ZAM/MoOx/Au; ZnO NBE again indicates the near-band edge emission (NBE) of ZnO; the curve that is higher at 500 nm but lower at 900 nm is the PL (thin film) spectrum; the other curve (with more fluctuation on the signal) is the 12.5 V EL spectrum;
[0074] FIGS. 12 a (top), 12 b (bottom) show I-V characteristics (top) and EL spectra taken at 10 V (bottom) of ZAM devices with a ZrO blocking layer; in FIG. 12 b , PL refers to photoluminescence, EL BA refers to electroluminescence before annealing and EL AA refers to electroluminescence after annealing;
[0075] FIG. 13 schematically shows an embodiment of energy band diagrams of the n-ZnO/SiOx/p-type Si diodes under thermal equilibrium (left) and positive bias at Si side (right).
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0076] For the compositions Zn(1-x)MgxO desired quantities of zinc oxide (5N purity, Aldrich) and magnesium oxide (FO Optipur, Merck) were weighed into a 100 ml beaker and mixed for 4 minutes at 1800 rpm using a speed mixer (Hauschild, type DAC 150 FVZ-K). The compositions were put into an aluminum oxide crucible and fired inside a chamber furnace in air for 8 hours at 1100° C. using a heating and cooling rate of 200° C./hour. After cooling down the powders were grinded using an agate mortar and pestle and fired once again at 1100° C.
[0077] For aluminum doped Zn(1-x)MgxO first a desired amount of aluminum nitrate nonahydrate (p.a., Merck) was dissolved in a small amount of deionized water and diluted with 200 ml ethanol. Next desired amounts of zinc oxide (5N purity, Aldrich) and magnesium oxide (FO Optipur, Merck) were added and the obtained suspension was dried using a rotary evaporator. The compositions were put into an aluminum oxide crucible and fired inside a chamber furnace in air for 8 hours at 1100° C. using a heating and cooling rate of 200° C./hour. After cooling down the powders were grinded using an agate mortar and pestle and fired once again at 1100° C. From the Zn0.9Mg0.10+10 ppm Al powder, targets suitable for sputtering and pulsed laser deposition (PLD) were prepared.
[0078] A number of 400 nm thin films were grown on epi-polished a-cut sapphire substrates by PLD and RF magnetron sputtering. The base pressure of the PLD system was 2×10-7 mbar. During the deposition the substrate temperature was between 25° C. and 550° C. and the partial oxygen pressure was 0.2 mbar. The RF magnetron sputtering system had a base pressure of 6×10−7 mbar and the used substrate conditions were either 25° C., 450° C. or 550° C. The gas flows during the sputtering process were resp. 78 and 2 sccm for Ar and O2, the total pressure was 0.038 mbar, RF power was 60 W.
[0079] The thin film composition was analyzed using x-ray fluorescence (XRF) and secondary ion mass spectrometry (SIMS). For optical analysis of the powders, they were sandwiched between Asahi quartz substrates (that were found to be non-luminescent with at the excitation wavelengths used) and the sides were sealed with a UV-transparent epoxy glue (Epo-Tek 305). UV/Vis spectra were measured on a Perkin Elmer Lambda-950 spectrometer, emission and excitation spectra on an Edinburgh FLS920 fluorescence spectrometer. Photoluminescence (PL) emission spectra were measured on a home-built setup consisting of a Ocean Optics QE65000 spectrometer operating at −20° C., with either a 25 mW 325 nm CW He—Cd laser or a Spectraphysics Explorer 349 nm Nd:YLF pulsed laser as excitation sources. The latter laser was operated at 2.5 kHz repetition rate with a pulse length of ˜5 ns. The power incident on the sample was tuned with a VBA-200 beam splitter from Jodon Laser combined with a set of neutral density filters. Emission was detected at 90° angle to the incident laser beam by collection with a collimating lens, passed through a long-pass filter to remove residual laser light and then focused into an optical fiber connected to the spectrometer. The sample was oriented at a 120° angle with respect to the incident beam to prevent the specular reflection of the laser beam from entering the collimating lens. Absolute external quantum efficiencies were determined using a 6″ integrating sphere from Labsphere (model RTC-060-SF) which was equipped with a center mount. The laser only spectrum was taken with the center mount rotated parallel to the beam, so that the beam did not touch the sample mount directly. For the sample measurement, the beam hit the sample at 10° C. rotated with respect to the normal of the sample surface, so that the specular reflection of the laser beam was kept inside the sphere. Spectrometer, optical fibers and integrating sphere were all calibrated with a LS-1-CAL calibration lamp from Ocean Optics, to enable absolute irradiance measurements. Cathodoluminescence (CL) was measured on a modified SEM. All optical characterizations were conducted at room temperature.
[0080] Normalized PL emission spectra of ZnO+10% Mg (curve c), ZnO:Al (10 ppm) (curve b) and Zn0.9Mg0.1+10 ppm Al (curve d) are shown in FIG. 1 . The PL from pure ZnO (curve a) is the typical near-band gap emission (NBE) at ˜385 nm, with a very shallow, broad emission in the visible that is generally attributed to (oxygen related) defects. For all the other samples the situation is reversed and the primary PL signal is a broad emission in the visible, centered around 500-600 nm, again attributed to defect emission. This visible emission is specifically not originating from direct luminescence of the dopants themselves. Some minor NBE signal is visible in the UV. It is especially noteworthy that the addition of only a small amount of Al (10 ppm) (curve b) changes the PL output completely from almost entirely NBE-emission to almost entirely defect emission, with the peak maxima remaining virtually unchanged from the host ZnO.
[0081] Some differences in the wavelength of maximum visible emission between the different powders are observed: 520 and 585 nm for Zn0.9Mg0.1O (curve c) and ZnO:Al (curve b), respectively, with the sample according to the invention being in the middle at 555 nm (curve d).
[0082] The excitation spectra of ZnO+10% MgO (curve c), ZnO:Al (10 ppm) (curve b) and Zn0.9Mg0.1+10 ppm Al (curve d) as measured with an Edinburgh fluorescence spectrometer are shown in FIG. 2 . The excitation spectrum of ZnO could not be measured due to the very low emission. It can be seen that the optimal excitation wavelength is about 385 nm for the non-Mg containing powder which coincides with the NBE emission of ZnO. The Mg containing samples have their optimal excitation wavelength at 350 nm, but in both cases a secondary peak is observed at 385 nm, which is especially high in the ZnO/Mg case. This secondary maximum is again indicative that the ZnO and MgO have not fully mixed.
[0083] Table I shows the results from absolute (external) quantum efficiency (EQE) measurements on ZnO powders with various amounts of Mg and/or Al, measured at 349 nm excitation. Absorption at this wavelength is typically about 85% of the incident light. The power of the laser was tuned so as to be in a regime where the emission varied linearly with the intensity. It is immediately clear that having none or only one of Mg and Al present in the powder results in only limited quantum efficiency. When both are present, a large increase in EQE is observed.
[0000]
TABLE I
External quantum efficiencies (%) of Zn(1 − x)Mg x O:Al
powders as a function of composition. Excitation with 349 nm laser.
% Mg
ppm Al
0
1
5
7.5
10
15
20
0
0.8
2.1
3.0
2.5
10
2.5
5.6
13.7 a
8.7
20
14.7
40
15.3
23.7
70
10.6
100
2.0
9.4
1000
1.1
8.0
a an earlier batch of powder, that was used to prepare the target for PLD and sputtering, was found to have an EQE of 9.8%.
[0084] The dependence on the Al content is intriguing. Only a tiny amount (˜10 ppm) is needed to increase the EQE of the ZnO/Mg powder, and adding (much) more has no substantial effect or may lead to other undesired properties, like a too large electric conductivity. Hence, an amount of at maximum 200 ppm, especially at maximum 100 ppm seems beneficial.
[0085] Normally for a phosphor at low activator content, the PL output increases linearly with doping content as the emission competes with non-radiative processes in the host lattice. This linearity generally remains until concentration quenching sets in, typically above a few percent dopant, as at such higher concentrations the dopant centers start to interact by processes like Auger recombination. The dependence on Mg content is also found to be non-linear.
[0086] From the Zn0.9Mg0.10+10 ppm Al 400 nm thin layers were deposited on sapphire substrates by PLD and RF sputtering. Analysis of the sputtered layers by XRF and SIMS showed the Mg and Al content to be 9.6% and 14 ppm respectively, so the concentration of both dopants is more or less preserved during the deposition process. X-ray analysis showed both deposition techniques to afford essentially epitaxial layers.
[0087] While the layers were deposited at elevated substrate temperatures (500° C. for PLD, 450° C. for sputtering), the PL of the as deposited layers was low. It was found that annealing of the samples was required to achieve maximum luminescence, as is shown for both types of deposition. The minimum temperature for maximum PL appears to be 900° C. for both samples, although there is a marked difference in the evolution of the PL as a function of anneal temperature for the two deposition techniques.
[0088] For the PLD sample, at 700° C. there appears to be an intermediate stage where 2 peaks are visible in the PL spectrum. After anneal at 900° C., the spectrum is more or less identical to that of the parent powder. Above 900° a slight apparent increase in PL output could still be observed. The sample itself however exhibited formation of a haze in the formerly transparent sample according to the invention layer. SEM showed this haze to be due to the presence of slightly larger ‘crystallites’ that have grown at elevated temperatures. Cracks were not observed. This haze affect is likely to lead to a more efficient outcoupling of the light normal to the plane of the sample according to the invention layer (where the PL emission is measured). The sputtered layers were found to remain clear upon annealing up to 1100° C. SEM pictures from a sputtered aluminum doped zinc magnesium oxide layer before (a) and after (b) annealing at 1100° C. are shown in FIG. 3 ( a and b , respectively).
[0089] In order to answer the question if annealing at higher than 900° really results in higher output or if the hazing effect clouds the issue, for both types of deposition techniques the absolute EQE as a function of anneal temperature was also determined. The results are listed in Table II, and indeed the EQE at 1000° C. anneal is slightly lower than at 900° C. (although the values are close to the detection limit). A similar anneal experiment was performed for Zn0.85Mg0.150+40 ppm Al where a similar trend was observed, as well as higher EQE values. The optimum temperature was found to be 950° C., in line with the data for Zn0.9Mg0.10+10 ppm Al.
[0090] Table II reflects systems wherein the layers have the nominal composition Zn0.9Mg0.1G:Al (10 ppm) and Zn0.85Mg0.15O:Al (40 ppm).
[0000]
TABLE II
Absolute EQE (at 349 nm excitation) for samples according
to the invention layer deposited on sapphire, versus anneal
temperature. Anneal performed in air for 30 minutes.
Absolute QE (%)
Absolute QE (%)
Zn 0.9 Mg 0.10 : Al
Zn 0.85 Mg 0.15 O: Al
(10 ppm)
(40 ppm Al)
Anneal Temperature (° C.)
(PLD)
(sputter)
500 (as deposited)
0.26
700
0.55
900
1.10
1.64
950
7.23
1000
0.97
6.13
1050
4.32
1100
0.9
1150
0.46
[0091] In the case of the sputtered layer, two things become apparent. Firstly, the wavelength of maximum emission is red shifted some 50 nm with respect to the parent powder emission. Secondly, upon annealing at increased temperatures, a second peak starts to appear at 480 nm. Upon further annealing, the 480 nm peak starts to disappear again and a slight blue shift of the main peak is observed. At the highest anneal temperature (1100° C.) the 480 nm peak is completely gone and the main peak has shifted to 550 nm. The resulting PL spectrum is completely identical to a powder sample according to the invention. It appears that sputtering results in different phases in the layer, and annealing at 1100° C. is gives best results.
[0092] Apart from the temperature, the effect of the annealing atmosphere was also checked. Identical samples of sample according to the invention on sapphire, deposited by deposition, were annealed in different atmospheres (neutral, reducing and oxidizing) for 1 hour at 650° C. Note that this lower temperature was dictated by the requirements of one of the electrode materials (ZnO+2% Al). The PL output was measured using the qualitative part of the setup as the EQE's were generally below the detection limit of the quantitative setup. As the outcoupling characteristics of the samples were similar, this still affords a good comparison of the emission. For most atmospheres, the maximum emission was observed at 610 nm. In several samples a shallow shoulder was observed at 790 nm that was especially visible in the vacuum annealed sample. The relative results of the PL output are listed in Table III, with the sample annealed for 1 hour in air set at 100%. The conductivities of the layers were also determined.
[0000]
TABLE III
relative PL output and conductivity of PLD samples according
to the invention-10 layers on sapphire, as a function of
the anneal atmosphere. Anneal done for 1 hour (unless stated
otherwise) at 650° C. and atmospheric pressure.
Relative photon
Sheet resistance
Anneal atmosphere
flux (%)
(MΩ/square)
As deposited (500° C.)
0.6
1E+5
Air (1 hour)
100.0
<1E+4
Air (64 hour)
96.8
3E+4
Argon
97.5
4E+1
Oxygen
64.1
3E+4
5% hydrogen in argon
1.1
8E+4
vacuum
42.3
1E+1
NH 3
6.7
1E+4
Nitrogen (dry)
83.8
1E+1
[0093] From Table III it is clear that ambient air affords the best performing samples for PL output. Upon annealing for prolonged periods of time in air, a slight decrease in performance is observed as well as a small redshift of the emission to about 630 nm. The ‘neutral’ atmospheres argon and nitrogen provided results similar to air. Vacuum and pure oxygen, had roughly half the output of the air sample, presumably by both influencing the (number of) oxygen vacancies in a non-ideal way. The reducing atmospheres (H2/Ar and NH3) had severely diminished output, presumably by removal of oxygen from the sample according to the invention layer.
[0094] The sheet resistance of the layers was generally high (10-100 GΩ/square) for all atmospheres barring the ‘neutral’, non-oxygen containing ones (vacuum, argon, nitrogen) where it was 3 orders lower.
[0095] Hence, a new type of zinc oxide based phosphors has been prepared by incorporating both MgO (e.g. up to 15%) and a trace (e.g. 10-40 ppm) of Al as dopants. These phosphor powders showed visible emission and an order of magnitude increase in quantum efficiency compared to ZnO with no or only one of Mg and Al present. The phosphors proved robust to thin layer deposition techniques such as PLD and RF sputtering. Annealing in air at elevated temperatures (up to 900-1100° C. depending on the deposition technique) was found to be very beneficial for integration of all the substituent materials in the thin layers and increase the photoluminescence. The enhanced emission in both powder and thin layer could not be attributed to direct emission of the additives, but is thought to stem from radiating defects in the ZnO lattice, most likely oxygen-related. Only band edge excitation was observed, which was further corroborated by CL, showing that these phosphors operate through energy absorption by the host material, followed by energy transfer to the radiant defect and subsequent emission, making these materials potential candidates for the emissive layer in large area LEDs.
[0096] Herein, we further present a generic solution toward achieving light-emission from devices that are made of thin-films of ZnMgO:Al phosphor sandwiched between two/or more layers. Functional ZnO LEDs are demonstrated, with EL spectra that match that of the ZnO phosphor.
[0097] For detailed preparation of emissive material, we refer to the above. Here a short explanation of the phosphor preparation is given. For aluminium doped Zn(1-x)MgxO first a desired amount of aluminium nitrate nonahydrate (p.a., Merck) was dissolved in a small amount of deionised water and diluted with 200 ml ethanol. Next desired amounts of zinc oxide (5N purity, Aldrich) and magnesium oxide (FO Optipur, Merck) were added and the obtained suspension was dried using a rotary evaporator. The compositions were put into an aluminium oxide crucible and fired inside a chamber furnace in air for 8 hours at 1100° C. using a heating and cooling rate of 200° C./hour. After cooling down the powders were grinded. After firing once again at 1100° C., targets suitable for sputtering and pulsed laser deposition (PLD) were prepared.
[0098] Thin films of ZnO phosphor were RF magnetron sputtered on a variety of substrates. Thin films of other metal oxides were either sputtered of physical vapor deposition. First 400 nm thin films of ZnO phosphor was grown on ITO coated epi-polished a-cut or c-cut sapphire substrates by PLD or RF magnetron sputtering. The base pressure of the PLD system was 2×10-7 mbar. During the deposition the substrate temperature was between 25° C. and 550° C. and the partial oxygen pressure was 0.2 mbar. The RF magnetron sputtering system had a base pressure of 6×10-7 mbar and the used substrate conditions were either 25° C., 450° C. or 550° C. The gas flows during the sputtering process were resp. 78 and 2 sccm for Ar and O2, respectively. The total pressure was 0.038 mbar, and the RF power was 60 W, and the bias voltage was around 250V. Next a layer of metal-oxide was deposited on to the phosphor layer and then metal contacts were deposited. Devices were annealed and then measured.
[0099] Photoluminescence (PL) emission spectra were measured as defined above.
[0100] Electrical measurements were conducted in a dark chamber at ambient. Light emission from the devices was recorded using a photo-diode. Current-voltage characteristics of the diodes were recorded using HP semiconductor analyzer. To record the EL spectrum of the LED, the Ocean Optics QE65000 spectrometer operating at −20° C. was used. The emitted light from the LED was fed into an optical fiber that was mounted on top of the emissive area and connected to the spectrometer.
Sputtered Thin Layers
[0101] The RF magnetron sputtering was used to sputter thin films of different variation of Zn0.90Mg0.10O (ZAM-10) and Zn0.85Mg0.15O. The phosphors used here were doped with Al in range of 0 to 100 ppm. The range of Al doping can be higher. The substrate temperature could be controlled during the deposition. Many phosphor compositions were made, measured and used in devices. Thin-film deposition conditions were varied, e.g. substrate temperature, from RT, to ˜500° C. Here we only present the results on the Zn0.85Mg0.15O doped with 40 ppm Al (ZAM-40) deposited at RT.
[0102] Thin film sputtering was conducted at a base pressure of 6×10-7 mbar. The substrate temperature during deposition was kept at room temperature. The RT substrate temperature was justified by our investigation that showed samples having different substrate deposition temperature have similar PL after annealing at T>550° C. Hence the choice of low substrate temperature is justified.
[0103] Sputtered films were prepared on Sapphire and ITO-coated Sapphire substrates. After deposition each substrate was subjected to annealing at one particular temperature. Thus no thermal histories were present for the samples. The annealing temperature was varied between RT up to 1150° C. for 30 min in ambient. After annealing samples were cooled down relatively slowly for 10-15 min in ambient air. Subsequently PL and EQE were measured. Later XRD and AFM were performed.
[0104] Primary results of the PL measurements are given in FIG. 4 a -4 b , where PL is measured as a function of post-annealing for RT sputtered thin film of Zn0.85Mg0.15O doped with 40 ppm Al, on the sapphire and ITO-coated sapphire substrates. Deposition of the phosphor layer at room temperature results in low PL emission as shown in the insets of FIG. 4 a -4 b . It is clear that post-annealing of the films have a profound influence on the PL spectra, as the emission enhances with increasing annealing temperature. However there is an optimum for the anneal temperature. It seems that there is an optimum annealing temperature is between 900-1000° C., where the PL response maximizes.
[0105] The optimum of post-anneal temperature for ZAM/sapphire was determined by EQE measurement of the different samples. The results of the EQE measurements as function of temperature, is given in FIG. 5 . It seems that the best annealing temperature for ZAM-40/sapphire is 950° C., where EQE exceeds 7.2%. EQE of the sputtered thin-film of ZAM-40 is almost a factor of 2 larger than that of the epitaxially grown GaN (4%).
[0106] In fabrication of the LED however the ZAM layer is deposited on to another layer of either metal or metal-oxide which acts as the electrode for charge injection into the device. Therefore PL response of the ZAM layer could be different. To this point ZAM-40 was deposited onto ITO-coated sapphire. PL spectra is given in FIG. 4 a . The only effect of the ITO seems to be red-shifting the defect emission peak of the ZAM-40 from 550 nm to >600 nm. The initial red-shift gradually decreases toward the original defect emission of ZAM-40 ( FIG. 4 a ) as the annealing temperature rises. At 900° C. however the shift of the defect emission peak toward lower wavelengths stops and PL abruptly changes. This abrupt change in the PL spectra has to do with the fact that ZAM-40 at temperatures higher than 900° C. start to form alloy with ITO hence changes the PL spectra. It is however of interest to see whether presence of ITO hampers the light emission from the ZAM-40 layer. To do so, we calculated photon flux emitted from ZAM-40 deposited on both sapphire and ITO-coated sapphire and compared both.
[0107] In FIG. 6 a comparison has been made for the photon flux (PF) of the ZAM on sapphire, and ITO/sapphire. Presence of the ITO does not compromise on the optical performance of the ZAM layer up to 800° C. At the same time this figure shows that annealing temperatures in the range of 400° C. to 800° C. have a very negligible influence on the PL emission of the ZAM. At 400° C. the phosphor is already activated. The lower performance of the ZAM/ITO/sapphire in compare to ZAM/sapphire, at temperatures higher than 800° C. is due to the degradation of the ITO and possibly formation of ZAM:ITO alloy. For ZAM/sapphire substrates, there is a rise in photon flux with a maximum at around 950° C.-1000° C., indicating the optimum annealing temperature. Surprisingly, light emission from both samples is the same and the best of phosphor activation is reached when ZAM is annealed up to 950° C.-1000° C. ITO however cannot withstand these high temperatures. Application of metals or conducting metal-oxide which can stand high annealing temperature would be advantageous in this respect, as it allows full activation of phosphor in real devices.
PL Spectra of ITO/ZAM/Insulating-Oxide Stack
[0108] The first question to be addressed here is whether deposition of an extra oxide layer would change the emission spectra of the ZAM layer. To do so, we sputtered ZAM onto the ITO-coated substrate. As a test model, we deposited 5 nm and 10 nm of ZrO onto the ZAM layer. The substrates were annealed at 600° C. for 30 min and slowly cooled down. The respective PL spectra of the samples are shown in FIG. 7 a -7 b . Clearly insertion of the ZrO layer does not change the PL spectra. The intensity however seemingly drops slightly in the presence of ZrO layer. Excluding all the experimental and instrumental errors, one possible reason will be less light out-coupling when an extra ZrO oxide layer is incorporated onto the stack.
[0109] To further investigate whether the top insulating layer influences the PL of the ZAM layer, we deposited MgO layer onto the ZAM layer and subsequently annealed the stack at 800° C. FIG. 8 shows the PL spectra of the ZAM layer capped with MgO layer in comparison with a bare ZAM. Clearly there is no influence of the insulating MgO layer on the PL of the phosphor even after annealing at 800. Incorporation of an insulating layer into the diode stack therefore has no influence on the PL spectra of the emissive ZAM layer. In fabrication of the diodes we therefore tried different insulating metal oxides such as, MgO, MoOx, V2O5, NiOx and ZrO. Experiments with SiO 2 (SiOx) and other oxides were also conducted, and similar results were obtained.
Fabrication of ZnO LEDs
[0110] Here, a diode is realized by incorporation of an insulating layer in the device stack, i.e. metal-insulator-semiconductor-metal (MISM) diode. Typical diode layout is shown in FIGS. 9 a -9 b . However, other configurations may also be possible (including an inverted structure).
[0111] In the following we present the data obtained for MISM ZnO diode fabricated with the sputtered thin films of Zn0.75Mg0.15O doped with 40 ppm Al. We used different substrates, e.g. sapphire, quartz and glass. Here only the results of devices fabricated on sapphire substrate are presented. The operation mechanism of the diode is discussed in the later section.
[0112] As cathode we used both Al doped ZnO and ITO both sputtered onto the substrate. We note that any metal, or transparent conductive metal-oxide can be used as cathode. ZnO:Al however is advantageous as it provides a good template for ZAM growth. In most of our experiments we used ITO as cathode. Thermal annealing at temperatures ˜600° C. was performed to activate the phosphor. Sputtered ITO on glass did show very little degradation in sheet conductivity upon annealing up to 750° C. Conductivity varied from 30 at RT to 75 Ω/square for ITO annealed at 750° C. Glass however, is not stable at T>700° C. Therefore we used either ITO coated sapphire or ITO coated quartz as substrate for ZAM growth and device fabrication.
[0113] In the next step we introduced the Pt pad on the ITO-coated sapphire with shadow mask evaporation followed by ZAM deposition. We note that it in our experiments the Pt-cathode pads were masked from the ZAM layer. We do not expect however significant differences if the Pt-contact pads are in touch with the ZAM layer. In the next step either a combination of metal contacts e.g. Ni/Au, or a combination of metal-oxide/metal contacts were introduced as anode. Later annealing of the device was performed to activate the phosphor and to form the contact.
[0114] We note that annealing of the devices is another crucial step in device fabrication. In order to fabricate reproducible device, first the contacts were deposited and then annealed at the desired temperature. Subsequent slow cooling down process of the substrate to RT is vital. Rapid cooling of the sample or deposition of contact after annealing, both resulted in devices with symmetric I-V characteristics and no light emission.
[0115] Here we present the results obtained with magnesium oxide (MgO), molybdenum oxide (MoOx), vanadium oxide (V2O5) and zirconium oxide (ZrO). We note that the same results were obtained with other insulating blocking layers in combination with different anodes. Moreover ZnO LEDs with the MISM layout can also be fabricated in an inverted structure. An example would be ZAM deposited onto p-type Si with a few nm thick SiOx oxide layer.
Electrical Characterization of ZnO LEDs
[0116] In this section we present electrical characteristics of MISM ZnO diodes. Current-voltage characteristics and electroluminescent spectra for sapphire/ITO/ZAM/MgO/Au diode are given in FIGS. 10 a -10 b . The I-V characteristic of the device, measured in dark, shows that the diode is rectifying. The rectification ratio however is not large due to the leakage current. The primary target here is demonstration of a functional diode and electroluminescence. A photo-detector (photo-diode) was placed over the ZnO diode to record the light emission of the device. In dark we measured light with the photo diode. The power dissipated in the ZnO LED was less than 0.5 W, hence just not enough to record a measurable black body radiation. We measured the electroluminescent of the ZnO LED in forward bias of 10 V. The current running through device was 50 mA. An EL spectrum of the device is given in FIG. 8 . The PL spectrum of the ZAM is also presented as a reference.
[0117] FIGS. 10 a -10 b show nice matching of the EL spectrum of the ZnO LED with the PL of the ZAM thin film. It is really intriguing to note that the EL shows a peak at 358-360 nm. This EL peak is exactly at the position where near-band edge emission of the ZnO in thin films of ZAM takes place. Moreover the peak at 670 nm also nicely matches with the emission of the ZAM phosphor. Presence of 358-360 peak unambiguously demonstrate that hole injection is achieved with the MISM structure. The MISM device layout is therefore viable to overcome the challenge that has impeding arriving at ZnO LED for more than 60 years. To further prove that the MISM concept is generic for ZnO LEDs, in the next step we used MoOx as a blocking layer. The device layout therefore was sapphire/ITO/ZAM/MoOx/Au.
[0118] In FIG. 11 . we have only presented the EL spectra of the device. El was measured at 12.5 V and a good spectral match between the PL of ZnO thin film and EL is achieved. Once again, presence of the near-band edge emission in the EL spectra indicates successful achievement of hole injection into the valance band of the ZnO.
[0119] It is highly desirable to have a blocking layer that first, is stable in air, and second, does not intermixes with the underlying ZnO phosphor layer upon annealing. A good candidate for such layer is ZrO, which is a stoichiometric oxide with very limited solubility in ZnO. ZnO diodes were fabricated with ZrO blocking layer. The device stack was sapphire/ITO/ZAM/ZrO/Au. ZrO layer was sputtered from Zr target in an oxidizing atmosphere. FIGS. 12 a -12 b . show the I-V characteristics and EL spectra of the respective ZnO diodes. The diodes show an excellent rectification behavior as well as decent light emission. The power dissipated in the diode was ˜50 mW. The emitted light therefore cannot be infra-red emission due to heat dissipation, as shown by the EL spectra of the device. EL spectra were recorded before and after annealing of the diode. Before annealing, EL shows a peak at 900 nm, and it is not due to heat dissipation. Upon annealing, several peaks appear in the EL spectra of the device, with the first peak being at ˜650 nm. In comparison with the PL spectra of the thin-film with ZrO layer on top, it seems that the main emission peak at 600 nm is red shifted. Moreover the near band edge emission peak of the ZAM layer is not present in the EL spectra. Additionally few other peaks are present in the EL. We believe that sputtering of the ZrO layer on to ZAM has caused damages at the ZAM/ZrO interface. Due to soft bombardments of the ZAM interface, shallow diffusion of the Zr or ZrO into the ZAM layer could potentially change the EL spectrum by causing more surface recombination, which is manifested by appearance of the new peaks. Physical vapour deposition of ZrO (and potentially all the blocking layers) onto the ZAM layer is therefore recommended for having good spectral match.
[0120] The EL-spectra presented here are among the first EL spectra reported for ZnO LEDs. The I-V characteristics and EL spectra achieved for the ZnO LEDs demonstrate the viability of the MISM device layout.
Light-Emission Mechanism of ZnO LEDs
[0121] A tentative mechanism is presented in FIG. 13 for the MISM stack with highly p-type doped Si as the anode and SiOx as the blocking contact. Similar mechanism is at work when p-type Si is replaced with a metal electrode as anode.
[0122] The energy band diagrams of the diode at equilibrium and under bias are shown. When positive forward bias is applied on the anode, here p-type Si, the bands of Si near the Si/SiOx interface will bend upward. The band bending at the Si/SiOx interface will gradually induce an inversion layer for n-ZnO/SiOx/p-Si diodes, which is responsible for the hole injection. As a result, accumulated holes in the inversion layer could tunnel through the barrier into the valence band of ZnO and recombine with the electrons in ZnO conduction band that are blocked by the SiOx interface layer, resulting in UV emission of 359 nm as well as the visible emission at 600 nm.
[0123] A zinc oxide light emitting diode based on a newly developed zinc oxide phosphors has been demonstrated. These phosphor thin film showed visible emission. The phosphors proved robust to thin layer deposition techniques such as PLD and RF sputtering. Annealing in air at elevated temperatures (400-1100° C.) was favorable to increase the photoluminescence and initiate the electroluminescence. To fabricate ZnO LED we used a blocking layer between the anode and the emissive layer. The blocking layer impedes the electron to arrive at the anode from the ZnO layer. Accumulation of the electron enhances hole injection and hence the LED begin the light emission.
[0124] The recorded electroluminescence and the photoluminescence spectra of the ZnO thin film and ZnO LED match nicely. Interestingly even band gap emission of the ZnO is present in the EL spectra, which indicates that hole injection has been successfully achieved by incorporation of the blocking layer. The enhanced emission in ZnO thin layer could not be attributed to direct emission of the additives, but is thought to stem from radiating defects in the ZnO lattice, most likely oxygen-related. Only band edge excitation was observed, which was further corroborated by CL, showing that these phosphors operate through energy absorption by the host material, followed by energy transfer to the radiant defect and subsequent emission. The combination of the material and device presented here makes ZnO phosphors an attractive potential candidate for the large area LEDs.
[0125] As insulating layers, SiO2, MgO and ZrO were tried, and they all worked. | The invention provides a light emitting semiconductor device comprising a zinc magnesium oxide based layer as active layer, wherein the zinc magnesium oxide based layer comprises an aluminum doped zinc magnesium oxide layer having the nominal composition Zn 1-x Mg x O with 1-350 ppm Al, wherein x is in the range of 0<x≦0.3. The invention further provides a method for the production of such aluminum doped zinc magnesium oxide, the method comprising heat treating a composition comprising Zn, Mg and Al with a predetermined composition at elevated temperatures, and subsequently annealing the heat treated composition to provide said aluminum doped zinc magnesium oxide. | 7 |
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 60/511,004 filed Oct. 14, 2003.
FIELD OF THE INVENTION
[0002] The present invention relates to improvements in hub units for vehicles and more specifically to a novel asymmetric bearing arrangement for rotatably supporting a wheel of a vehicle.
BACKGROUND OF THE INVENTION
[0003] Hub units for vehicle wheels are not new per se. Typical of the prior are units are shown in patents such as the OSHIAKI, U.S. Pat. No.: 6,036,371 for ROLLING BEARING UNIT FOR VEHICLE WHEEL issued Mar. 14, 2000 and the Evans, U.S. Pat. No.: 4,333,695 for ROLLING BEARING issued Jan. 8, 1982. As shown in these patents, the hub units typically comprise a generally cylindrical hub having a radially outwardly directed flange for mounting to a wheel of a vehicle via a series of circumferentially spaced bolt holes accommodating lugs or studs for supporting the wheel. A pair of axially spaced rows of bearings support the wheel for rotation between an outer ring having internal raceways for the rolling elements. In the Yoshiaki '371 patent, the bearing support comprises a row of balls and a row of tapered rollers.
[0004] Even though these hub assemblies are generally satisfactory for the intended purpose, the present invention is an improvement in hub assemblies of this general type and is characterized by novel features of construction and arrangement providing functional advantages over the prior art such as a more balanced load distribution on the bearings and what is termed a “stiffer” hub reducing bending moments particularly beneficial in cornering maneuvers.
SUMMARY OF THE INVENTION
[0005] The present invention provides an asymmetric unit wherein the diameter of the pitch circle of the bearing in the outboard row adjacent the radial flange of the hub is of a greater diameter than the diameter of the pitch circle of the bearing at the inboard end. In a preferred embodiment of the invention, the inner and outer rows of the bearings are angular contact ball bearings and the diameter of the row at the outboard or wheel end is preferably at least five mm greater than the diameter of the pitch circle of the row at the inner suspension end. By this arrangement the distance between the pressure centers where the contact angle of the two bearing rows intercept the axis of the hub can be maximized to provide high camber stiffness. Further the outboard row preferably intercepts the hub axis outboard of the hub flange which balances the loads on the system more evenly between the inner and outer bearing rows. Additionally, by reason of the asymmetric design, the outboard row can accommodate more balls and thereby increase the capacity of the bearing without changing the package geometry. With this design, the outboard pressure center can be placed further outboard than a symmetrical unit without having to increase the contact angle and reducing bearing radial dynamic capacity.
[0006] In other words, comparing the symmetrical ball units of the prior art with the asymmetrical unit of the present invention, the asymmetric arrangement provides more capacity without impacting the knuckle or axial flange geometry. Thus bearing designers can utilize ball bearings in applications which would normally require tapered bearings thus providing an economy without jeopardizing performance.
[0007] As noted above, increasing hub stiffness by the asymmetric design improves noise and vibration harshness, enhances steering accuracy and vehicle dynamic behavior and also improves brake wear due to true running of the rotors.
[0008] With the enhanced stiffness of the asymmetrical design, the hub unit can accommodate large diameter wheels which apply a heavier bending moment on the hubs. The asymmetric designs allows wheel size increases without any changes in the hub design.
[0009] In summary, the present invention improves hub flange strength and increases robustness and enhances safety of hubs.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] These and other objects of the present invention and the various features and details of the operation and construction thereof are hereinafter more fully set forth with reference to the accompanying drawings, wherein;
[0011] FIG. 1 . is a transverse sectional view of an asymmetric hub assembly in accordance with the present invention;
[0012] FIG. 2 . is a transverse sectional view of another embodiment of asymmetric hub assembly in accordance with the present invention;
[0013] FIG. 3 . is a transverse sectional view of an asymmetric hub in accordance with the present invention showing balancing the loads and a reduction in the radial load component on the outer row as compared to the prior art symmetric arrangement;
[0014] FIG. 4 . is a free body diagram comparing load distribution for symmetric prior art system and the asymmetric hub assembly of the present invention; and
[0015] FIG. 5 . is a free body diagram comparing bending moment of asymmetric hub design of the present invention verses prior art asymmetric systems.
DESCRIPTION OF PREFERRED EMBODIMENTS
[0016] Referring now to the drawings and particularly to FIG. 1 thereof, there is shown an asymmetric hub assembly in accordance with the present invention generally designated by the numeral ( 10 ). The hub assembly ( 10 ) includes an elongated hub ( 12 ) having a splined center opening running axially of the hub ( 12 ) and having at its outboard or wheel end a circumferentially extending radially outwardly directed flange ( 16 ) having a series of circumferentially spaced holes ( 18 ) to mount a wheel of a vehicle by means of studs ( 20 ).
[0017] The hub assembly ( 10 ) has an outboard and an inboard row of the ball bearings, Ro, Ri which ride on outer raceways ( 22 ), ( 24 ) of an outer ring ( 26 ). The inner raceway ( 28 ) for the outboard row Ro is formed integrally with the hub ( 12 ) and the inner raceway ( 30 ) for the inboard row of ball bearings Ri is formed on a annular insert ( 32 ) held in place after assembly of the balls in the two rows Ro, Ri by a circumferentially extending lip ( 34 ) at the inner axial end of the hub ( 12 ). Conventional seals S are provided at the opposing axial ends of the annular space between the hub ( 12 ) and the outer ring ( 26 ). Further, the outer ring ( 26 ) has means ( 27 ) at its inboard or suspension end for securing it to a frame or steering mechanism of a vehicle. A sensor ( 38 ) is also mounted in the outer ring ( 26 ) which confronts a sensing ring ( 40 ) on the hub to measure speed of rotation in the conventional way.
[0018] The present invention is characterized by novel features of construction and arrangement providing an asymmetric bearing which has functional advantages over the prior art. To this end, the diameter D of the pitch circle of the outboard row of balls Ro is preferably greater than the diameter Di of the pitch circle of the inboard row of balls Ri. The difference in the diameters Do, Di is preferably at least five (5) mm. Further, the contact angle α of the bearings intersect the rotational axis A-A of the hub at points defined herein as pressure centers Po, Pi. The pressure centers Po, Pi lie outside the flange ( 16 ) at the outboard end of the hub assembly and at the inboard end as well to provide enhanced performance such as higher load carrying capability and better distribution of the load on the bearings Ro, Ri.
[0019] FIG. 3 illustrates how road forces act on the pressure centers Po, Pi of an angular contact ball hub unit in accordance with the present invention to provide improved load distribution on the bearings Ro, Ri and also to reduce the bending moment arm on the outboard flange ( 16 ) of the assembly.
[0020] As illustrated in FIG. 3 , for a bearing arrangement wherein the pitch diameters of the inner and outer rows Ri, Ro are the same the load force Fr from the road tire interface is acting outboard of the geometric center B-B of the bearing. Accordingly, the distance from the point of application of the force Fr at the bearing axis A-A to the outboard pressure center Po is a shorter distance than the distance to the inboard pressure center Pi and therefore the magnitude of the vertical force Fv 2 acting on the outboard row of the outboard bearing Ro will be larger than that of the inboard force Fv 1 based on a simple beam theory. By increasing the pitch circle diameter Do of the outboard bearing Ro without changing the contact angle ∝ as illustrated in FIG. 3 , the distance to the force Fv 3 is increased thereby producing a reduction of the magnitude of this force. Increasing the outboard pitch circle diameter Do provides more room or space between each of the balls so that the diameter increase of the outboard row of balls Ro produces a two fold improvement in life expectancy on the outer row Ro and additional load carrying capacity by more rolling elements and a more balanced load distribution between the bearings Ro, Ri. In most instances, the overall geometry of the assembly is not impacted by increasing the pitch diameter Do of the outboard row Ro of rolling elements since there is more radial space on the outboard side of the bearing than on the inboard side mainly due to the knuckle and brake geometry.
[0021] FIG. 5 is a free body diagram showing effect of the lateral road force Fa under cornering conditions on the bending moment acting on the hub assembly. As can be seen in FIG. 5 , the moment arm L 1 of a symmetric arrangement is greater than the moment arm L 2 of the asymmetric arrangement and by reason of this difference, the moments about A which is a product of Fa x L 1 is greater than the moment about B which is Fa x L 2 . Therefore, by reason of the moment arm differential, the effective moment on the symmetric is higher and thus the hub flange will yield more and adversely effect the “stiffness” of the hub assembly.
[0022] A modified embodiment of asymmetric hub assembly in accordance with the present invention is shown in FIG. 2 . The hub assembly generally designated by the numeral 10 a is the same in terms of components except in this instance, the inboard bearing Ri is a tapered roller bearing and is used in applications where the predominant load is radial this arrangement can be used where an existing taper roller bearing needs to be replaced without having to change the knuckle diameter.
[0023] The invention provides improved performance in predominantly radial load conditions such as in heavy truck applications which typically utilize tapered rollers. The bearings incorporate the same offset relationship of the inner and outer rows Ri, Ro as described above and the intersection of the contact angle α is preferably outward of the axial end of the hub. The preferred asymmetric design utilizing balls in the outboard row Ro provides hub stiffness and structural strength improvement without sacrificing load carrying capacity.
[0024] As noted above, in the symmetric design, the magnitude of the vertical force acting on the outboard row designated F v2 is larger than the force F v1 on the inboard side which lowers life expectancy of the outboard row Ro. By increasing the pitch circle diameter to produce an asymmetric design, the beneficial effects are many fold even without a change of the contact angle α. As illustrated in FIG. 3 , the magnitude of the force is reduced (F v3 ), more room is created to accommodate more balls further improving life expectancy and producing further force reduction F y4 .
[0025] In summary, benefits of the asymmetric design include high camber stiffness providing improved brake wear, better driving precision, optimized bearing capacity and life expectancy.
[0026] Even though particular embodiments of the present invention have been illustrated and described herein, it is not intended to limit the invention and changes and modifications may be made therein within the scope of the following claims. | A hub bearing assembly comprising a hub having a radially outwardly directed flange at one axial end for mounting the wheel of a vehicle, an outer ring having axially spaced raceways and a plurality of rolling elements arranged in two rows in the annular space between the outer ring and the hub, the diameter of the pitch circle of the outboard row of rolling elements adjacent said flange being greater than the diameter of the pitch circle of the rolling elements in the inboard row. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable
RELATED CO-PENDING U.S. PATENT APPLICATIONS
[0002] The following related U.S. patent application(s), submitted by at least one of the present Applicant(s)/Inventor(s) is/(are) recently co-pending: U.S. utility patent application Ser. No. 13/916,370, entitled “FIREARM LOCKING ASSEMBLY”, submitted to the United States Patent and Trademark Office (USPTO) on Jun. 12, 2013, U.S. provisional Patent Application No. 61/966,788, filed on Mar. 4, 2014, U.S. provisional Patent Application No. 61/966,784, filed on Mar. 4, 2014, and U.S. Provisional Patent Application mailed to the USPTO on Apr. 23, 2014
FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0003] Not applicable.
REFERENCE TO SEQUENCE LISTING, A TABLE, OR A COMPUTER LISTING APPENDIX
[0004] Not applicable.
COPYRIGHT NOTICE
[0005] A portion of the disclosure of this patent document contains material that is subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or patent disclosure as it appears in the Patent and Trademark Office, patent file or records, but otherwise reserves all copyright rights whatsoever.
FIELD OF THE INVENTION
[0006] One or more embodiments of the invention generally relate to firearms. More particularly, the invention relates to firearms with improved safeties to
1) allow faster response going from safe to fire modes, and automatic return to safe mode. 2) prevent unauthorized handling and theft, 3) provide a personalized firearm with an automatic processor controlled trigger lock, not requiring any external device, and locked safety assembly in a tamper proof compartment.
BACKGROUND OF THE INVENTION
[0010] The following background information may present examples of specific aspects of the prior art (e.g., without limitation, approaches, facts, or common wisdom) that, while expected to be helpful to further educate the reader as to additional aspects of the prior art, is not to be construed as limiting the present invention, or any embodiments thereof, to anything stated or implied therein or inferred thereupon.
[0011] The following is an example of a specific aspect in the prior art that, while expected to be helpful to further educate the reader as to additional aspects of the prior art, is not to be construed as limiting the present invention, or any embodiments thereof, to anything stated or implied therein or inferred thereupon. By way of educational background, another aspect of the prior art generally useful to be aware of is that a firearm is a weapon that launches one or more projectile at high velocity through confined burning of a propellant.
[0012] Firearms using AR 15 and similar military type trigger assemblies typically use a safety selector lever that rotates a cam laterally above the extended back portion of the trigger. When the lever points to the rear, it is in its safe setting, the cam blocks the rear of the trigger from rising, and in front of the trigger's pivot point, the front sear of the trigger is prevented from dropping to release the hammer and fire the gun. Typically the shooter would carry an AR 15 with the end of their gun hand thumb resting on the left side of the lower receiver. To prepare to fire the AR 15, the end of the thumb must be moved back and up 2″ in order to press the safety selector lever down and forward, then return to its original resting place, a total of 4″. To return the gun to its safety setting the thumb must push the safety up and back, repeating the 4″ of movement in reverse. Overall the unlocking and relocking cycle involves 8″ of thumb movement. In contrast with the instant invention the thumb need only move about ½″ to move the safety selector lever to its fire position, then simply release it to allow the internal spring to automatically return the safety to its safe setting. When a conventional AR 15 shooter reaches back and up with their thumb, this forces part of the gun hand to come off the grip at a critical time. When the trigger is pulled, using a conventional safety selector lever, the rear of the trigger over the cam can raise and front drop, due to opposing flats on the trigger and cam, this action requires a ¼turn of the safety selector lever and cam. By comparison a shotgun's safety may only need a ¼″ or less of thumb movement. A faster and easier to use safety for AR 15 type firearm is needed but the placement of AR 15 trigger mechanism components do not lend to the use of traditional safeties. The instant invention teaches the design of a safety selector lever that solves the described problems.
[0013] Typically, there are several types of mechanical thumb operated trigger locks and safeties that strive to prevent accidental discharge, injuries and death. Some owners may simply neglect to switch the safety back on, or decide not to because of the needed 4″ of thumb movement and to be ready to go. If they trip, lean the gun against a tree or fence, the risk of accidental discharge is greatly increased. Occasionally an unauthorized child or person may switch the safety off and mistakenly fires a firearm thinking it was unloaded. Clamp on trigger locks may be used for pistols but unlikely are used for AR 15 type weapons. The military suffers from accidental shootings due to the safety lever not being reengaged after being placed in fire mode.
[0014] The AR 15 is the most popular rifle in the US, however it is believed many buyers do not have a gun safe to store them, relying on hiding them in the closet, or under the bed. Other than a safe or home security system, a hand gun type of trigger lock, even if used, permits the firearm to be stolen. It is estimated about 200,000 firearm are stolen every year. Many AR 15 owners likely do not have the room, money or inclination to own a gun safe. In many homes the AR 15 likely is the most valuable idem a thief could steal.
[0015] Unfortunately AR 15 have been used in well publicized mass shootings. The smart safeties disclosed in this patent application will guard against an AR 15 from being stolen and if stolen prevent it from being fired.
[0016] Typically, there is no practical defense against firearm theft. Stolen firearms often wind up on the street used in other crimes. There are currently no known commercially available firearms suitable for home defense that have an internal defense against being moved, stolen or unauthorized handling, including being taken to a school, other public place.
[0017] Typically there are no known commercially available firearms suitable for home defense, that warn an unauthorized user to put the firearm down, have an internal trigger lock to prevent unauthorized use by a child or others, that automatically locks the firearm if put down or taken away, or sounds an alarm in response to unauthorized handling or theft. Unauthorized use of a firearm requires 1) that it can be moved, and 2) the potential the trigger can be pulled, allowing the firearm to be fired. The instance invention processor, motion detector and alarm not only defend against the firearm being moved or stolen, but a second safety prevents the firearm from being firing.
[0018] The AR 15 is used by many of our troops along with many other firearm's using the same trigger, hammer and safety selector lever arrangement. The safety selector lever and its cam, referred herein as the “safety”, are located above the natural position of the gun hand thumb when the weapon is griped. The safety is intended to be used to prevent accidental discharge, injury and death. Unfortunately the design is awkward to use, likely resulting in many users simply not using the safety. The AK 47 outsells the AR 15 on the world market. It appears an experienced shooter could go from safe to fire modes faster using the AK 47 than if he used the AR 15. It is unknown if tests have been conducted to compare how fast an AR 15 can go from safe to fire settings verses the AK 47. Overall the AR 15 shooter must move his thumb 4″ compared about ½″ with the disclosed invention. Likely the AR 15 shooter with the instant invention selector lever can go from safe to fire faster than the AK 47 shooter, a potential life and death issue. It is obvious a shooter who only needs to push their thumb ½″ forward, could fire a lot faster than an someone who had to move their thumb 4″, or their whole hand up and down as with the AK 47. The slowest shooter at a gun fight is at a disadvantage. Our troops should not be the slow ones in a firefight or competition.
[0019] The design and location of the conventional AR 15 safety selector lever is such that the side or back of the shooters thumb likely would be used to return to the safety on setting, which is cumbersome. The instant invention eliminates this problem by automatically returning to its “safety on position”, when the thumb is released. This improvement likely can eliminate many friendly fire accidents. Troops would be less likely to carry their weapon with the safety off.
[0020] The electronic smart “PPS”, or personal press safety feature in conjunction with the countdown warning light, alarm, and automatic trigger lock can prevent unauthorized handling, theft, accidents and the need to purchase an expensive gun safe.
[0021] The processor and timer permit military firearms to ultimately be controlled by superior officers over several years of use. As an example troops could be issued weapons that typically would be unlocked for 12 hours in the morning, yet automatically relock if left unattended beyond a time limit, requiring the press safety be entered. Every week or month a new press safety would be given out. A squad or larger of soldiers might use the same press safety. Each issued weapon would have years of monthly press safeties stored. A special press safety would be required to remove the smart grip from the lower receiver. Conventional grips will not fit on the lower receiver if the smart grip was cut off.
[0022] The US competes against Russia and others in international arms sales. The Russian AK 47 appears to have a faster to operate safety than the AR 15 and other U.S. military firearms. To compete internationally the US needs a faster to operate AR 15 and military arms. Our troops are deployed overseas, often with possible hostile locals in the area. The instant invention automatically guards against unauthorized handling and theft.
[0023] The US recently lost numerous firearms in Libya that were stolen. The disclosed firearms of this invention unlikely would have been stolen due to the security features.
[0024] In view of the foregoing, it is clear that these traditional techniques are far from perfect and leave room for more optimal approaches.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The present invention is illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar elements and in which:
[0026] FIG. 1 illustrates a detailed perspective view of an exemplary firearm safety joined with a portion of the lower receiver of a firearm 100 , in accordance with an embodiment of the present invention;
[0027] FIG. 2 illustrates a detailed perspective view of an exemplary grip safety assembly 201 joined with an exemplary lower receiver 202 of a firearm in an exemplary smart locked mode, in accordance with an embodiment of the present invention;
[0028] FIG. 3 illustrates a detailed perspective view of an exemplary grip safety firearm locking assembly 301 joined with a portion of an exemplary firearm lower receiver 302 in an exemplary smart safety locked mode, in accordance with an embodiment of the present invention; and
[0029] FIG. 4 illustrates a typical computer system that, when appropriately configured or designed, may function in an exemplary firearm locking assembly, in accordance with an embodiment of the present invention.
[0030] Unless otherwise indicated illustrations in the figures are not necessarily drawn to scale.
DETAILED DESCRIPTION
[0031] The present invention is best understood by reference to the detailed figures and description set forth herein.
[0032] Embodiments of the invention are discussed below with reference to the Figures. However, those skilled in the art will readily appreciate that the detailed description given herein with respect to these figures is for explanatory purposes as the invention extends beyond these limited embodiments. For example, it should be appreciated that those skilled in the art will, in light of the teachings of the present invention, recognize a multiplicity of alternate and suitable approaches, depending upon the needs of the particular application, to implement the functionality of any given detail described herein, beyond the particular implementation choices in the following embodiments described and shown. That is, there are numerous modifications and variations of the invention that are too numerous to be listed but that all fit within the scope of the invention. Also, singular words should be read as plural and vice versa and masculine as feminine and vice versa, where appropriate, and alternative embodiments do not necessarily imply that the two are mutually exclusive.
[0033] It is to be further understood that the present invention is not limited to the particular methodology, compounds, materials, manufacturing techniques, uses, and applications, described herein, as these may vary. It is also to be understood that the terminology used herein is used for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. It must be noted that as used herein and in the appended claims, the singular forms “a,” “an,” and “the” include the plural reference unless the context clearly dictates otherwise. Thus, for example, a reference to “an element” is a reference to one or more elements and includes equivalents thereof known to those skilled in the art. Similarly, for another example, a reference to “a step” or “a means” is a reference to one or more steps or means and may include sub-steps and subservient means. All conjunctions used are to be understood in the most inclusive sense possible. Thus, the word “or” should be understood as having the definition of a logical “or” rather than that of a logical “exclusive or” unless the context clearly necessitates otherwise. Structures described herein are to be understood also to refer to functional equivalents of such structures. Language that may be construed to express approximation should be so understood unless the context clearly dictates otherwise.
[0034] Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this invention belongs. Preferred methods, techniques, devices, and materials are described, although any methods, techniques, devices, or materials similar or equivalent to those described herein may be used in the practice or testing of the present invention. Structures described herein are to be understood also to refer to functional equivalents of such structures. The present invention will now be described in detail with reference to embodiments thereof as illustrated in the accompanying drawings.
[0035] From reading the present disclosure, other variations and modifications will be apparent to persons skilled in the art. Such variations and modifications may involve equivalent and other features which are already known in the art, and which may be used instead of or in addition to features already described herein.
[0036] Although Claims have been formulated in this application to particular combinations of features, it should be understood that the scope of the disclosure of the present invention also includes any novel feature or any novel combination of features disclosed herein either explicitly or implicitly or any generalization thereof, whether or not it relates to the same invention as presently claimed in any Claim and whether or not it mitigates any or all of the same technical problems as does the present invention.
[0037] Features which are described in the context of separate embodiments may also be provided in combination in a single embodiment. Conversely, various features which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub combination. The Applicants hereby give notice that new Claims may be formulated to such features and/or combinations of such features during the prosecution of the present application or of any further application derived therefrom.
[0038] References to “one embodiment,” “an embodiment,” “example embodiment,” “various embodiments,” etc., may indicate that the embodiment(s) of the invention so described may include a particular feature, structure, or characteristic, but not every embodiment necessarily includes the particular feature, structure, or characteristic. Further, repeated use of the phrase “in one embodiment,” or “in an exemplary embodiment,” do not necessarily refer to the same embodiment, although they may.
[0039] As is well known to those skilled in the art many careful considerations and compromises typically must be made when designing for the optimal manufacture of a commercial implementation any system, and in particular, the embodiments of the present invention. A commercial implementation in accordance with the spirit and teachings of the present invention may configured according to the needs of the particular application, whereby any aspect(s), feature(s), function(s), result(s), component(s), approach(es), or step(s) of the teachings related to any described embodiment of the present invention may be suitably omitted, included, adapted, mixed and matched, or improved and/or optimized by those skilled in the art, using their average skills and known techniques, to achieve the desired implementation that addresses the needs of the particular application.
[0040] In the following description and claims, the terms “coupled” and “connected,” along with their derivatives, may be used. It should be understood that these terms are not intended as synonyms for each other. Rather, in particular embodiments, “connected” may be used to indicate that two or more elements are in direct physical or electrical contact with each other. “Coupled” may mean that two or more elements are in direct physical or electrical contact. However, “coupled” may also mean that two or more elements are not in direct contact with each other, but yet still cooperate or interact with each other.
[0041] A “processor” may refer to one or more apparatus and/or one or more systems that are capable of accepting a structured input, processing the structured input according to prescribed rules, and producing results of the processing as output. Examples of a processor may include: a computer; a stationary and/or portable computer; a computer having a single processor, multiple processors, or multi-core processors, which may operate in parallel and/or not in parallel; a general purpose computer; a supercomputer; a mainframe; a super mini-computer; a mini-computer; a workstation; a micro-computer; a server; a client; an interactive television; a web appliance; a telecommunications device with internet access; a hybrid combination of a computer and an interactive television; a portable computer; a tablet personal computer (PC); a personal digital assistant (PDA); a portable telephone; application-specific hardware to emulate a computer and/or software, such as, for example, a digital signal processor (DSP), a field-programmable gate array (FPGA), an application specific integrated circuit (ASIC), an application specific instruction-set processor (ASIP), a chip, chips, a system on a chip, or a chip set; a data acquisition device; an optical computer; a quantum computer; a biological computer; and generally, an apparatus that may accept data, process data according to one or more stored software programs, generate results, and typically include input, output, storage, arithmetic, logic, and control units.
[0042] “Software” may refer to prescribed rules to operate a computer. Examples of software may include: code segments in one or more computer-readable languages; graphical and or/textual instructions; applets; pre-compiled code; interpreted code; compiled code; and computer programs.
[0043] A “computer-readable medium” may refer to any storage device used for storing data accessible by a computer. Examples of a computer-readable medium may include: a magnetic hard disk; a floppy disk; an optical disk, such as a CD-ROM and a DVD; a magnetic tape; a flash memory; a memory chip; and/or other types of media that can store machine-readable instructions thereon.
[0044] A “computer system” may refer to a system having one or more computers, where each computer may include a computer-readable medium embodying software to operate the computer or one or more of its components. Examples of a computer system may include: a distributed computer system for processing information via computer systems linked by a network; two or more computer systems connected together via a network for transmitting and/or receiving information between the computer systems; a computer system including two or more processors within a single computer; and one or more apparatuses and/or one or more systems that may accept data, may process data in accordance with one or more stored software programs, may generate results, and typically may include input, output, storage, arithmetic, logic, and control units.
[0045] A “network” may refer to a number of computers and associated devices that may be connected by communication facilities. A network may involve permanent connections such as cables or temporary connections such as those made through telephone or other communication links. A network may further include hard-wired connections (e.g., coaxial cable, twisted pair, optical fiber, waveguides, etc.) and/or wireless connections (e.g., radio frequency waveforms, free-space optical waveforms, acoustic waveforms, etc.). Examples of a network may include: an internet, such as the Internet; an intranet; a local area network (LAN); a wide area network (WAN); and a combination of networks, such as an internet and an intranet.
[0046] Exemplary networks may operate with any of a number of protocols, such as Internet protocol (IP), asynchronous transfer mode (ATM), and/or synchronous optical network (SONET), user datagram protocol (UDP), IEEE 802.x, etc.
[0047] Embodiments of the present invention may include apparatuses for performing the operations disclosed herein. An apparatus may be specially constructed for the desired purposes, or it may comprise a general-purpose device selectively activated or reconfigured by a program stored in the device.
[0048] Embodiments of the invention may also be implemented in one or a combination of hardware, firmware, and software. They may be implemented as instructions stored on a machine-readable medium, which may be read and executed by a computing platform to perform the operations described herein.
[0049] In the following description and claims, the terms “computer program medium” and “computer readable medium” may be used to generally refer to media such as, but not limited to, removable storage drives, a hard disk installed in hard disk drive, and the like. These computer program products may provide software to a computer system. Embodiments of the invention may be directed to such computer program products.
[0050] An algorithm is here, and generally, considered to be a self-consistent sequence of acts or operations leading to a desired result. These include physical manipulations of physical quantities. Usually, though not necessarily, these quantities take the form of electrical or magnetic signals capable of being stored, transferred, combined, compared, and otherwise manipulated. It has proven convenient at times, principally for reasons of common usage, to refer to these signals as bits, values, elements, symbols, characters, terms, numbers or the like. It should be understood, however, that all of these and similar terms are to be associated with the appropriate physical quantities and are merely convenient labels applied to these quantities.
[0051] Unless specifically stated otherwise, and as may be apparent from the following description and claims, it should be appreciated that throughout the specification descriptions utilizing terms such as “processing,” “computing,” “calculating,” “determining,” or the like, refer to the action and/or processes of a computer or computing system, or similar electronic computing device, that manipulate and/or transform data represented as physical, such as electronic, quantities within the computing system's registers and/or memories into other data similarly represented as physical quantities within the computing system's memories, registers or other such information storage, transmission or display devices.
[0052] In a similar manner, the term “processor” may refer to any device or portion of a device that processes electronic data from registers and/or memory to transform that electronic data into other electronic data that may be stored in registers and/or memory. A “computing platform” may comprise one or more processors.
[0053] A non-transitory computer readable medium includes, but is not limited to, a hard drive, compact disc, flash memory, volatile memory, random access memory, magnetic memory, optical memory, semiconductor based memory, phase change memory, optical memory, periodically refreshed memory, and the like; however, the non-transitory computer readable medium does not include a pure transitory signal per se.
[0054] The present invention will now be described in detail with reference to embodiments thereof as illustrated in the accompanying drawings.
[0055] A simplest form of this invention may be an improved safety selector lever, its cam and/or trigger assembly. This assembly may also be used in conjunction with various electronic embodiments of this invention.
[0056] There may be various types of firearm locking assemblies that may be provided as embodiments of the present invention. In one embodiment of the present invention, a firearm locking assembly may provide multiple locking modes and/or integrates into a firearm. In some embodiments, the firearm locking assembly may utilize various components, including, without limitation, access codes, personal press safety (“PPS”), a safety selector lever or grip switch, and a processor to switch between the various locking modes. In at least one embodiment, the firearm locking assembly may utilize a blocker and/or blocking element. In some embodiments, the blocking element may include a bar that may be any suitable shape, including, without limitation, round, rectangular or square. In some of these embodiments, the bar may be operable to restrict backward movement of a firearm trigger or trigger assembly to prevent discharge. However, in other embodiments, the blocking element may include, without limitation, a mechanical barrier of a variety of shapes and/or dimensions which may be configured to restrict movement of the trigger. In some embodiments, a safety selector lever cam may serve as part of a trigger blocking element in conjunction with a blocking bar or rod in one or more embodiments, a thumb safety lever may provide a tactile indication of whether a smart safety is engaged. In some embodiments, when a personal safety press (“PSP”) is entered, a motor or other suitable device may move the blocking element.
[0057] In one embodiment of the present invention, a safety module with a rearward facing keyboard with pushbuttons and warning lights may allow a firearm to be unlocked through a predetermined personal code that may be entered using pushbuttons or other suitable input means. In some embodiments, a safety code and/or personal press safety portion may accept a predetermined amount of incorrect entries before performing panic procedures. In a non-limiting example, a personal press safety portion may accept 3 incorrect code entries, then not accept more attempts for 30 minutes, and cause an alarm to sound. In some embodiments, a processor may actuate a loud alarm for a given amount of time in response to other user actions. In a non-limiting example, a processor may actuate an alarm for 15 to 20 seconds after a firearm is moved as determined by a motion detector. In many embodiments, an assembly may also include, without limitation, a vibration motor to verify successful programming, an accelerometer, and a loud alarm portion for dissuading unauthorized handling. In some embodiments, a tamper resistant grip safety module may house safety components. In at least one embodiment, an alternative power source may provide backup power. In this manner, trial and error unlocking of the firearm or the defeating of the safety mechanism may be prevented.
[0058] In one embodiment of the present invention, the firearm locking assembly may include a multiplicity of modes that may provide different accessibility to the firearm. In many embodiments, a multiplicity of modes may include, without limitation, an alarm locked mode, a locked travel mode with the accelerometer/alarm off, an unlocked mode with automatic re-locking if the firearm is put down or taken, and a timed unlocked mode with automatic relocking after a programed period of time, to prevent accidently leaving the firearm unlocked for a long period of time. In some embodiments, the locked mode may provide a physical barrier to prevent the firearm from discharging. The locked mode may include a restriction portion that may be positioned such that the trigger and/or the safety lever member may be above an end of the trigger. In at least one embodiment, the restriction portion may be internally located in the firearm to engage the trigger. In some embodiments, the restriction portion may serve as a physical barrier that may restrict rotation of the trigger, and thereby may prevent the trigger from discharging the firearm. In some embodiments, a motor may power the restriction portion to and from the trigger and/or the safety member. In some embodiments, a thumb safety lever may be positioned on an exterior of the firearm. In many embodiments, the safety lever may be configured to be operable to signal an owner if smart restriction portion blocks and/or allows the trigger assembly to discharge the firearm. In one or more embodiments, the safety lever may be configured to be operable to be pressed forward by pressure from a user's gun hand thumb. In some embodiments, the safety lever may be operatively joined to a processor and/or act as an electronic switch. In some of these embodiments, the processor may be programmed to actuate a motor to position the restriction portion upon the safety lever being pressed or released as a switch. However, in other embodiments, the processor may be operable to provide numerous other functions for the firearm locking assembly, including, without limitation, communicating with the owner, communicating with the access code portion, communicating that the code must be entered or the alarm will sound because the safety cannot be pressed forward, communicating via a light or lights on the control module keyboard, communicating with the motor, communicating with the power source and the alternative power source, communicating with the alarm portion, communicating with the GPS, communicating the firearm location to a remote receiver, communicating that an accelerometer indicates the firearm has been fired, communicating with the vibration motor, communicating digital images of what the firearm was pointed at when fired or when the safety lever is pressed, communicating digital images of the party holding the firearm when a false access code is entered. Those skilled in the art, in light of the present teachings, will recognize that the camera feature may help identify if and when an officer is justified in discharging the firearm.
[0059] In one embodiment of the present invention, the firearm safety assembly may be operable to automatically regulate functions of a firearm through the use of, without limitation, an accelerometer, a processor, a code entry, and a timer. In some embodiments, the firearm safety assembly may be un-locked by a pushbutton combination lock that may prevent unauthorized access to the safety assembly without first entering the correct push code. In some embodiments, the code may be set very short with 2 or 3 numbers, potentially allowing unauthorized trial and error attempts to unlock the firearm. In at least one embodiment, to mitigate unauthorized access, the processor may for 30 minutes prevent more than 3 wrong code entries. Moreover, in some embodiments, to further protect against unauthorized handling the motion detector may alert the processor if the firearm was moved cumulatively over 20 seconds over 30 minutes, and if so the alarm may commence to sound. In many embodiments, when the alarm is triggered, the code may be entered to cancel it.
[0060] In one embodiment of the present invention, the keyboard may include, without limitation, one or more back-lit pushbuttons and/or one or more LED lights. In a non-limiting example, a keyboard may have three back-lit pushbuttons and one greed LED light. In the present non-limiting example, when firearm is picked up the processor and motion detector may cause the green light to blink once per second for 10 seconds as a warning, then yellow that the code must be entered or the alarm will sound if the code is not entered or if the firearm is not put down; after 15 seconds a 1 second alarm will sound the warning light blinks red very rapidly as a final warning. Further, in the present non-limiting example, after 20 seconds the alarm may begin to sound and continue until the personal safety is entered. In some instances, a purpose of the warning blinking lights, motion detector and/or alarm may not be to warn the owner or an unauthorized person that the firearm is unlocked or locked, or signal others the firearm is being handled, but to discourage unauthorized persons such a child, teenager or thief from handling or attempting to unlock the firearm in the first place, without the alarm ever having to sound. In some embodiments, the owner may be warned by the blinking light that the code may be entered. Those skilled in the art, in light of the present teachings, will recognize that police officers, may select an embodiment using a 3 press personal safety, then pre enter two presses leaving 1 press to unlock. As there are 12 possible 1 press combinations, 144-2 press and over 1500 3 press possible combinations, the odds of an assailant taking an officers weapon away, guessing which and how many presses are needed, appears slight.
[0061] In some embodiments a police officer, soldier or homeowner may simply enter all but a last 1 or 2 presses, then put the firearm aside, and the motion detector may be automatically off for 24 hours and the firearm locked. In some of these embodiments, remaining single press or presses may be entered to unlock the firearm. In at least one embodiment, if the firearm was locked and wrestled away the advisory would have to correctly guess the necessary presses and risk setting off the alarm. In some embodiments, during an initial 24 hours the firearm could be handled without setting off the alarm.
[0062] In many embodiments, if the alarm is triggered to stop the alarm the full code should be entered. In some embodiments, an advisory's risk for a wrong entry could be a silent alarm which may send a signal to police headquarters, a military headquarters or a security company, and/or a loud alarm would sound.
[0063] In some embodiments, the assembly may include, without limitation, an unlocked mode that may allow the firearm to discharge. In some of these embodiments, the unlocked mode may function to disengage the restriction portion from the trigger. In one or more embodiments, an access code portion may be operatively joined with the processor for switching between the modes. In a few embodiments, the control module may include a plurality of buttons that may be depressed in combination to switch between modes. In some embodiments, the firearm locking assembly may switch between each mode depending on the manipulation of the access code portion, the processor commands.
[0064] In one embodiment of the present invention, the firearm locking assembly may include a firearm. In some embodiments, the firearm locking assembly may be integrated into the firearm. However, in other embodiments, the firearm locking assembly may detachably join the firearm. In some embodiments, the firearm may include, without limitation, a handgun, a pistol, a rifle, an AR 15, an M 16, other military type weapons and a shotgun. In many embodiments, the firearm may include a trigger configured to engage a triggering object. In some of these embodiments, the trigger may provide an exterior access for firing the firearm. In some embodiments, the firearm may include a grip. In some of these embodiments, the grip may be operable to be held by a hand. Moreover, in some of these embodiments, the grip may include a pressure sensitive switch. In at least one embodiment, the switch may be configured to be operable to be depressed by pressure from a hand. In some embodiments, a grip switch may initiate the functional aspects of the firearm locking assembly by communicating with the processor, actuating an alarm, and operatively joining with the access code portion.
[0065] In some embodiments, a safety control module may be positioned in proximity to the grip and operatively joined with the processor. In some of these embodiments, the safety control module may include, without limitation, warning LED lights, push buttons, a camera and or a laser for sighting. In a non-limiting example, in a military situation an ergonomically placed keypad having a multiplicity of buttons could program the processor to require a different smart push safety every day, week or month. In the present non-limiting example, the government could control supplying smart push codes in the future, in order to keep friendly troops friendly, or deny firearm use.
[0066] In many embodiments, the multiplicity of buttons may be depressed in predetermined combinations to communicate with the processor for locking or unlocking the firearm. In some embodiments, manipulating the multiplicity of buttons on the smart safety module may provide communication with the processor to switch the firearm locking assembly between each mode.
[0067] In one embodiment of the present invention, the firearm locking assembly may include an alarm portion to dissuade an unauthorized person from handling the firearm in the first place, or trial and error attempts to get the correct combination. In a non-limiting example, three wrong attempts lock the weapon down for 30 minutes. In the present non-limiting example, when the firearm is moved a warning light on the keyboard would blink green once per second for 10, seconds, amber for 6 seconds, then red to dissuade handling. In many instances, even if no one was within listening distance to be alerted, the mere prospect of a loud alarm sounding should persuade most unauthorized persons to put the firearm down. In some embodiments, the alarm portion may alert with an illumination or an audio signal. However, in one embodiment, the alarm portion may alert inaudibly. In one embodiment, the alarm portion may sound if a specific button is depressed, or if the access code portion has not been manipulated in a predetermined amount of time. In some embodiments, the alarm portion may include a motion sensor. In some of these embodiments, the processor may actuate the alarm portion when the motion detector detects movement and the safety control module is not properly manipulated.
[0068] In some embodiments, the grip safety assembly portion may include, without limitation, a motor and a trigger assembly blocker. In some of these embodiments, a restriction portion or blocker may be advanced and/or retracted by a threaded motor shaft to alternatively block and unblock the trigger. In at least one embodiment, when the processor detects low power in the power source, it may automatically alert the operator by use of the keyboard lights.
[0069] In one embodiment, pushbuttons may signal the processor to put the assembly into timed unlocked mode.
[0070] Those skilled in the art, in light of the present teachings, may recognize personalized firearm locking designs based on fingerprint reading technology, biometrics, chips placed under the skin, special rings or wrist watches that lock the trigger but do not lock access to the firearm locking assembly, would be vulnerable to tampering and possible defeat of the firearm locking assembly. A so called smart gun that contains a trigger lock, that allows access to the safety components by the removal of a screw or pins, so that the safety can be defeated, is flawed. In many embodiments, the safety assembly requires the gun be unlocked before the safety assembly may be accessed. Moreover the motion detector and alarm, combined with programming to deny access after wrong entries, are configured to deny prolonged trial and error attempts to unlock.
[0071] In some embodiments, the disclosed firearm locking assembly may utilize a 100+ decibel alarm that may operatively join with the processor and a potion detector. In a non-limiting example, the firearm may sound its alarm if the personal safety code is not entered within 20 seconds of the firearm being picked up. In this manner an unauthorized person may have very little time to try to defeat the personalized locking assembly or commit theft. In some embodiments, the firearm may be programmed to have the alarm sound when the safety lever is released, or shortly thereafter, in case of a takeaway situation. In some of these embodiments, firearm may cancel alarm if any button is pressed before the safety lever is released. In many embodiments, the firearm locking assembly may further utilize, without limitation, lights associated with the access code portion, a timer and/or an accelerometer to safeguard against theft, tampering and/or unauthorized handling by children and others. In some embodiments, firearms intended for hunting or being retrofitted may not utilize a motor, restriction portion, or safety selector lever to prevent the firearm from firing, and instead may use the accelerometer to alert the processor of movement requiring the access code be used or the firearm put down within the programmed period of time, and if not the alarm may begin to sound an alarm as programmed, making theft or unauthorized handling impractical.
[0072] FIG. 1 illustrates a detailed perspective view of an exemplary firearm safety joined with a portion of the lower receiver of a firearm 100 , in accordance with an embodiment of the present invention. In the present embodiment, a smart safety lever 101 , which may replace a conventional safety selector lever, may point generally down to slightly forward in this view in a safety off position, and may generally be flat against a lower receiver. Further, in the present embodiment, a smart safety cam 102 may extend laterally from a pivot end of the smart safety lever 101 , over a rear portion of a trigger blocking element 103 . Still further, in the present embodiment, a trigger 105 may be configured at 110 to permit a trigger blocking element to raise and not be blocked by the cam at 104 , which may permit the safety lever and/or cam to only rotate a little instead of a normal 90-degree rotation for an AR 15 and M 16. In some embodiments, if the safety lever and/or cam are being used to select, without limitation, semi-automatic, burst and/or automatic fire, a cam opening at 104 may be larger to permit the cam more rotation. In one or more embodiments, if the safety is pulled back to its safety on position at 109 , or pushed back by spring 108 , a recess 104 in the cam may rotate so that the trigger blocker may not be aligned, and the cam may prevent the rear of the trigger from rising, which may prevent the trigger from being pulled. If the cam rotates to permit the trigger blocker to raise, the trigger may be pulled to allow its front end shear 106 to drop, to release the hammer and fire the firearm.
[0073] FIG. 2 illustrates a detailed perspective view of an exemplary grip safety assembly 201 joined with an exemplary lower receiver 202 of a firearm in an exemplary smart locked mode, in accordance with an embodiment of the present invention. This weapon may have five or more safeties. In the present embodiment, a countdown warning light safety 231 may alert a person that the firearm may be put down and/or PPs entered, a motion detector activated alarm 238 , a spring and thumb actuated automatic mechanical thumb safety lever 214 , a pushbutton automatic electronic trigger lock with a timer 232 , a trigger blocking element safety rod 203 that may also lock a grip safety assembly 201 to the lower receiver to prevent disabling of the safety assembly.
[0074] In the present embodiment, a processor 212 may direct a motor 209 to rotate a threaded shaft 207 . In some embodiments, the threaded shaft 207 may push a threaded connector 210 forward. In some of these embodiments, the threaded connector 210 may push a blocking element or rod 203 forward into a recess 204 in a trigger 225 to prevent the trigger from rotating to drop a shear 206 and release the hammer. In at least one embodiment, the safety lever 214 may be held forward by a gun hand thumb at 241 , so that a cam 215 may permit a trigger blocking element 242 to raise, so that the trigger may be pulled after an owner enters his or her personal press safety via keyboard pushbuttons 232 , which may cause the blocking element to be retracted. In some embodiments, the grip assembly 201 may contain a locked and/or watertight safety assembly 208 which may contain, without limitation, the gear motor 209 , threaded shaft, connector, batteries 211 , and a piezo alarm 238 , configured to produce 100 decibels, to dissuade theft and unauthorized handling when triggered by the motion detector and timer mounted on the processor.
[0075] In one or more embodiments, a smart control module 230 may have a camera and lens 234 that alternatively may be located elsewhere on the firearm, and a warning light 213 , in addition to the pushbuttons and lights. In other embodiments, a laser may be located at 234 .
[0076] In some embodiments, the processor may contain a silent alarm such as, without limitation, an FM transmitter and GPS device to communicate that the firearm is being handled or stolen if the PPS was not entered triggering the alarm. In many instances, military firearms in storage overseas thus could be secured.
[0077] In the present embodiment, the firearm locking assembly may include an unlocked mode that may allow the firearm to discharge. In some embodiments, the unlocked mode may function to disengage the blocking element from the trigger. In this manner, the trigger may freely move for discharging the firearm. In some embodiments, a smart control module may be operatively joined with a processor using a cable 236 for entering the owner's personal press safety. In some of these embodiments, the safety control module may include a plurality of buttons 232 that may be depressed in combination to switch between modes. Those skilled in the art, in light of the present teachings will recognize that myriad combinations of button manipulation may be utilized for any function of the firearm locking assembly. In one embodiment, the multiplicity of buttons may include 2 or 3 buttons in a row on a keypad measuring approximately 1.″×0.4″. Those skilled in the art, in light of the present teachings will recognize that a 3 button keypad would have the equivalent of 12 buttons if the processor is programmed to regulate the pressing of 2 buttons at once as additional numbers and regulating a less than 0.5 second as 1 number and over 0.5 second as another. For example, without limitation, 3 buttons may be positioned close together in a row to allow the users thumb to press 2 buttons at once. In this embodiment buttons 1 and 2 pressed at once may be the equivalent of button 4, buttons 2 and 3 the equivalent of button 5, 1 and 3 the equivalent of button 6. In many embodiments, 6 press combinations may double to 12 as the software may regulate regular and slightly longer presses as different presses. In some embodiments, a 3 button keyboard may have the equivalent of 12 buttons, if pressed only once, twice 144 possible PPS and 3 times over 1700 PPS. In many instances, an unauthorized person may not know if 1, 2 or 3 presses were needed, or if just 1 press would cause the alarm to sound.
[0078] In yet another embodiment, a law enforcement officer may chose a single press for a safety for daily carry with an alarm to sound with a single wrong press or if the weapon is unlocked and the safety lever released, the alarm may sound unless all 3 buttons are pressed to cancel. In one embodiment the grip safety assembly is attached to the lower receiver vertically and must be removed vertically. The takedown pin 237 has been redesigned to both connect the lower receiver to the gun's upper half but connect the grip safety assembly to the lower receiver. To disconnect the grip safety assembly from the lower receiver the takedown pin must be pushed through and the safety rod 203 fully retracted into the grip safety module 208 .
[0079] In some embodiments, the firearm locking assembly may include a plurality of modes operable to restrict use of a firearm. In some of these embodiments, an accelerometer may be configured to detect potential unauthorized handling. In many embodiments, a timer associated with the processor may allow a programmed amount of time such as, without limitation, 20 seconds for an authorizing code to be entered by the use of a plurality of buttons on a rearward facing keyboard. In some embodiments, the smart control module may include, without limitation, a keyboard, a digital display, a switch system, warning lights, digital camera components, silent alarm FM and GPS components.
[0080] In one embodiment of the present invention, the motor 209 may power the blocker 203 to and from the trigger recess 204 . In some embodiments, the motor 209 may include a threaded motor shaft 207 connecting to a threaded connector 210 that may orient 90 degrees so that when the motor is powered, the threaded motor shaft 207 may extend and/or retract the connector through the threaded aperture in the connector, that in turn may extend and/or retract the blocker to lock or unlock the trigger. In one alternative embodiment, an illumination portion 232 may be used to signify each mode. In some embodiments, the illumination portion may include, without limitation, colored lights. Those skilled in the art, in light of the present teachings will recognize that in emergency situations the mode of the firearm may be important to discern by feel and through a quick visual inspection.
[0081] In some embodiments, the processor may be programmed to actuate the motor to position the blocker in response to the personal press safety or PPS being entered. However, in other embodiments, the processor may be operable to provide numerous other functions for the firearm safety mechanism, including, without limitation, communicating with the safety, communicating with the smart control module, communicating with the motion detector, communicating with the vibration motor, communicating with the motor, communicating with a camera, communicating with a GPS, communicating via a FM radio, communicating with a lazier, communicating with a flashlight communicating with the a police station, security service or others that unauthorized firearm handling occurred via a silent alarm, communicating with an unauthorized person via warning lights and or an audio alarm to put the weapon down, communicating via lights that the power source was low and should be changed, communicating with the power source and the alternative power source.
[0082] In one embodiment of the present invention, the firearm locking assembly may include an alarm portion for dissuading an unauthorized person from stealing or handling the weapon. In at least one embodiment, an alarm portion may alert with an illumination or an audio signal. In some embodiments, the alarm portion may include a 100+ decibel audio signal. However, in one embodiment, the alarm portion may alert inaudibly. In one embodiment, the alarm portion may sound 20 seconds after the motion detector registers movement if the smart control module buttons have not received the personal press safety. In some embodiments, the alarm portion may include, without limitation, an accelerometer, processor and/or piezo speaker. In one embodiment, the accelerometer may be sufficiently sensitive to signal to the processor if the firearm is picked up by an unauthorized user. For example, without limitation, after the firearm is moved the alarm portion may blink a warning for 20 seconds and if the firearm is not put down or the PPS is not entered the alarm may sound. In one embodiment the alarm sounds a 1 second warning at 15 seconds. However, in other embodiments, different time frames a silent FM signal may send the GPS coordinates. In some embodiments, the power source may include, without limitation, a battery, and a thermal power source. In one embodiment, the power source may be positioned above the processor and adjacent to the motor.
[0083] In some embodiments, the firearm locking assembly may include an external power port for docking with an external power source, in the event the power source fails. For some embodiments, power failure may be unlikely as the processor may cause a warning light when the firearm is picked up, to blink green, yellow green etc. when the power source is, in a non-limiting example, 50% down. In another non-limiting example, when the power source is 75% down the warning light may blink yellow, yellow, green, then yellow, yellow red when 80% down. However in other embodiments, the firearm locking assembly may alert the owner by an illuminated light and/or alarm that the power source may need replacing.
[0084] In one embodiment of the present invention, an access code portion and a plurality of backlit buttons 232 positioned on a keyboard may be ergonomically oriented and aligned, to be seen by the owner when aiming the firearm. In alternative embodiments, lights 233 may be positioned adjacent to said buttons on a keypad. In some embodiments, the multiplicity of buttons may be positioned in a control module 230 in proximity to the grip and configured to be operable, such that a thumb may press either outer buttons, or either outer buttons and an adjacent button simultaneously. In some embodiments, a flush thumb safety 214 may be configured to allow the owner to reach and operate the pushbuttons on the keyboard with their thumb, which might not be possible with the raised safety selector lever currently used in the AR 15 and M 16. In one or more embodiments, the control module may house a laser and/or camera components.
[0085] FIG. 3 illustrates a detailed perspective view of an exemplary grip safety firearm locking assembly 301 joined with a portion of an exemplary firearm lower receiver 302 in an exemplary smart safety locked mode, in accordance with an embodiment of the present invention. In the present embodiment, unlike the grip safety assembly of FIG. 2 , a shooter may not push the thumb safety 314 forward without first unlocking the smart electronic trigger lock, so as to avoid confusion under stress of whether the gun may be unlocked or not. Further, in the present embodiment, the traditional grip 107 of FIG. 1 has been replaced with grip safety assembly 301 that may fit over a lower receiver 302 . In some embodiments, the motor 309 , threaded shaft 307 and trigger blocking element 303 , may be aligned off-center with a center of the cam 322 . In the present embodiment, the smart safety lever 314 may be held in a safe position by a spring, may be pushed forward a comparatively short distance by the gun hand thumb into its safety off position, and unlike a conventional AR 15 safety selector lever, released by the thumb to automatically return to the safety on position.
[0086] In the present embodiment, a blocking element may be extended so that a wider of two narrower portions 334 may abut a narrower portion 342 of the cam 322 , so that the smart thumb safety and its cam may not rotate to permit the trigger to be pulled. In some embodiments, an owner may confirm if the smart safety is locked simply by pushing the smart safety lever to see if it will go forward. In some of these embodiments, if the safety blocking element 310 is extended so that a narrower of two narrower portions abuts the cam at 342 , the cam and safety lever may then rotate so that the cam may allow the trigger blocking element to rotate up to permit the firearm to be fired. FIG. 3 safety may require a hole be drilled in lower receiver frame, while FIG. 2 design may use an existing grip bolt hole that may align with the trigger and/or helps to retrofit AR 15s.
[0087] In one embodiment of the present invention, the smart safety assembly may include special law enforcement modes. For example, without limitation, a police department may adopt use of the Smart AR 15 to be carried in squad cars. In the present non-limiting example, a squad car may be notified to respond to reports of an active shooter at a mall. Further, in the present non-limiting example, officers may respond and unlock Smart AR 15s by inputting standardized Department's Press Safety or DPS, which may unlock smart safety and may trigger silent FM alarm. In the present non-limiting example, an FM transmitter may broadcast and identify weapon's GPS location to a portable command center. Further, in the present non-limiting example, command personnel may be able track locations of all police Smart AR 15s on a laptop map. Still further, in the present non-limiting example, if an officer loses or puts a weapon down, it may automatically relock due to non-movement. In some embodiments, if a weapon is fired, a motion detector may detect a kick and may send a special GPS signal. In a few embodiments, when the silent alarm is activated an officer may be able to broadcast his current status by using pushbuttons.
[0088] In one embodiment of the present invention, security personnel may be armed with locked Smart AR 15. In the present embodiment, if a guard is attacked and disarmed before being able to use a weapon, the weapon may not be unlocked and used against him, the public or other responding officers. In some embodiments, smart law enforcement weapons may be set so that when they are unlocked in an emergency or the correct combination of buttons are pressed a signal is sent to other security personnel or headquarters.
[0089] In one embodiment of the invention, false entries and/or failure to enter the personal press safety may cause a silent and/or audio alarm. In some embodiments, a 100+dB alarm may be loud enough to distract or detour an unauthorized person or thief and alert public and others of danger. In some of these embodiments, alarms may optionally be triggered by an officer simply by pressing and holding any button for 2.5 seconds.
[0090] In some instances, law enforcement personnel modes may be operable to prevent a criminal from forcibly obtaining a firearm. In some situations, law enforcement personnel modes may be used for civilian use. In a non-limiting example, a civilian attacked in their home who is unable to unlock a weapon in time, or if it is unloaded, might press any button to trigger the alarms.
[0091] In some embodiments, a device may have one or more buttons. In the present non-limiting example, a device may have three buttons. In the present embodiment, a device may determine whether a correct first button of a code has been pressed in. Further, in the present embodiment, if the correct first button has been pressed the device may continue a blinking warning light countdown until gun is put down, or a balance of code is entered and unlocks the gun, or a wrong entry is made and then an alarm may sound after time limit expires. In some embodiments, when a correct first code press is made, a gun may be in “hold to complete” until rest of the code is entered, with motion detector and/or alarm off for 24 hours. In some of these embodiments, after 24 hours the motion detector, countdown and alarm automatically reengage, however the owner could still keep the gun with only one or two presses needed to unlock, however only one try would be allowed using remainder of original 20-second time. In one embodiment, an owner could let remaining time go to a few seconds if desired. In some embodiments, the device may determine whether a specific first button has been pressed and cause an emergency alarm to sound. In other embodiments, the device may determine whether any button has been pressed. In some embodiments, device may have a timer that may require a same or a new code be entered every 24 hours, for years. In at least one embodiment, a special code may be needed to remove and access grip safety assembly, which if not accessed to replace batteries and/or extend the code life, would intentionally render gun useless. In the present embodiment, if a second button has been pressed, device may determine whether device timed out before second button was pressed in. In some embodiments, device may have the timer set for any time length. In a non-limiting example, a timer may be set for 20 seconds or 24 hours before the alarm sounds. In the present non-limiting example, if a user fails to correctly select the first press code of their code within 20 seconds of cumulative movement over 30 minutes, the processor will cause the alarm to sound. Further, in the present non-limiting example, if during said 20 seconds motion stops, countdown it put on hold to complete. Still further, in the present non-limiting example, after a failed unlocking attempt, processor may be reset to receive a new code when any button is held in 2+ seconds and buttons blink yellow. In the present non-limiting example, with a failed unlocking attempt, any button may be held in 2+ seconds until buttons blink yellow once. Further, in the present non-limiting example, a full code may then be entered. Still further, in the present non-limiting example, if that entry is wrong a 3rd entry may be attempted however if that entry is wrong, the alarm would sound. In some embodiments, timer may pause based on specific user actions. In a non-limiting example, if user puts down device, device timer may pause until a user picks up device. In the present embodiment, if a first button has been pressed, device may determine whether a second button has been pressed in a step. In some embodiments, the device may determine whether a specific second button has been pressed. In other embodiments, the device may determine whether any button has been pressed. In the present embodiment, if a second button has been pressed, device may determine whether device timed out before second button was pressed in a step. In a non-limiting example, if a user fails to select correct second button within 20 seconds of selecting a first button, process may require any button be pressed 2+ seconds to reset for a second try. In the present embodiment, if device has not timed out, device may determine whether a third button has been pressed in a step. In some embodiments, the device may determine whether a specific third button has been pressed. In other embodiments, the device may determine whether any button has been pressed. In the present embodiment, if a second button has been pressed, device may determine whether device timed out before third button was pressed. Further, in the present embodiment, if device has not timed out, device may determine whether user has cancelled unlocking attempt in a step. In some embodiments, user may select a predetermined combination of buttons to cancel an unlocking attempt. In alternative embodiments, user may select a unique “cancel” button to cancel an unlocking attempt, or simply press any button 2+ seconds. In many embodiments, canceling an unlocking attempt may be equivalent to resetting of unlocking process. In the present embodiment, if user has not cancelled unlocking attempt, device may determine whether user's input was correct in a step. Further, in the present embodiment, if input was correct, device may unlock in a step. In some embodiments, various events may take place during unlocking of device. In a non-limiting example, a warning light and/or one or more other lights may blink to indicate declining time remaining. In yet another embodiment with a longer press on a button, all blue buttons briefly blink green, to signal a different input to the processor, and with a longer press on two buttons at once, all blue buttons briefly blink yellow to signal another input to the processor. In a non-limiting example, a single press can produce 12 different inputs, and two presses 144 combinations. In the present embodiment, if input was not correct, device may determine whether current unlocking attempt was user's third consecutive unlocking attempt in a step. In some embodiments, device may have a counter to keep track of user's failed attempts. In some of these embodiments, counter may reset after a certain amount of time. In the present embodiment, if current unlocking attempt is user's third consecutive attempt, device may activate an alarm. Further, in the present embodiment, device may block further entries for a specific period of time in a step. In a non-limiting example, device may block further entries for a period of 30 minutes. In some embodiments, device may allow any number of attempts prior to activating alarm and/or blocking further entries.
[0092] In a non-limiting example, user may change safety lever from a “safe” mode to a “fire” mode by moving user's thumb ½-inch forward, as opposed to approximately 4-inch motion in typical available solutions. In some embodiments, safety lever may automatically return from fire mode to safe mode upon user's thumb release of safety lever. In a non-limiting example, safety lever may automatically return to “safe” mode when user releases lever.
[0093] In many embodiments, a device may automatically engage various safety features after a certain period of inactivity while in timed unlocked mode. In a non-limiting example, a device may activate a motion detector and/or processor after a 10-minute period of inactivity by user, after warning light blinks yellow for 30 seconds. Some embodiments may incorporate a silent alarm which may activate when handled by an unauthorized user and/or when used in an unauthorized way.
[0094] In some embodiments, an unlocked device may remain unlocked for a specific amount of time. In a non-limiting example, an unlocked device may remain unlocked for a period of 10 minutes, blink a warning for 30 seconds then automatically relock. In the present non-limiting example, if the device motion detector detects movement during 10 minute period, time limits would be reset. In another non-limiting example, timer for unlocked period may be set anywhere between 30 seconds to 24 hours. In some embodiments, movement of device and/or pressing of buttons on device may reset timer.
[0095] In many embodiments, device buttons may have a variety of unique functions. In a non-limiting example, holding a first button for a given period of time may cause an alarm to sound until button is released. In another non-limiting example, holding a second button down for a given period may cause an alarm to sound until a predetermined code is entered on device buttons. In yet another non-limiting example, holding a third button for a given period may activate a silent alarm. In still another non-limiting example, holding multiple buttons for a given period may activate both an audio alarm and a silent alarm until a predetermined code is entered on device buttons.
[0096] In a non-limiting example, a smart AR 15 may be set to use a 2 to 4 personal press safety (“PPS”) to unlock a gun. In the present non-limiting example, when an owner knows they made an entry mistake, the owner may release and re-grip the safety lever, or press any button 2.5 seconds until gun vibrates. Further, in the present embodiment, if their 2ed attempt is wrong, they may try again but a wrong 3ed attempt may cause the alarm to sound and a 30 minute lockout for code entries. In a non-limiting example, when the gun is locked the owner may pre-enter all but the last 1 or 2 numbers of the PPS, within 20 seconds of picking up the weapon, then put the weapon down which causes the motion detector and processor to stop countdown. In the present non-limiting example, the weapon may remember an entry and may accept last 1 or 2 presses, if entered within remainder of initial 20-second time period or anytime later. Further, in the present non-limiting example, if the owner or an unauthorized person picks up the weapon and makes a 3 ed wrong entry within the of original 20-second time period, the alarm may sound and block all entries for 30 minutes.
[0097] In some embodiments, when the correct safety is entered the warning light and 3 button lights go off and the thumb safety lever may be pressed forward to also confirm the weapon is unlocked.
[0098] In many instances, the Smart safety selector lever may go from safe to fire settings faster than current AR 15s and military firearms in about ½″ instead of 4″ of thumb travel, and may automatically returns to safe when released. Both of these features may be seen as significant improvements. As the weapon may be used in a gun fight with an enemy, minimal movement to release the safety could be critical.
[0099] In some embodiments, the personal press safety must be entered to unlock the automatic electronic trigger lock, and if not, the trigger remains locked. In some of these embodiments, the smart thumb safety cannot be pushed forward, confirming to the owner that the automatic electronic was engaged. In some embodiments, the motion detector and processor would reengage the smart safety when the weapon was put down and not moved for, in a non-limiting example, 10 minutes. In another non-limiting example, in a military setting the smart electronic safety could be unlocked for extended periods such as a day or week and automatically re-engaged after a brief time when the weapon was put down as determined by the processor and motion detector. In some embodiments, if an unauthorized attempt is made to handle or steal the weapon, a loud alarm may sound. In many embodiments, if somehow the weapon is acquired by an enemy while unlocked, it would automatically re-lock as programmed. Moreover, in some embodiments, the silent alarm safety option may be employed in military deployment.
[0100] In one embodiment when the personal press safety is entered, the weapon may be programmed to remain unlocked for 24 hours, however lack of movement for 10 minutes, e.g. due to the weapon being put down, may cause relocking after a warning period. In a non-limiting example, a warning period may be one minute. In other embodiments, the 10 minute no motion automatic relock setting may be reprogrammed to between 30 seconds to 24 hours.
[0101] In some embodiments, holding button 1 in 2.5+ seconds may cause the audio alarm to sound until released,
holding button 2 in 2.5+ seconds may cause the audio alarm to sound until the PPS is entered, holding button 3 in 2.5+ seconds may cause silent alarm to sound, and/or holding buttons 2 and 3 in 2.5+ seconds may cause both audio and silent alarms to sound until PPS entered.
[0105] In one embodiment of the present invention, the processor may be operable to provide numerous other functions for the firearm safety assembly, including, without limitation, communicating with the thumb safety lever, communicating with push buttons, communicating with warning lights, communicating with the smart control module, communicating with the motor, communicating with the power source and the alternative power source, communicating with the motion detector/accelerometer, communicating with the audible alarm, communicating with the silent alarm, communicating with a GPS, communicating with digital image recording component communicating with the vibration motor, communicating with an internal FM transmitter, communicating with a law enforcement agency, communicating with a private security company, communicating with the keyboard, communicating with status lights in the keyboard, communicating with the firearm owner that the power source, which may be batteries are weak, and that they should be replaced. In some embodiments, upon the motion detector sensing movement and/or receiving a predetermined PPS from the smart control module, the processor may actuate the motor for positioning the blocker into the unlocked mode. In one or more embodiments, the power source may include, without limitation, 2 or 4-1.5 volt AAAA batteries, a volt battery, coin batteries . . . . In some embodiments, the processor through the lights would communicate to the owner that the power supply needed replacement
[0106] In one alternative embodiment, the processor may record and transmit all activity of the firearm locking assembly to a remote processor. In some embodiments, the firearm locking assembly may include an external power port for docking with an external power source in the event of battery failure. In one embodiment of the present invention, the firearm may include a keyboard having colored LED lights and a vibrating motor. In some embodiments, lights and/or vibrating motor may light or vibrate to indicate various signals, including, without limitation, when the authorized user successfully unlocks or commands the firearm, warn a child or owner to put the firearm down, or other status of the mechanism. In at least one embodiment, forward and/or rearward facing digital camera image sensors may be located in the smart safety control module or in the forward end of the receiver.
[0107] In some embodiments, an alternative power source may commence generating power when the personal identification number is entered, or when the processor communicates to the alternative power source. In some of these embodiments, the power source may include, without limitation, a battery, and a thermal power source. In one embodiment, the power source may be positioned below and adjacent to the motor.
[0108] In a non-limiting example, a military assault-type firearm processor may require a new entry code be entered every day, week or month as provided by the military. In the present non-limiting example, military or our CIA could retain control of firearms supplied to foreign fighters beyond one day.
[0109] In one alternative embodiment, the processor may be programmed to switch between modes during various times in a 24 hour period. For example, without limitation, the firearm locking assembly may switch to unlocked mode during working hours in the day, and then switch to locked mode during the night. Those skilled in the art, in light of the present teachings, will recognize that firearms used for hunting such as rifles and shotguns may include automatic relocking by releasing the restriction portion. In some embodiments, the restriction portion, however, may be replaced with the processor timing programing automatically implementing the safety mode including the motion detector, alarm portion, and locking the trigger.
[0110] FIG. 4 illustrates a typical computer system that, when appropriately configured or designed, can serve as an exemplary tracking system, in accordance with an embodiment of the present invention. In the present invention, a communication system 400 includes a multiplicity of clients with a sampling of clients denoted as a client 402 and a client 404 , a multiplicity of local networks with a sampling of networks denoted as a local network 406 and a local network 408 , a global network 410 and a multiplicity of servers with a sampling of servers denoted as a server 412 and a server 414 . It should be understood processor 212 and 312 FIGS. 2 and 3 may be used as computer system FIG. 4 .
[0111] Client 402 may communicate bi-directionally with local network 406 via a communication channel 416 . Client 404 may communicate bi-directionally with local network 408 via a communication channel 418 . Local network 406 may communicate bi-directionally with global network 410 via a communication channel 420 . Local network 408 may communicate bi-directionally with global network 410 via a communication channel 422 . Global network 410 may communicate bi-directionally with server 412 and server 414 via a communication channel 424 . Server 412 and server 414 may communicate bi-directionally with each other via communication channel 424 . Furthermore, clients 402 , 404 , local networks 406 , 408 , global network 410 and servers 412 , 414 may each communicate bi-directionally with each other.
[0112] In one embodiment, global network 410 may operate as the Internet. It will be understood by those skilled in the art that communication system 400 may take many different forms. Non-limiting examples of forms for communication system 400 include local area networks (LANs), wide area networks (WANs), wired telephone networks, wireless networks, or any other network supporting data communication between respective entities.
[0113] Clients 402 and 404 may take many different forms. Non-limiting examples of clients 402 and 404 include personal computers, personal digital assistants (PDAs), cellular phones and smartphones.
[0114] Client 402 includes a CPU 426 , a pointing device 428 , a keyboard 430 , a microphone 432 , a printer 434 , a memory 436 , a mass memory storage 438 , a GUI 440 , a video camera 442 , an input/output interface 444 and a network interface 446 .
[0115] CPU 426 , pointing device 428 , keyboard 430 , microphone 432 , printer 434 , memory 436 , mass memory storage 438 , GUI 440 , video camera 442 , input/output interface 444 and network interface 446 may communicate in a unidirectional manner or a bi-directional manner with each other via a communication channel 448 . Communication channel 448 may be configured as a single communication channel or a multiplicity of communication channels.
[0116] CPU 426 may be comprised of a single processor or multiple processors. CPU 426 may be of various types including micro-controllers (e.g., with embedded RAM/ROM) and microprocessors such as programmable devices (e.g., RISC or SISC based, or CPLDs and FPGAs) and devices not capable of being programmed such as gate array ASICs (Application Specific Integrated Circuits) or general purpose microprocessors.
[0117] As is well known in the art, memory 436 is used typically to transfer data and instructions to CPU 426 in a bi-directional manner. Memory 436 , as discussed previously, may include any suitable computer-readable media, intended for data storage, such as those described above excluding any wired or wireless transmissions unless specifically noted. Mass memory storage 438 may also be coupled bi-directionally to CPU 426 and provides additional data storage capacity and may include any of the computer-readable media described above. Mass memory storage 438 may be used to store programs, data and the like and is typically a secondary storage medium such as a hard disk. It will be appreciated that the information retained within mass memory storage 438 , may, in appropriate cases, be incorporated in standard fashion as part of memory 436 as virtual memory.
[0118] CPU 426 may be coupled to GUI 440 . GUI 440 enables a user to view the operation of computer operating system and software. CPU 426 may be coupled to pointing device 428 . Non-limiting examples of pointing device 428 include computer mouse, trackball and touchpad. Pointing device 428 enables a user with the capability to maneuver a computer cursor about the viewing area of GUI 440 and select areas or features in the viewing area of GUI 440 . CPU 426 may be coupled to keyboard 430 . Keyboard 430 enables a user with the capability to input alphanumeric textual information to CPU 426 . CPU 426 may be coupled to microphone 432 . Microphone 432 enables audio produced by a user to be recorded, processed and communicated by CPU 426 . CPU 426 may be connected to printer 434 . Printer 434 enables a user with the capability to print information to a sheet of paper. CPU 426 may be connected to video camera 442 . Video camera 442 enables video produced or captured by user to be recorded, processed and communicated by CPU 426 .
[0119] CPU 426 may also be coupled to input/output interface 444 that connects to one or more input/output devices such as such as CD-ROM, video monitors, track balls, mice, keyboards, microphones, touch-sensitive displays, transducer card readers, magnetic or paper tape readers, tablets, styluses, voice or handwriting recognizers, or other well-known input devices such as, of course, other computers.
[0120] Finally, CPU 426 optionally may be coupled to network interface 446 which enables communication with an external device such as a database or a computer or telecommunications or internet network using an external connection shown generally as communication channel 416 , which may be implemented as a hardwired or wireless communications link using suitable conventional technologies. With such a connection, CPU 426 might receive information from the network, or might output information to a network in the course of performing the method steps described in the teachings of the present invention.
[0121] Those skilled in the art will readily recognize, in light of and in accordance with the teachings of the present invention, that any of the foregoing steps and/or system modules may be suitably replaced, reordered, removed and additional steps and/or system modules may be inserted depending upon the needs of the particular application, and that the systems of the foregoing embodiments may be implemented using any of a wide variety of suitable processes and system modules, and is not limited to any particular computer hardware, software, middleware, firmware, microcode and the like. For any method steps described in the present application that can be carried out on a computing machine, a typical computer system can, when appropriately configured or designed, serve as a computer system in which those aspects of the invention may be embodied.
[0122] All the features disclosed in this specification, including any accompanying abstract and drawings, may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. Thus, unless expressly stated otherwise, each feature disclosed is one example only of a generic series of equivalent or similar features.
[0123] Having fully described at least one embodiment of the present invention, other equivalent or alternative methods of implementing firearm locks that operate by command of a processor and an access code, and include an alarm to warn against unauthorized users according to the present invention will be apparent to those skilled in the art. Various aspects of the invention have been described above by way of illustration, and the specific embodiments disclosed are not intended to limit the invention to the particular forms disclosed. The particular implementation of the firearm locks that operate by command of a processor and an access code, and include an alarm to warn against unauthorized users may vary depending upon the particular context or application. By way of example, and not limitation, the firearm locks that operate by command of a processor and an access code, and include an alarm to warn against unauthorized users described in the foregoing were principally directed to locking firearms against unauthorized users implementations; however, similar techniques may instead be applied to tools in a scientific laboratory or construction site, which implementations of the present invention are contemplated as within the scope of the present invention. The invention is thus to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the following claims. It is to be further understood that not all of the disclosed embodiments in the foregoing specification will necessarily satisfy or achieve each of the objects, advantages, or improvements described in the foregoing specification.
[0124] Claim elements and steps herein may have been numbered and/or lettered solely as an aid in readability and understanding. Any such numbering and lettering in itself is not intended to and should not be taken to indicate the ordering of elements and/or steps in the claims. | An apparatus comprises a trigger assembly for initiating a firing of a firearm. The trigger assembly comprises a trigger blocking portion. A safety selector lever is configured for joining to the firearm. The safety selector lever has an on position with the safety selector generally in a downward position and accessible to a user's thumb of a hand gripping a grip of the firearm. The safety selector is rotatable by the user's thumb to an off position where the user operates the trigger assembly while maintaining the safety selector in the off position. A safety cam is in engagement with a pivot end of the safety selector. The safety cam is configured for engaging the trigger blocking portion in the on position to inhibit the firing and for engaging the trigger blocking portion in the off position to enable the firing. | 5 |
BRIEF DESCRIPTION OF THE INVENTION
The invention pertains to machines for forming signs by routing the indicia in the sign material, usually wood, the router being guided by a template.
Signs have long been formed by routing techniques wherein the indicia is carved or cut into a panel. Routed signs are widely used in recreation areas, such as parks, campgrounds and the like, and machines for the template forming of such signs are often owned by the land proprietor, municipality or government agencies, and are often operated by relatively unskilled personnel. One machine of the aforedescribed type is shown in U.S. Pat. No. 3,171,207, and while the machine shown in this patent is of a relatively economical nature, and can be operated by relatively unskilled personnel, the fact that the panel being routed is remotely located with respect to the operator decreases his visibility,and the means for supporting the router and templates does not permit variations between router and template guide movements whereby letter variations can be produced from a common template.
It is an object of the invention to provide a router-type sign cutting machine wherein the apparatus may be operated by relatively unskilled personnel and yet indicia variations can be produced from a common template.
An additional object of the invention is to provide sign cutting apparatus utilizing templates, a template follower and a router wherein excellent router visibility during operation is provided and improved access to the sign panel supporting portion of the machine is achieved.
Another object of the invention is to provide a router-type sign cutting machine utilizing a template and template follower wherein a pantograph type linkage is employed to support the template follower and router permitting variations in movement between the template follower and router.
The sign cutter in accord with the invention includes a frame having an upper planar surface which includes clamping means for supporting the template and the panel to be routed. Along a lateral side of the frame a track is mounted upon which a carriage is linearally movable upon rollers. This carriage supports a pantograph type linkage consisting of four links, one of which is fixed to the carriage, two elements being pivotally mounted to the fixed link, and the fourth link being pivotally mounted to the two pivoted links. A template follower selectively positionable upon the links extend below for engagement with the indicia grooves of the template, and the router is fixed to the fourth link. After positioning of the template and sign panel, the operator grasps the router handle and raises and lowers the router and linkages to selectively engage and disengage the template follower with the templates and the router with the sign panel.
By relocating the template follower upon the linkages, and varying the location of the pivot points of the linkages, indicia variations may be produced from a common template configuration, and the sign cutting machine of the invention provides a wider variety of indicia from a single set of templates than machines of this type have previously offered.
BRIEF DESCRIPTION OF THE DRAWINGS
The aforementioned objects and advantages of the invention will be appreciated from the following description and accompanying drawings wherein:
FIG. 1 is a perspective view of sign cutting apparatus in accord with the invention,
FIG. 2 is a plan view of the sign cutting apparatus,
FIG. 3 is an enlarged, detail, elevational sectional view taken through the track along Section III--III of FIG. 2,
FIG. 4 is an elevational, detail, enlarged view taken through the template and illustrating the template follower, partially in section.
FIG. 5 is an exploded plan view of the linkages constituting the support for the router, and
FIGS. 6-11 are variations of the types of indicia capable of being produced by a single type of block letter templates.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The relationship of the components of sign cutting apparatus in accord with the invention is best appreciated from FIGS. 1 and 2. The apparatus includes a frame generally indicated at 10 which is of a rectangular configuration including side rails 12 and 14 interconnected at their ends by end rails 16 and stringers 18 interconnect the side rails intermediate the ends. The aforedescribed components may be formed of rectangular tubing, as apparent in FIG. 3, and are welded to form a rigid flat upper supporting surface 20. The frame members defining the supporting surface 20 are mounted upon formed legs 22 received within hollow sockets 24 welded to and extending downwardly from side rails 12 and 14.
The "rear" rail 14 serves as the support for the linear track 26. The track 26, FIG. 3, consists of a cylindrical rod 28 welded to the top of an angle 30 whose base is welded to the upper surface of the rear side rail 14. As will be appreciated from FIGS. 1 and 2, the ends of the rod 28 extend beyond the end rails 16 to provide carriage support when cutting a sign panel of a length substantially equal to that of the table.
A pair of vises or clamps are defined upon the table supporting surface 20. The template clamp 32 includes an elongated jaw bar 34 which extends parallel to the table length and is welded to the end rails 16 and stringers 18. The template jaw 36 is movably mounted on the table support surface 20 parallel to the bar 34, and consists of an angle iron laying across the support surface wherein its ends extend beyond the end rails 16, and tubular collars 38 are welded to the underside thereof. Threaded rods 40 are attached at their rear ends to the frame 10 for fixing the associated rod with respect to the frame, these rods extend through collars 38 and a wing nut 42 threaded on each rod 40 engages the associated collar whereby rotation of the wing nuts will move the jaw 36 toward the jaw 34 to clamp the template blocks 44 therebetween, as will be appreciated from FIGS. 1, 2 and 4. Preferably, the jaw 36 is of a slight arcuate configuration convexly bowing in the direction of the jaw 34 whereby template blocks clamped at the central region of the template clamp 32 will be firmly held by the jaws 34 and 36.
The sign panel 46 to be routed is clamped in the sign clamp 48 between a pair of jaws 50 and 52 each formed of an angle iron of a length greater than the frame 10 whereby the ends of the jaws extend beyond the end rails 16. Tubular collars are welded to the underside of the jaws 50 and 52 for slidably receiving the threaded rods 40, and wing nuts 54 permit the jaw rails to be located as desired upon the table surface 20. Rotation of the wing nuts permits the jaws 50 and 52 to be tightly forced toward each other to clamp the sign panel 46 between the upright portions of the jaws. Preferably, nuts 56 are mounted upon the threaded shafts 40 for engagement with one end of the collars associated with jaw 50, and the associated wing nut forces the sleeve against the nut 56 to selectively "fix" the jaw 50 relative to the frame, and the jaw 50 will be adjusted so as to be parallel to the jaws of the template clamp 32. Thus, it is usually only necessary to adjust the wing nuts associated with jaw 52 to achieve clamping and unclamping of the sign panel 46, and unless major adjustments between the widths of the jaws 50 and 52 are required the position of jaw 50 will not be changed.
An elongated carriage 58 is mounted upon the track 26, and the carriage includes a set of rollers 60 adjacent each end thereof. The rollers 60 are preferably formed of nylon or similar material, and are each rotatably mounted upon a vertical bolt-shaft assembly 62 upon either sleeve or antifriction bearings, not shown. The rollers 60, at their lower portion 64 are substantially cylindrical, and each includes a concave shoulder portion 66 of a radius substantially equal to the radius of track rod 28 whereby the rollers and carriage are supported upon the track in a manner apparent from FIG. 3. This type of mounting of the carriage upon the track permits the carriage to be readily tilted with respect to the rod 28 about its longitudinal axis, and in fact, permits the carriage to be lifted from the track, if necessary, yet the carriage closely follows the track as it is linearally displaced thereon during cutting.
A cast bracket 68 is mounted upon the carriage 58 and includes V-shaped arms which, at their outer end, are attached by fasteners to the carriage at spaced locations to rigidly attach the bracket to the carriage. The bracket 70 is of an enlarged circular configuration and includes four bolts 72 whereby link 74 is rigidly attached to the bracket portion 70 in a non-pivotal manner.
The pantograph linkage, generally indicated at 76, in addition to link 74, includes link 78 and 80, and link 82. Link 78 is pivotally mounted to the bracket portion 70 by pivot pin 84 and includes integral boss 79 having a hole 81 formed therein, while link 80 is mounted to link 74 by pivot pin 86. The link 82 is pivotally mounted to the free ends of links 78 and 80 by pivot pins 88 and 90, respectively, and link 82 includes an integral boss 92 having a hole defined therein whereby the router 94 may be fixed to the link 82 in a predetermined angular relationship.
The links 74, 78, 80 and 82, in the commercial embodiment, are of a cast construction and include ribs 96 having vertical holes 98 defined therein. The holes 98 are spaced between the pivot holes defined at the ends of the links, and in FIG. 5 the various holes 98 have been given letter designations.
The construction of the template follower is best appreciated from FIG. 4 wherein it will be noted that the template follower basically comprises of a vertical threaded member 100 which is closely received within a link hole 98 and is fixed to the associated template by means of lock nuts 102 and 104 located on opposite sides of the associated link. At its lower end, the template follower is provided with a bearing block 108 preferably formed of nylon or other self-lubricating synthetic material tightly threaded upon the follower 100. The bearing block 108 includes a pointed end 106 and a lower surface 110 adapted to engage the flat upper surface 112 of the template block 44 being followed, and in this manner the bearing block supports much of the weight of the pantograph linkage 76, but prevents the template follower end from gouging or being unduly forced into the template groove 114. The bearing block assures ease of movement of the router during tracing and cutting.
The router 94 is of a conventional type except that its base plate 116 is provided with an ear and hole whereby it may be adjustably fixed to the link boss 92 by bolt 118. The router includes handles 120 which may be grasped, and an electric trigger switch, not shown, adjacent one of the handles permits the operator to start and stop the router while using the router to raise and lower the linkage 76, and exert those forces necessary on the linkage to translate the carriage 58 along track 26 and maintain the template follower 100 within the template groove 114.
In use, the operator chooses those template blocks 44 desired to form the words that are to be cut into the sign panel 46. The template blocks are placed between jaws 34 and 36, and tightening of the wing nuts 42 forces the jaw 36 against the template blocks to tightly clamp the blocks, and the bowed configuration of the jaw 36 assures that all of the blocks will be firmly held relative to the frame.
The operator then places the sign panel 46, usually a wood board, between jaws 50 and 52, and tightening of associated wing nuts 54 will clamp the sign board.
The template follower 100 is located within the desired hole 98 by means of the lock nuts 102 and 104, and the operator will grasp the router handles 120, raise the router 94 above the panel 46, move the router and linkage 76 to align to follower end 106 with the desired template groove 114, start the router motor, and lower the router, linkage and template follower so that the template follower end 106 enters the groove 114. The router is lowered onto the panel 46 until the router base plate 116 rests upon the panel and the operator then moves the router in those directions permitted by the follower 100. It will be appreciated that the raising and lowering of the router 94 and linkage 76 is achieved by pivoting of carriage 58 about the track rod 28, and the configuration of rollers 60 readily permits such pivoting. The operator will move the router so that the template follower fully travels the extent of the associated template groove and the router will cut the desired indicia into the sign panel. The operator then lifts the router from the sign panel, and the template follower from the template groove, moves the router to the right or left to align the follower 10 with the adjacent template block groove 114 and repeats the process to cut the next letter. The pivoted interconnection of the links permits ease of movement of the router as it follows the dictates of the template, and as the carriage 58 readily moves upon the track 26 ease of router movement is assured in all directions. When the cutting is completed the operator backs off wing nuts 54 and removes the sign panel 46 from the sign clamp 48. Unloosening of the wing nuts 42 permits the clamped template blocks 44 to be removed if a similar sign is not to be cut.
It is desired that pivoting of the linkage 76 be relatively free, but the interconnection between the links must be accurate and free of "play". The pivots 84, 86, 88 and 90 constitute threaded bolts having spring washers of the bellvue type, and it would be possible to use sleeve or antifriction bearings at the pivots, but such expensive constructions are not required.
A variety of letter configurations can be produced from a single style of templete merely by changing the position of the linkage pivots, and the position of the template follower. In FIG. 6 the STANDARD template and pivot positioning is utilized wherein the cut letters correspond to the block lettering of the templates, and it is to be understood that the modifications of FIGS. 7-11 are all cut from block letters similar to those shown in FIG. 6. To produce the STANDARD cutting of the FIG. 6 pivot 84 is located in holes A and C, pivot 86 in holes B and E, pivot 88 in holes D and G, pivot 90 in holes F and H, and the template follower 100 is located in hole I.
The SLANT configuration of indicia of FIG. 7 is produced by locating pivot 84 in holes A and C, pivot 86 in holes E and J, pivot 88 in holes D and G, pivot 90 in holes H and F, and the template follower in hole I. The lettering embodiment of FIG. 8 which inclines to the left and produces an arcuate vertical upright is achieved by positioning pivot 84 in holes A and C, pivot 86 in holes B and E, pivot 88 in holes G and K, pivot 90 in holes F and L, and the template is located in hole 81.
The RUSTIC configuration of FIG. 9 is achieved by placing pivot 84 in holes A and C, pivot 86 in holes E and J, pivot 88 in holes G and K, pivot 90 in holes F and H and the follower in hole 81.
FIG. 10 represents a LEFTY modification achieved by placing pivot 84 in holes A and C, pivot 86 in holes B and E, pivot 88 in holes D and G, pivot 90 in holes F and L and the follower in hole 81.
The SCRIPT modification of FIG. 11 is achieved by placing pivot 84 in holes A and C, pivot 86 in holes E and M, pivot 88 in holes D and G, pivot 90 in holes F and H and the template follower in hole I.
It will therefore be appreciated that the cutting machine of the invention may be operated by a relatively unskilled operator, provides excellent visibility during cutting, is of economical construction, and permits a wide variety of indicia modifications from the single template form. The conical end 106 will enter the template groove before the router tool engages the sign panel and this fact minimizes errors and the vertical flexibility of the linkage permits uneven sign panels to be cut.
It is understood that various modifications to the inventive concepts may be apparent to those skilled in the art without departing from the spirit and scope of the invention. | The invention pertains to apparatus for forming signs with a motor driven router. A frame defines a surface for supporting the sign panel to be routed, usually wood, and for supporting the letter forming templates. A carriage linearally movable upon the frame supports a polygonal, four-sided linkage, a template follower is mounted upon one of the links, and the router is also link-mounted. By varying the position of the linkage pivot points relative to each other, and the location of the template follower, a variety of letter styles can be produced from a single template, and a characteristic of the apparatus lies in the excellent visibility provided of the router during operation. | 8 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to computer systems and more particularly to instruction handling circuitry in computer systems.
The invention finds particular utility in computer systems where instructions are fetched a byte at a time and bytes are fetched successively to completely fetch an instruction. In such computer systems it has been the practice to fetch one instruction byte per machine cycle. This was accomplished by accessing storage during a first portion and updating the storage address during a second portion of the machine cycle. The instruction byte or segment retrieved from storage is entered into a selected register of the CPU. For example, the first byte of an instruction which is fetched is usually the operation code (OP code) byte and it is entered into the operation register. The IAR is updated and then the next byte of the instruction is fetched and placed into another register. The process continues until all bytes of the instruction are fetched and placed into appropriate registers in the CPU. This process is called the I phase or I fetch. The instruction is then executed according to the operation specified by the OP code. The execution of an instruction is the E phase.
2. Description of the Prior Art
The prior art techniques for speeding up the instruction processing rate include pre-fetching instructions so as to overlap instruction fetch and instruction execution phases. Another technique is to fetch more bytes of the instruction at any one time. These prior art techniques are effective but are relatively more expensive. This is because they require many parallel paths or wider paths for data as well as attendant control circuitry. In the present invention there is one additional data path, one additional register, and an auxiliary ALU together appropriate controls; however, the data paths, except for the paths from the additional register and auxiliary ALU, are one byte or segment wide. The present invention fetches only one byte or segment of the instruction at a time; however, because of the additional data path from storage; i.e., one that bypasses the register which feeds the regular ALU, it is possible to enter the fetched byte in the destination register, such as the OP register, faster. The auxiliary ALU can update the IAR in one operation and hence the IAR can be updated earlier witin a machine cycle. This only involves using an earlier clock signal for clocking the IAR. With the IAR updated earlier it is possible to initiate and complete a second storage access within the same machine cycle. Since the bytes are still fetched successively, the data path to the destination registers did not have to be widened.
SUMMARY OF THE INVENTION
The principal objects of the invention are to provide improved instruction fetching apparatus which:
a. increases the instruction fetch rate in a computer system where bytes or segments of an instruction are fetched successively one byte or segment at a time;
b. can be incorporated into an existing computer system and still permit normal instruction rate processing; and
c. is relatively inexpensive.
The foregoing objects are achieved by shortening the data path timewise from data storage to the destination registers and by updating the instruction address register in one operation and earlier in the machine cycle. Normal rate instruction processing is preserved by generating an idle or dummy half cycle during which time the CPU is idle, i.e., no storage fetches, no IAR updates, etc. take place.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram illustrating the arrangement of FIGS. 1a, 1b and 1c which taken together are a schematic diagram of the data flow in a computer system incorporating the present invention;
FIG. 2 is a block diagram illustrating the arrangement of FIGS. 2a, 2b, and 2c which taken together are a schematic logic diagram of logic circuitry for developing control signals for fast and normal instruction rate processing;
FIGS. 3a and 3b with FIG. 3a disposed to the left of FIG. 3b taken together are a schematic logic diagram of the logic circuitry for controlling entry of data into the auxiliary B register;
FIG. 4 is a block diagram illustrating the arrangement of FIGS. 4a, 4b, 4c, and 4d which taken together are a logic circuit diagram of the CPU LSR address circuitry;
FIG. 5 is a logic circuit diagram of the LSR WRITE GATE circuitry;
FIG. 6 is a schematic diagram illustrating instruction formats of the different types of instructions;
FIG. 7 is a timing diagram showing the instruction cycles required to fetch the different types of instructions;
FIG. 8 is a timing diagram illustrating the I-OP and I-Q cycles of different types of instructions;
FIG. 9 is a timing diagram illustrating the I-H and I-L cycles for different types of instruction, and,
FIG. 10 is a timing diagram illustrating the I-X cycles for different types of instructions.
DESCRIPTION OF THE INVENTION
With reference to the drawings and particularly to FIG. 1, the invention is shown by way of example as being incorporated into a computer system of the type shown and described in U.S. Pat. No. 3,828,327, dated Aug. 6, 1974 for Simplified Storage Protection and Address Translation Under System Mode Control In A Data Processing System by Berglund et al. and in the IBM 5415 Processing Unit Theory -- Maintenance -- Diagrams manual (Form No. SY31-0367-2), copyrighted 1974 by International Business Machines Corporation which are incorporated herein by reference. The invention enhances data processing of the type described in the aforementioned references by increasing the instruction rate. While this may be considered a performance enhancement, it is also a functional enhancement in that the multiprogramming capabilities of the system can be expanded without performance degradation. In other words, the invention makes it feasible to expand the functional programming capabilities of the system.
Main storage unit 10, FIG. 1, stores both instructions and data in the form of bytes, each byte consisting of 8 bits of data. The instructions are stored in storage 10 at addressable byte locations according to a program, whereby the instructions will be fetched and executed in a predetermined sequence to perform a particular job or operation. Basically, an instruction must be fetched and then executed. The number of machine cycles required to fetch an instruction and execute it depends upon the type of instruction.
The present invention is particularly concerned with the fetching of instructions rather than the execution of them. The different types of instructions which are used in the referenced computer system are shown in FIG. 6. In this particular example each instruction has an operation code (OP code) byte and a Q code byte. In addition to these bytes there are either address bytes or a control byte within an instruction. The address bytes are for addressing storage to fetch data or operands to be used in the execution phase of the instruction. The control byte is used for command purposes such as halt program level, advance program level, jump on condition or start I/O. The instructions vary in length from 3 to 6 bytes depending upon the type of instruction.
The four high order bits of the OP code byte are encoded to identify to the central processing unit (CPU) the format of the instruction and the type of addressing which is to take place, i.e., direct or indexed. Instructions having one address, i.e., 2 bytes for an address to fetch one operand from storage, have OP codes with either bits 0 and 1 both or bits 2 and 3 both ones. Instructions containing two storage addresses have OP codes where one of the bits 0 and 1 is a zero or one of the bits 2 and 3 is a zero. Instructions having OP codes where bits 0, 1, 2 and 3 are all ones are command instructions. Command instructions do not contain addresses for addressing storage 10.
The meaning of the Q byte of an instruction depends upon the type of instruction. For instructions having one address, the Q byte can be immediate data, a bit selection mask, a register selection address, a branch condition, or an I/O device address and data selection. The Q byte of instructions containing two addresses can be a field length indicator or half byte selector. The Q byte of command instructions can be a halt identifier (tens digit), an advance program level condition, a jump condition, or an I/O device address.
The computer system in this example has a fixed machine cycle of 1.52u seconds. This machine cycle is formed by a group of clock times 0-8 generated by clock 11, FIG. 1. Clock times 0 and 1 are each 200 nano (n) seconds (s) and the remaining clock times 2-8 are each 160ns. Each clock time is subdivided into phase times, each phase being 40ns. Hence, clock times 0 and 1 have phases A, B, C, D and E and clock times 2-8 have phases A, B, C and D. Details of clock 11 are shown on page 2-1 of manual SY31-0367-2.
In the past each I cycle was one machine cycle long. Each machine cycle was divided into five functional time periods. Clock 0 was used to address storage. The storage address contained in the local storage registers (LSR's) 100, i.e., in the instruction address register (IAR) was transferred to storage address register (SAR) 20. The second functional time was clock 1 and 2 times and was a miscellaneous time for processing data through the arithmetic and logic unit (ALU) 50 during the delay or the time it takes for the addressed data to emerge from storage 10.
The next functional period was the compute time consisting of clocks 3 and 4. Compute time was for combining the data from storage 10 and entered into B register 25 with the contents of A register 30 by means of ALU 50. The results at the ALU output were available for transfer into storage.
The fourth and fifth functional times were used for address modification, i.e., the low byte of the selected LSR was updated (modified) and then the high byte was updated.
In the present invention the machine cycle has remained fixed and the functional times have been changed. The clock and phase times also remain the same. During the first part of a machine cycle, clock times 0 and 1, FIGS. 1 and 8. IAR in LSR's 100 is selected and the storage address in the IAR is transferred via HI and LO buses 105 and 110 into SAR 20. The address in SAR 20 addresses storage via main storage address register 21. The two registers 20 and 21 exist because of address translation capability which is not pertinent to the present invention, but is described in the aforementioned U.S. Pat. No. 3,828,327. A memory or storage cycle takes place from clock time 1 phase B through clock time 3 phase A. The byte of data fetched from storage 10 is entered into fetch data register 12 and becomes available to bus 14 via error correcting code circuitry 13. The OP code byte addressed transfers from storage over bus 14 to an auxiliary ALU 60 and from ALU 60 via gate 80 and bus 85 into OP register 90 during clock 3 time.
The address in the IAR is updated during the memory cycle. The contents of the IAR are loaded into an auxiliary B register 26 during phases D and E of clock 0 time. The path from the IAR into the auxiliary B register is via buses 105 and 110. The contents of the auxiliary B register 26 are entered into the auxiliary ALU 60 via bus 27 which is 16 bits wide. Auxiliary ALU 60 increments the address from register 26 and the incremented address is returned to the IAR during phase D of clock 1 time. Note that the incrementing operation of the IAR does not conflict with the data taken from storage and passed through the auxiliary ALU 60 because data is not available at the storage output until the end of phase A of clock 3 time.
Although other activities take place during the I-OP cycle, i.e., the contents of condition register 115 are stored in the program status register which is one of the LSR registers 100, the I-OP cycle is completed at the end of phase B of clock 4 time. The I-OP cycle is the same for any type of instruction.
The next I cycle within the machine cycle is dependent upon the particular type of instruction. If the instruction is one containing one address, two addresses, or a command instruction, then the next I cycle is an I-Q cycle. If the instruction is a halt program level, an advance program level, or an I/O instruction, the next I cycle is a dummy I cycle. This is illustrated in FIG. 8 which shows an I-OP cycle followed by an I-Q cycle for the one address, two address and non I/O command instructions and an I-OP cycle followed by a dummy I cycle for halt program level, advance program level and I/O instructions. A dummy I cycle, of course, is a dummy or idle machine half cycle.
Assuming that the OP code defines an instruction having one address, two addresses, or a command then the I-Q cycle immediately follows the I-OP cycle and starts at clock 4 time, phase C. The IAR is selected in the same manner as it is for the I-OP cycle. SAR is loaded with the contents of the IAR starting at phase D of clock 4 time. The memory or storage cycle begins at phase C of clock 5 time. The Q byte retrieved from storage is entered into Q register 95 during clock 8 time. The Q byte in storage 10 passes into the fetch data register 12 and from there to bus 14 via the error correcting code circuitry 13. The Q byte then enters the auxiliary ALU 60 and passes through it to Q register 95 via gate 80 and bus 85.
The address in the IAR is updated during the I-Q cycle by transferring the address into the auxiliary B register 26 during phases D and A of clock 4 and 5 times respectively. The address is then transferred into the auxiliary ALU 60 via bus 27 and incremented by 1 and returned to the IAR via gate 80. The I-Q cycle terminates at the end of clock 8 time. It is thus seen that an I-OP cycle and an I-Q cycle are completed within a single machine cycle where heretofore the I-OP cycle took one machine cycle and the I-Q cycle took another machine cycle.
If the instruction being fetched is a halt program level, an advance program level or an I/O instruction as determined by decoding the OP code byte, then a dummy I cycle is taken. This is because the circuitry related to these instructions can not take advantage of the accelerated I fetch time without a major modification. Therefore, for compatability purposes the I-Q cycle does not start at phase C of clock time 4 but instead a dummy I cycle is taken and during the dummy I cycle, no activity takes place within the CPU or storage. The dummy I cycle terminates at clock 8 time and the I-Q cycle starts at the following clock 0 time.
The dummy I cycle or dummy machine half cycle occurs under control of cycle control circuitry 120. The details of cycle control circuitry 120 which are pertinent to the present invention are shown in FIGS. 2a and 2b. The dummy half cycle signal is present when trigger 132 is in the set state. The data input of trigger 132 is connected to the output of OR circuit 130 and its clock signal is connected to the output of AND circuit 131. The AC reset input of trigger 132 is connected to inverter 133 and the DC reset input is connected to the output of OR circuit 134. AND circuit 131 receives a fast I cycle signal, a clock 4 time signal, and a phase B signal. The fast I cycle signal comes from OR circuit 136 which receives the I-OP, the I-Q, the I-H1, the I-L1, the I-H2, the I-L2, the I-X1 and the I-X2 signals. Thus, a dummy half cycle can take place during any of the I fetch times corresponding to the inputs into OR circuit 136 and at clock 4, phase B time. Whether or not a dummy half cycle will occur, of course, depends upon whether OR circuit 130 is providing a signal to the data input of trigger 132.
OR circuit 130 receives the output of OR circuit 128. The inputs into OR circuit 128 are signals indicative of a Start I/O instruction, a Load I/O instruction, a Sense instruction, a Halt Program Level instruction, and a Test I/O or Advance Program Level instruction. The origin of these signals is set forth in manual SY31-0367-2 at page 2-27 thereof.
A dummy half cycle will also occur after an I-X1 cycle for an instruction having one address. This is accomplished by means of AND circuit 127 which also feeds OR circuit 130. The origin of the signals applied to AND circuit 127 is set forth on page 2-37 of manual SY31-0367-2. A dummy half cycle also follows an I-X2 or I-L2 cycle of an instruction having two addresses, see FIGS. 9 and 10. This condition is detected by AND circuit 129. The origin of the signals applied to AND circuit 129 is shown on page 2-37 of manual SY31-0367-2.
Dummy half cycles also occur for program checks, machine cycle step, and for diagnostic mode. The origin of the program signal is shown on page 2-42 of manual SY31-0367-2. The machine cycle step signal comes from a manually operated switch located on the computer system console (see page 7-7 of manual SY31-0367-2).
A dummy half cycle occurs when in the diagnostic mode after any of the I cycles which generate the fast I cycle signal. The diagnostic mode signal comes from latch 125 which has its set input connected to AND circuit 123 and its reset input connected to AND circuit 124. AND circuit 123 receives an input from AND circuit 121, an IR cycle input and an input from inverter 122. AND circuit 121 receives a Command CPU Instruction signal and bit one of the Q byte. Inverter 122 receives a signal from bit 6 of ALU 50. The origin of the IR cycle signal is shown on page 2-2 of manual SY31-0367-2. AND circuit 124 for resetting latch 125 has an input from AND circuit 121 and it receives the IR cycle signal and the ALU bit 6 input.
The output of OR circuit 136 for providing the fast I cycle signal is also applied to an input of AND circuit 137. AND circuit 137 also receives an input from OR circuit 130 via inverter 135 and receives a clock 4 input. The output of AND circuit 137 is an Allow Half Cycle OPS signal.
FIGS. 2b and 2c show the details of gate 80 and the controls thereof. Gate 80 includes OR circuits 81 and 82 for passing high and low bytes respectively. The output of OR circuit 82 is bus 85 and as previously mentioned it feeds OP register 90, Q register 95, and the low byte input of the LSR's 100. OR circuit 82 has inputs from AND circuits 83 and 84. AND circuit 83 controls the high speed path from auxiliary ALU 60. Bits 8-15 on bus 61 are split off via bus 62 and applied to AND circuit 83. AND circuit 83 is conditioned by a signal from AND circuit 140 which receives the fast I cycle signal from OR circuit 136 and also receives an input from inverter 141. Inverter 141 is fed by AND circuit 142 which receives the I-OP cycle signal and a clock 2 signal. Thus, AND circuit 140 will be satisfied during fast I cycle when in the I-OP cycle at a clock time other than clock 2 time.
Referring again to FIG. 8 as well as FIG. 2b it is seen that the OP code byte on bus 14 can be entered into the OP register via ALU 60, bus 61, bus 62, AND circuit 83, OR circuit 82 and bus 85 during clock 3 time. It was also previously mentioned that the condition register 115 is loaded into an LSR 100 during clock 2 time. The contents of the condition register 115 are loaded into a selected LSR by first entering A register 30 via bus 116. The condition register contents then pass from A register 30 into ALU 50 and out of ALU 50 via bus 51 to AND circuit 84. AND circuit 84 is conditioned by the output of inverter 143 which is fed by AND circuit 140. Therefore, since AND circuit 140 is not conditioned during clock 2 time during fast I cycle and I-OP cycle, inverter 143 will condition AND circuit 84 to pass the condition register contents via OR circuit 82 and over bus 85 to the low byte of the selected LSR 100.
Although the output of ALU 50 is also applied to AND circuit 88, this AND circuit is not conditioned during fast I cycle because of inverter 144. Thus, gate 88 is primarily used to pass the byte from ALU 50 during execute cycles of an instruction and during I/O instructions.
AND circuit 86 controls the passage of the high byte from auxiliary ALU 60. AND circuit 86 is essentially conditioned anytime there are two bytes passed from auxiliary ALU 60. Two bytes are passed from auxiliary ALU 60 when the IAR is being updated and during an index cycle. An index cycle is used for adding a one byte displacement to an index register to form a new storage address. The index register is one of the LSR registers 100. AND circuit 86 is conditioned during an index cycle by an I-X signal during clock 3 or 8 time via OR circuit 145. OR circuit 145 also receives a signal from OR circuit 149 which has an output when the IAR is to be updated. It will be recalled that the IAR is updated during clock 0-1 time and during clock 4CD to clock 6 time. Latch 151 is set during clock 0-1 time under control of AND circuit 150. AND circuit 150 receives the clock 0-1 time and a phase CD signal. The output of latch 151 is applied to AND circuit 148 which also receives the fast I cycle signal. Latch 151 is reset under control of a clock 2 signal. AND circuit 147 controls the conditioning of AND circuit 86 when in the fast I cycle, but not in a dummy half cycle. Thus, AND circuit 147 receives the fast I cycle signal and has an input from inverter 146 which receives the dummy half cycle signal. AND circuit 147 receives a timing signal 4CD to clock 6 time.
Gate 87 controls the passage of the low byte from auxiliary ALU 60 during I-H1 and I-H2 cycles. The I-H1 and I-H2 cycles are for passing the high bytes of operand addresses one and two from storage to selected LSR's 100. Gate 87 is controlled by AND circuit 153 which receives the fast I cycle signal and the output of inverter 152. Inverter 152 is fed by OR circuit 145.
The incrementing of the contents of the IAR by auxiliary ALU 60 is accomplished under control of AND circuit 156 and OR circuits 160, 161, and 164. Auxiliary ALU 60 has function control inputs A, B, C, and carry. The auxiliary ALU 60 will perform an increment by one operation by forcing a carry and providing zero inputs to A, B, and C. The carry is forced via OR circuit 164 under control of AND circuits 162 and 163.
AND circuit 162 receives the fast I cycle signal and the output of latch 151. Hence, a carry will be forced into auxiliary ALU 60 for incrementing the IAR during phase C and D of clock 0-1 time. AND circuit 163 also receives the fast I cycle signal and receives a clock 4C to 6 timing signal and an output from inverter 165 which receives the dummy half cycle signal. Thus, AND circuit 163 controls the forcing of the carry into auxiliary ALU 60 for updating the IAR during clock 4CD to 6 time. AND circuit 156 is not active at this time because it receives an input from exclusive OR circuit 155 which has a clock 2-3 input and an input from latch 154. Latch 154 is set by a clock 7-8 timing signal and is reset by the output of latch 151. The other inputs into AND circuit 156 include a branch or jump signal and an I-Q cycle signal.
It should be noted that the output of AND circuit 156 also feeds OR circuit 161. The other input into OR circuit 161 comes from AND circuit 159 which receives the fast I cycle signal and signals from exclusive OR circuit 155, and inverters 158 and 165. Inverter 158 is fed by an I-X cycle signal. Since AND circuit 159 is fed by exclusive OR circuit 155, it will not be providing an output for the B control input of auxiliary ALU 60 at this time. OR circuit 160 is fed by AND circuits 156 and 157. AND circuit 157 receives the I-X cycle signal and outputs of exclusive OR circuit 155 and inverter 165. Thus, AND circuit 157 will not be providing a signal to OR circuit 160 for activating the A control input of auxiliary ALU 60 at this time.
It should be noted that auxiliary ALU 60 passes the data from bus 14 directly to its output bus 61 when the B control input is receiving a signal and there are no signals present at the A, C, or carry inputs. AND circuit 159 must and will be active to pass the data on bus 14 directly through the auxiliary ALU 60 to bus 61 when not in a dummy half cycle and not during an I-X cycle.
In order to increment the contents of the IAR it is necessary to transfer them into auxiliary B register 26. Auxiliary B register 26 is loaded under control of OR circuit 175, see FIG. 3. LSR HI bus 105 feeds AND circuit 176 which is representative of a group of AND circuits; one for each bit of the bus. The output of AND circuit 176 feeds AND circuit 178 which is conditioned by the output of OR circuit 175. AND circuit 176 is conditioned by inverter 177 which is fed by AND circuit 173. The LSR LO bus 110 is shown as feeding into AND circuits 179, there being one AND circuit for each bit of the bus. These AND circuits are also conditioned by the output of inverter 177 and feed AND circuits 180. AND circuits 180 are controlled by the output of OR circuit 175. It should be noted that bits 2 and 7 from the condition register can also enter the auxiliary B register 26 via AND circuits 179 and OR circuits 183 and 184.
OR circuit 175 receives a Load SAR signal from OR circuit 188 which is fed by AND circuits 186 and 187. Thus, the load SAR signal is used for loading the auxiliary B register 26 as well as SAR 20. AND circuit 186 receives the Allow Half Cycle OPS from AND circuit 137, FIG. 2a, and a clock 4D-5A timing signal. AND circuit 187 receives a clock 0 signal and a phase DE signal. Thus, register 26 can be loaded during half cycle operations under certain timing conditions. Register 26 can also be loaded under control of AND circuit 171 which receives an I-X Cycle Internal signal, a Phase CD Pwd A signal and a signal from OR circuit 170. OR circuit 170 receives clock 2 and clock 7 to Channel signals. The other input into OR circuit 175 is from AND circuit 174. AND circuit 174 receives the Phase CD Pwd A signal and an output from AND circuit 173. AND circuit 173 receives the NOT dummy cycle signal, an I-Q Cycle Pwd signal, a branch or jump signal, and a signal from OR circuit 172. OR circuit 172 receives clock 2 and clock 6 signals.
The Allow Half Cycle OPS signal from AND circuit 137, FIG. 2a, is also used for controlling the I-OP and I-Q triggers 55 and 56 via AND circuit 195 and OR circuit 197. The normal path for controlling triggers 55 and 56 is via AND circuit 196 and OR circuit 197. AND circuit 195 receives the Machine Advance signal and a phase CD signal as well as the Allow Half Cycle OPS signal. AND circuit 196 receives a clock 0 signal, an Inhibit Advance signal and a Machine Advance signal.
The Allow Half Cycle OPS signal is also used for controlling the setting of latch 190, FIG 3. The output of latch 190 is applied to AND circuit 191 which also receives a clock 5 signal. AND circuit 191 feeds the data input of trigger 192 which receives a phase C signal at its clock input. The output signal from trigger 192 is a BSM SEL signal for activating main storage 10.
As previously mentioned, no CPU or main storage activity takes place during a dummy half cycle. Thus, the dummy half cycle signal from trigger 132 is applied to OR circuit 202 FIG. 4b. The output of OR circuit 202 is used for inhibiting AND circuit 205 via OR circuit 203 and inverter 204. The output of OR circuit 202 also inhibits AND circuits 207, 208, 209 and 210 via inverter 206. OR circuit 202 uses inverter 215 for inhibiting AND circuits 216 and 217. Or circuit 202 inhibits AND circuits 219, 221, and 223 via inverters 218, 220, and 222, respectively. The logic circuitry just described is for normally addressing the CPU LSR's of LSR's 100.
The dummy half cycle signal is also used to inhibit LSR Write LO Gate and LSR Write HI Gate signals. The dummy half cycle signal is applied to OR circuit 225, FIG. 5 and its output is applied to inverter 226. The output of inverter 226 is applied to AND circuits 227, 228, and 229 which feed OR circuit 230 and to AND circuits 231 and 232 which feed OR circuit 233. The LSR Write LO Gate and LSR Write HI Gate signals are taken from OR circuits 230 and 233 respectively.
From the foregoing it is seen that the invention provides fast and normal rate I cycles depending upon the type of instruction being fetched. The fast rate I cycles improve the rate of instruction processing without a significant change in the hardware of the computer system which is responsive to the instructions processed at the fast rate. On the other hand, hardware such as the controls for I/O devices which would require extensive changes to take advantage of the faster instruction rate, can be operated without any change by processing the associated instructions at the normal rate. The normal rate is achieved by use of dummy I cycles or machine half cycles. | Instruction processing rate in a computer system is increased by providing a high speed data path to central processing unit (CPU) registers and including an auxiliary arithmetic and logic unit to enable updating the instruction address register (IAR) in one operation concurrently with a storage fetch whereby two storage fetches can be made within a single machine cycle. Normal instruction rate processing is retained by generating idle or dummy half cycles to enable a single storage fetch per machine cycle and thereby maintain flexibility for I/O instruction processing, for diagnostic purposes and for fetching the last byte or segment of an instruction having an odd number of bytes or segments. | 6 |
REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of application Ser. No. 09/141,812, filed Aug. 28, 1998.
FIELD OF THE INVENTION
[0002] The present invention relates generally to the removal of residues during fabrication of integrated circuits. More particularly, the invention relates to the removal of residues after opening vias for contact information.
BACKGROUND OF THE INVENTION
[0003] During fabrication of integrated circuits, it is often necessary to construct vias to interconnect metal lines or other devices in the semiconductor. These vias, are etched through an insulating layer to expose a metal or other conductive element below. The insulating layer is typically a form of oxide, such that fluorocarbons are used to etch through the insulating layers. In plasma etch reactors, the wafer is often subjected to an electrical bias to obtain more uniform etching. Biasing the wafer also greatly increases the rate of etching.
[0004] Organic residues are left in the via after the etching process. These residues can compromise the reliability of the contact to be formed within the via, and should therefore be removed. Typically, the residue is removed with an organic stripper, which simultaneously strips the resist mask. Such organic strips are expensive and difficult to dispose, however, such that oxygen plasma is more currently favored to burn off the resist and etch residue.
[0005] More recently, fluorine has been added to an oxygen plasma strip, aiding the complete removal of the residue by undercutting the oxide walls. Unfortunately, the fluorine also undercuts the metal and can also laterally recess upper layers of the metal. If this lateral recessing causes a gap between the dielectric and the metal line below, filling the via with conductive material to form a contact between two layers will be incomplete, and the resulting contact will have reliability problems.
[0006] U.S. Pat. No. 5,661,083 discloses reactive ion etches to clear the via walls. These etches also entail reliability issues due to metallic recessing, as well as safety problems from use of explosive mixtures and dimension control.
[0007] Accordingly, there is a need for a method of effectively removing residue from etching a via. Desirably, the method should protect the via surfaces, and particularly the metal layers exposed by the via etch.
SUMMARY OF THE INVENTION
[0008] In accordance with one aspect of the invention, a method is provided for fabricating a conductive contact through an insulating layer in an integrated circuit. A via is first etched through the insulating layer to expose a first metal element. The via sidewall is then exposed to a vapor formed, at least in part, from ammonia. Thereafter, a conductive material is deposited into the via.
[0009] In accordance with another aspect of the invention, a method is disclosed for removing etch residue from the via after the via has been etched through an insulating layer in a partially fabricated integrated circuit assembly. The etch residue is exposed to a plasma formed from a non-explosive source of hydrogen and oxygen. In accordance with still another aspect of the invention, a method is provided for forming an integrated circuit. A patterned mask is formed from a resist layer over a dielectric layer. A via is then formed in the dielectric layer by etching through the mask. This via is cleaned by exposure to a plasma generated from ammonia.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] These and other aspects of the invention will be apparent to the skilled artisan from the detailed description and claims below, taking together with the attached drawings, wherein:
[0011] [0011]FIG. 1 is a cross-sectional view of a partially fabricated integrated circuit, wherein a conducting layer, and a dielectric layer have been formed over a substrate;
[0012] [0012]FIG. 2 illustrates the integrated circuit of FIG. 1 following deposition patterning of a mask of a layer;
[0013] [0013]FIG. 3 illustrates the integrated circuit of FIG. 2 after a Via has been etched through the dielectric layer, leaving residue lining the via;
[0014] [0014]FIG. 4 illustrates the integrated circuit of FIG. 3 after removal of the residue and mask layer in accordance with the preferred embodiment; and
[0015] [0015]FIG. 5 illustrates the integrated circuit of FIG. 4 after the via has been filled with conductive material to form a contact.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0016] The present invention is directed to cleaning surfaces of integrated circuits during fabrication. While illustrated in the context of removing residue from within a via following a contact etch, the skilled artisan will recognize many other applications for the methods disclosed herein.
[0017] [0017]FIG. 1 shows an insulating layer 10 , such as BPSG. While not shown, the insulating layer 10 is formed over a substrate in which electrical devices are formed (e.g., integrated transistors). The substrate may be a semiconductor such as silicon or gallium arsenide, or it may be an insulating layer if Silicon-On-Insulator (SOI) or a similar technology is used. For example, the insulator may be sapphire, if Silicon-On-Sapphire (SOS) is used. The term substrate is therefore meant to be inclusive of various technologies known to those skilled in the art. The insulating layer 10 thus covers and electrically isolates the electrical devices from one another and from wiring layers to be formed.
[0018] A first conductive layer 12 , formed over the insulating layer, may be a metal, silicide, or other suitable material. Some examples of suitable metals for forming the first conductive layer 12 include, but are not limited to, copper, gold, aluminum, silicon, and the like. Mixtures of metals are also suitable for forming a conducting layer. Some suitable mixtures of metals include, but are not limited to, aluminum alloys formed with copper and/or silicon. Some exemplary methods of depositing the conductive layer include, but are not limited to, Rapid Thermal Chemical Vapor Deposition (RTCVD), Low Pressure Chemical Vapor Deposition (LPCVD), and Physical Vapor Deposition (PVD).
[0019] The first conductive layer 12 is electrically connected to the underlying devices of the integrated circuit assembly. In the illustrated embodiments, a contact 14 is formed integrally with the first conductive layer 12 . Such an integral contact is typically formed between wiring or conducting layers. In other arrangements, however, the contact makes direct contact to a transistor active area within the substrate. Such contacts to active areas typically comprise polysilicon or tungsten plugs, as will be recognized by the skilled artisan.
[0020] An anti-reflective coating (ARC) 16 is preferably formed adjacent to the first conductive layer 12 . The anti-reflective 16 coating can comprise any of a variety of materials suitable for its purpose. As is known in the art, the ARC 16 serves to reduce reflections of light energy during photolithographic patterning prior to etching the metal layer 12 . The anti-reflective coating 16 of the illustrated embodiment comprises titanium nitride (TiN).
[0021] An interlevel dielectric layer (ILD) 18 is then deposited over the anti-reflective coating 16 . The dielectric layer 18 preferably comprises a form of silicon oxide and the illustrated ILD 18 is formed by reaction of TEOS (tetraethyl orthosilicate) in a plasma deposition chamber 18 . In other arrangements, silicon oxide can be formed by reaction between silane and nitrous oxide or oxygen. The skilled artisan will understand, however, that a variety of materials can be used for the ILD 18 .
[0022] With reference to FIG. 2, a suitable masking material is deposited onto the dielectric layer 18 of the integrated circuit assembly. In accordance with conventional photolithographic processes, the mask material preferably comprises a photo-definable organic resist layer 20 . FIG. 2 shows the resist layer 20 after patterning to form an opening 22 . In practice, it will be understood that multiple openings are formed across the wafer.
[0023] As shown in FIG. 3, a via 24 is then etched through the dielectric layer 18 to expose a circuit element below. The etch process can be performed in a variety of manners. Preferably, the etch is directional and includes a physical component, thereby facilitating vertical sidewalls. As is conventional, the contact opening is “overetched” to ensure each opening exposes the underlying circuit across the substrate, despite any non-uniformities in ILD 18 thickness across the wafer. Furthermore, the via 24 preferably extends through the anti-reflective coating 16 to expose the conductive layer 12 .
[0024] In the illustrated embodiment, the etch comprises a plasma etch, and more particularly a reactive ion etch (RIE) formed of a fluorocarbon chemistry (e.g., CF 4 ). Such an etch can be performed, for example, in a magnetically enhanced RIE chamber commercially available from Applied Materials, Inc. of Santa Clara, Calif. under the trade name “5000 MXP.” Exemplary parameters include a chamber pressure of about 150 mTorr, RF power of about 900 W, magnetic field strength of about 50 Gauss, with the following gas flows: 111 sccm of Ar; 28 sccm of N 2 ; 15 sccm of CHF 3 ; and 60 sccm of CF 4 . The skilled artisan will recognize, however, that each of the above noted parameters can be varied significantly, and furthermore that different etch chemistries can be used, while still obtaining effective anisotropic etching of the via 24 .
[0025] The wafer is biased during the preferred RIE, thus increasing the rate of etching and the directionality of the etch. Furthermore, biasing physically etches through the ARC 16 without the aid of metal etchants such as chlorine. By the same token, however, the sputtering effect of this physical etch increases the metal content of the residue.
[0026] As also shown in FIG. 3, an etch residue or debris 26 is left in the via 24 . after the etch process. The residue 26 typically includes the chemical species used to create the etch plasma, in addition to atoms from the conductive layer 12 , the anti-reflective coating layer 16 , the dielectric layer 18 , and the resist layer 20 . The presence of the resist 20 contributes to the creation of a complex polymeric matrix, incorporating metals and etchant components. As the residue 26 interferes with electrical contact through the via 24 , it should be removed.
[0027] Conventional, post-etch cleaning steps are unsatisfactory, however. The metal content within the polymeric matrix makes the removal difficult. Moreover, the oxygen plasma tends to oxidize the residual metals as well as the exposed conductive layer 12 . The addition of fluorine, while helpful in removing the residue, laterally attacks the preferred TiN anti-reflective coating 16 and also increases the fluorine at the surface of the underlying metal 12 .
[0028] [0028]FIG. 4 shows the contact after the resist 20 and residue 26 have been removed. In accordance with the preferred embodiment of the present invention, the residue 26 is treated to aid removal of the residue 26 without excessive oxidation. Preferably, the residue 26 is exposed to a vapor or plasma with a reducing chemistry, more preferably including a nonexplosive source of hydrogen atoms. In the illustrated embodiment, the residue 26 is exposed to a plasma formed of ammonia (NH 3 ). In other arrangements, water can also serve as a nonexplosive source of hydrogen.
[0029] Preferably, the plasma also comprises air or oxygen. The residue treatment is thus combined with burning the resist layer 20 . Due to use of a nonexplosive source of hydrogen atoms, in combination with the oxygen or air, the preferred embodiment can safely treat the residue 26 while at the same time removing the resist layer 20 from the surface of the integrated circuit. In other arrangements, where the resist strip is separately performed, methane or hydrogen gas could be used to treat the residue 26 .
[0030] The hydrogen in the plasma treatment passivates the metal atoms present in the residue, as well as the underlying first conductive layer 12 , thus inhibiting oxidation of the metal. At the same time, the preferred plasma treatment facilitates removal of the residue 26 .
[0031] The plasma can be generated with a variety of instruments. For example, the invention has been implemented in microwave strippers sold under the trade names MCU™ or Gemini™, produced by Fusion of Rockville, Md. Aspen II™ produced by Matson of California, is a commercially available inductively coupled plasma reactor. Each of these reactors have been found suitable for generating a plasma suitable for removing polymeric debris from vias, according to the preferred embodiment.
[0032] The percentage of ammonia in the ammonia/oxygen mix used to generate the plasma is preferably greater than or equal to about 25%. More preferably, ammonia comprises about 50% to 100% of the ammonia/oxygen mix. In an exemplary implementation, the flow rates of NH 3 and N 2 were about equal, at about 2 L/min. Reactor pressure was maintained at approximately 1.5 Torr. Temperatures of the substrate are preferably maintained at about 100-400° C., and was maintained at about 270° C. in the exemplary implementation. In the Fusion reactors, microwave power was set to approximately 1,900 watts. In the inductively coupled plasma reactor from Matson, a power of approximately 975 watts was used. The skilled artisan can readily determine an appropriate power level to effect dissociation of the constituent gases and thus activate the plasma for a given reactor.
[0033] After the residue 26 is treated with the hydrogen-containing gas, the integrated circuit is preferably rinsed to remove the treated residue. For example, in an exemplary implementation, the substrate was dipped in a dilute phosphoric acid solution, such as an aqueous solution of at least about 5% phosphoric acid in water, giving a pH of approximately 1.8. Alternatively, the wafer may be dipped in hot deionized water or subjected to isopropyl alcohol vapor (i.e., a Margoni rinse) after the ammonia treatment.
[0034] As shown in FIG. 5, after the residue 26 has been removed from the via 24 by treatment and rinse, a second conductive layer 28 is deposited over the dielectric layer 18 and into the opening 24 , thus forming a contact 30 to the first conductive layer 12 . Suitable conductive materials for forming the second conductive layer 28 include aluminum, gold, copper, copper, silicon, and alloys of such metals.
[0035] In the illustrated embodiment, the conductive material deposited to form the contact also forms a metal wiring layer 32 above the contact, which can then be patterned into metal runners. The skilled artisan will readily recognize that the described method of cleaning vias is also applicable to damascene and dual damascene processes. Alternatively, the cleaned via 24 can be filled with a conductive material which is etched back to leave an. isolated conductive plug, typically formed of tungsten, metal silicides or polysilicon. The integrated circuit can then be completed by methods well known to those skilled in the art.
[0036] Advantageously, the preferred embodiments enable a fast, highly directional etch, while at the same time leaving a via free of impurities which might otherwise affect contact resistivity and reliability.
[0037] Various modifications and alterations of this invention will be apparent to those skilled in the art without departing from the scope and spirit of this invention. It should be understood that the invention is not limited to the embodiments disclosed therein, and the claims should be interpreted as broadly as the prior art allows. | Organic etch residues are often left within vias formed by etching through resist masks. Since the etch is designed to expose an underlying metal layer and is directional in order to produce vertical via sidewalls, the residue often incorporates metal. The present invention discloses a method of removing such etch residues while passivating exposed metal, including exposing the residue to ammonia. In the disclosed embodiment, ammonia and oxygen are mixed in a plasma step, such that the resist can be burned off at the same time as the residue treatment. The residue can thus be easily rinsed away. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from Japanese Patent Application No. 2007-224933 filed Aug. 30, 2007. The entire content of this priority application is incorporated herein by reference.
TECHNICAL FIELD
[0002] The present invention relates to a log collecting system and a computer apparatus.
BACKGROUND
[0003] In most cases, peripheral devices such as a printer, a scanner and a facsimile apparatus are connected to a personal computer (PC). While controlling the peripheral devices, the PC performs various processes. If any peripheral devices connected to the PC malfunction, the PC can no longer control these peripheral devices. In this case, the PC may not perform any process as desired by the user. The cause of the trouble in the peripheral devices cannot be identified in most cases, if the state in which the PC or the peripheral devices had been operating before the peripheral devices started malfunctioning is only checked.
[0004] In recent years, a log collecting system has been developed, which generates log items, i.e., record items about the operations a PC has performed, giving and receiving commands and data to and from a peripheral devices. The log collecting system stores the log items. If a trouble develops in the PC, the log collecting system sends the log items to the vendor provided in the peripheral devices. The vendor analyzes the log items to identify the cause of the trouble in the PC. However, the vendor cannot analyze the internal state the peripheral devices assume because only the log items the PC has generated are sent to the vendor. Therefore, the vendor can hardly identify the cause of the trouble.
[0005] Japanese unexamined patent application publication No. 2005-56018 describes a print-log management method, in which a PC receives the print information generated by a printer, every time the PC issues a print job to the printer, and merges the print information with a print log the PC has generated, thereby generating a print-management log item. The information about any printing the printer has performed can therefore be reliably managed.
SUMMARY
[0006] However, by using this print-log management method, the following problem can arise. That is, only the log items concerning a particular job called print job are collected. It the print-log management method is applied to the log collecting system described above, the peripheral devices cannot collect the information about anything other than the particular job. Therefore, all troubles that have taken place in the peripheral devices cannot be analyzed if the peripheral devices malfunction and cause a trouble in the process the PC performs. If the peripheral devices malfunction while executing a job other than the particular job, the cause of the trouble can hardly be identified, either.
[0007] The peripheral devices may generate log items concerning all jobs executed and may keep sending the log items to the PC at all times. If this is the case, the load of communication between the PC and the peripheral devices will inevitably increase.
[0008] In view of the above-identified problem, an object of the invention is to provide a log collecting system and a computer apparatus, which can collect log items, easily identifying the cause of a trouble in any process the computer apparatus performs, while suppressing the increase in the load of communication between the computer apparatus and the peripheral device.
[0009] In order to attain the above and other objects, the invention provides a log collecting system including a computer apparatus, and at least one peripheral apparatus connected to the computer apparatus, the computer apparatus collecting a log that records operation of the at least one peripheral apparatus. The peripheral apparatus includes a first log memory controlling section that stores a first log relating to all operation of the at least one peripheral apparatus in a first log memory region, and a second log memory controlling section that stores, in a second log memory region, a second log indicative of any influence on the operation of the at least one peripheral apparatus among the first logs. The computer apparatus includes a third log memory controlling section that stores, in a third log memory region, a third log relating to the operation of the computer apparatus concerning the at least one peripheral apparatus, a fourth log memory controlling section that continuously or discontinuously acquires the second logs stored in the second log memory region, and stores the second log in a fourth log memory region, a first log acquiring section that acquires, at a predetermined timing, the first log stored in the first log memory region, and a log information creating section that creates one log information with the acquired first log, the third log stored in the third log memory region, and the second log stored in the fourth log memory region when the first log acquiring section acquires the first log.
[0010] According to another aspect, the invention provides a computer apparatus connected to at least one of the peripheral apparatus and collecting the log of the operation of the peripheral apparatus including a first log memory region that stores a first log relating to a record of operation of the peripheral apparatus, and a second log memory region that stores, among the first log, a second log indicative of influence on the operation of the peripheral apparatus. The computer apparatus includes a third log memory controlling section, a fourth log memory controlling section, a first log acquiring section and a log information creating section. The a third log memory controlling section stores, in a third log memory region, a third log relating to the operation of the computer apparatus concerning the at least one peripheral apparatus. The fourth log memory controlling section continuously or discontinuously acquires the second logs stored in the second log memory region, and stores the second log in a fourth log memory region. The first log acquiring section acquires, at a predetermined timing, the first log stored in the first log memory region. The log information creating section creates one log information with the acquired first log, the third log stored in the third log memory region, and the second log stored in the fourth log memory region when the first log acquiring section acquires the first log.
[0011] According to another aspect, the invention provides a computer readable storage medium storing a set of image processing program instructions executable on a computer apparatus connected to at least one of the peripheral apparatus and Collecting the log of the operation of the peripheral apparatus including a first log memory region that stores a first log relating to a record of operation of the peripheral apparatus, and a second log memory region that stores, among the first log, a second log indicative of influence on the operation of the peripheral apparatus. The instructions include storing, in a third log memory region, a third log relating to the operation of the computer apparatus concerning the at least one peripheral apparatus, acquiring continuously or discontinuously the second logs stored in the second log memory region, and stores the second log in a fourth log memory region, acquiring, at a predetermined timing, the first log stored in the first log memory region, and creating one log information with the acquired first log, the third log stored in the third log memory region, and the second log stored in the fourth log memory region when the first log acquiring section acquires the first log.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is a schematic block diagram showing the electrical configuration of a log collecting system according to an embodiment of the present invention;
[0013] FIG. 2( a ) is a schematic illustration of the contents of a detail log stored in the detail log area of the log collecting system;
[0014] FIG. 2( b ) is a schematic illustration of the contents of an easy log stored in the easy log area of the log collecting system;
[0015] FIG. 2( c ) is a schematic diagram showing the configuration of the log folder of the log collecting system;
[0016] FIG. 2( d ) is a sequence chart showing the sequence of operation the log collecting system performs in the normal operating mode;
[0017] FIG. 2( e ) is a sequence chart showing the sequence of operation the log collecting system performs in the log-collecting mode;
[0018] FIG. 3 is a flowchart showing the log preparing process performed in a printer;
[0019] FIG. 4 is a flowchart showing the easy-log transmitting process performed in the printer;
[0020] FIG. 5 is a flowchart showing the device monitoring process performed by a PC;
[0021] FIG. 6 is a flowchart showing the easy-log acquiring process performed in the PC;
[0022] FIG. 7 is a flowchart showing the easy-log time correcting process performed in the PC;
[0023] FIG. 8 is a flowchart showing the log collecting process performed in the PC;
[0024] FIG. 9( a ) is a flowchart showing the detail-log acquiring process performed in the PC; and
[0025] FIG. 9( b ) is a flowchart showing the detail-log time correcting process performed in the PC.
DETAILED DESCRIPTION
[0026] Next, an embodiment of the present invention will be described while referring to the accompanying drawings. FIG. 1 is a schematic block diagram of a log collecting system according to the embodiment of the present invention, showing the electric configuration thereof.
[0027] As shown in FIG. 1 , the log collecting system 1 has an ink-jet printer 10 a (hereinafter called “printer 10 a ”), a scanner 10 b , a facsimile 10 c , and a personal computer 11 (hereinafter called “PC 11 ”). The printer 10 a , scanner 10 b and facsimile 10 c are connected to the PC 11 by communications cables 40 a , 40 b and 40 c , respectively. The log collecting system 1 is a system that can easily identify the cause of a trouble in any process the PC 11 performs, while suppressing the increase in the load of communication between the PC 11 , one the one hand, and the printer 10 a , scanner 10 b and facsimile 10 c , on the other hand.
[0028] The printer 10 a is an ink-jet printer that has an ink-let head 3 . In accordance with an instruction output from the PC 11 , the printer 10 e ejects ink droplets toward a recording medium through the nozzles made in the ink-jet head 3 for printing. The printer 10 a includes a CPU (Central Processing Unit) 20 , a ROM (Read Only Memory) 21 , a RAM (Random Access Memory) 22 , an EEPROM (Electrical Erasable and Programmable Read Only Memory) 23 , a Gate Array (G/A) 24 , and a Driver for Head 25 . Each of the CPU 20 , the ROM 21 , the RAM 22 , the EEPROM 23 , and the Gate Array 24 are connected via a bus line 26 . The Driver for Head 25 is connected to the Gate Array 24 .
[0029] The CPU 20 is a processing unit that controls the printer 10 a in accordance with a control program stored in the ROM 21 . The CPU 20 generates, for example, an ink-injection timing signal and a reset signal. The ink-injection timing signal and the reset signal are transferred to the gate array 24 , which will be described later.
[0030] An operation panel 27 , a transport-motor drive circuit 29 , a paper sensor 30 are connected to the CPU 20 . A user may operate the operation panel 27 to input instructions. The transport-motor drive circuit 29 can drive a transport motor (LF motor) 28 . When driven, the transport motor 28 feeds a recording medium. The paper sensor 30 can detect the leading edge of a recording medium. The CPU 20 controls the operation panel 27 , drive circuit 29 and paper sensor 30 .
[0031] A timekeeping circuit 31 is also connected to the CPU 20 . The timekeeping circuit 31 incorporates a timekeeping that measures time. The timekeeping circuit 31 is the known type circuit that compares the present time with the time when time-measuring was started and calculates the period that as elapsed from the start of the time measuring. Then, the timekeeping circuit 31 inform the CPU 20 of the present time and the period thus calculated.
[0032] The ROM 21 is a nonvolatile memory in which data cannot be rewritten. The ROM 21 stores various control programs, such as log-creating program 21 a and easy-log transmitting program 21 b that the CPU 20 may execute. The ROM 21 further stores fixed data items.
[0033] The log-creating program 21 a is a program that the CPU 20 executes to generate log items about the operation of the printer 10 a and to store these log items in a detail log area 23 a , which will be described later. By executing the program 21 a , the CPU 20 store those of the log items, which influence the operation of the printer 10 a , as easy log items, in an easy log area 22 a , which will be described later.
[0034] The log items concerning the operation of the printer 10 a are recorded information items about, for example, the control signals that the printer 10 a has received from the PC 11 , the information about the data that the printer 10 has transmitted and received to and from the PC 11 , the information about the control signals that the CPU 20 has output to respective parts of the printer 10 a , the operation results (e.g., success or failure), and the information about troubles in the printer 10 a . The CPU 20 activates and executes the log-creating program 21 a when any trouble that should be logged takes place.
[0035] A detail log 61 which are stored into the detail log area 23 a and an easy log 62 which are stored into the easy log area 22 a by the log-creating program 21 a will be explained with reference to FIGS. 2( a ) and 2 ( b ). FIG. 2( a ) is a schematic diagram illustrating the contents of the detail log 61 stored in the detail log area 23 a.
[0036] As FIG. 2( a ) shows, the detail log 61 has time 61 a , identification number 61 b , type 61 c and content 61 d pertaining to each log item. The time 61 a is the data acquired from the timekeeping circuit 31 when the log-creating program 21 a generated the log item. The identification number 61 b is the serial number of the log item and is incremented by one every time a log item is generated. The PC 11 or any person may use the identification number 61 b in order to associate the detail log 61 with the easy log 62 stored in the easy log area 22 a.
[0037] The type 61 c represents the type of the content of the log item, “INF,” “WRN” or “ERR.” Any log item of “TNF” type is an information log item showing an ordinary operation. Any log item of “WRN” type is a warning log item showing an operation that may induce a trouble in the future Any log item of “ERR” type is an error log item showing an operation that may result in a great consequence. The content 61 d is a character string that represents the specific content of the log item.
[0038] The detail log 61 consists of all log items about the operation of the printer 10 a , as described above. More precisely, the detail log 61 is composed of an information log item, a warning log item and an error log item. If the detail log 61 is used, any unusual event occurring in the printer 10 a can be easily identified.
[0039] FIG. 2( b ) is a diagram schematically illustrating the contents of the easy log 62 stored in the easy log area 22 a . As shown in FIG. 2( b ), the easy log 62 is composed of only two of the items that constitute the detail log 61 , i.e., the warning log item and error log item indicating that the log may adversely influence the operation of the printer 10 a . If the easy log 62 is used, any trouble in the printer 10 a can be tracked down to some extent, in accordance with the warning log item and the error log item. Further, a volume of data of the easy log 62 is smaller than a volume of data of the detail log 61 and is therefore advantageous over the detail log 61 .
[0040] Referring back to FIG. 1 , the log collecting system 1 will be described further. The easy-log transmitting program 21 b sends to the PC 11 the easy log 62 stored in the easy log area 22 a . The CPU 20 activates and executes the easy-log transmitting program 21 b when the printer 10 a receives an easy-log requesting command from the PC 11 . Executing this program, the CPU 20 acquires the present-time data from the timekeeping circuit 31 when the easy log 62 is transmitted and transmits the present-time data and the easy log 62 . If the easy log 62 is not stored in the easy log area 22 a , the CPU 20 transmits null data, in place of the present-time data the easy log 62 .
[0041] The RAM 22 is a volatile memory in which data can be rewritten, various data items can be temporarily stored in the RAM 22 . The RAM 22 has the easy log area 22 a . The easy log area 22 a is provided to store the easy log 62 generated by the log-creating program 21 a . The easy log area 22 a cannot be directly accessed from the PC 11 . Nonetheless, the PC 11 can acquire the easy log 62 stored in the easy log area 22 a , by issuing an easy-log requesting command.
[0042] The EEPROM 23 is a nonvolatile memory in which data cannot be rewritten. The EEPROM 23 functions as a device having a removable storage area that the PC 11 can directly access. The EEPROM 23 has a detail log area 23 a and an identification number counter 23 b . The detail log area 23 a is an area in which the detail log 61 generated by the log-creating program 21 a is stored. In the detail log area 23 a , the items of the detail log 61 are stored in the order they have been generated by the log-creating program 21 a , that is, in the ascending order of the identification numbers 61 b . The detail log area 23 a is a removable storage area. The PC 11 can directly access the detail log 61 stored in the detail log area 23 a and can therefore copy the contents of the detail log 61 . Because the detail log area 23 a is provided in the EEPROM 23 , the detail log remains held in the detail log area 23 a even if the user turns off the power switch of the printer 10 a when an error takes place. Therefore, when the user turns on the printer 10 a again, the PC 11 can acquire the detail log stored in the detail log area 23 a.
[0043] The identification number counter 23 h is a counter that is used to generate the identification numbers 61 b shown in FIG. 2( a ). The identification number counter 23 b is referred to, in order to make the log-creating program 21 a generate the log. The count is incremented by one every time the log-creating program 21 a refers to the count. Note that the counter 23 b is set to “0” when the printer 10 a is shipped from the factory.
[0044] The gate array 24 is connected to an image memory 32 configured to store image data that should be printed on a recording medium. In accordance with a print timing signal transferred from the CPU 20 , the gate array 24 outputs print data (drive signal), a transfer clock, a latch signal, a parameter signal, and an ejection-timing signal. The print data is used to print the image data on a recording medium. The transfer clock is synchronous with the print data. The parameter signal is used to generate a basic print-waveform signal. The ejection-timing signal is output at prescribed intervals. These signals are output to the head driver 25 .
[0045] The gate array 24 is connected to an interface 33 that may be connected to the PC 11 by a communication line 40 a . The gate array 24 can receive image data transferred from the PC 11 via the interface 33 . The image data thus received is stored in the image memory 32 .
[0046] The head driver 25 is a drive circuit that supplies drive pulses to the drive elements associated with the nozzles made in the ink-jet head 3 , in response to a signal output from the gate array 24 . The drive pulses drive the drive elements, which eject ink through the respective nozzles.
[0047] The scanner 10 b is a peripheral device having a document table (not shown). The scanner 10 b reads an image from the document set on the document table and generates image data representing the image. The image data is transmitted to the PC 11 . The facsimile 10 c is a peripheral device that can receive image data from the PC 11 and transmit the image data to another facsimile via the telephone line (not shown), and can receive image data from another facsimile and transmit the image data to the PC 11 . The components that perform the major functions of the scanner 10 b and facsimile 10 c have the configurations known in the art. The components of the scanner 10 b and facsimile 11 c , which generate and store a detail log 61 and an easy log 62 and transmit the easy log to the PC 11 , are identical to the configuration of the printer 10 a . Therefore, the electrical configurations of the scanner 10 b and facsimile 10 c will not be shown or described.
[0048] The PC 11 is a computer that cooperates with the peripheral devices, i.e., the printer 10 a , scanner 10 b and facsimile 10 c , to perform the processes the user wants them to do. The PC 11 includes a CPU 41 , a ROM 42 , a CAM 43 , a hard disk drive (hereinafter abbreviated to “HDD”) 44 , a liquid crystal display 46 (hereinafter abbreviated to “LCD”), a Keyboard 47 and an Interface 48 . Each of the HDD 44 , the liquid crystal display 46 , the Keyboard 47 , and the Interface 48 are connected via an Input/output (hereinafter abbreviated to “I/O”) port 49 . Each of the CPU 41 , the ROM 42 , the RAM 43 , and the I/O port 49 are connected via a Bus line 50 .
[0049] The CPU 41 is a processing unit that controls the pc 11 in accordance with a control program stored in the ROM 42 and the HDD 44 . A timekeeping circuit 45 is connected to the CPU 41 . The timekeeping circuit 45 is the known type circuit that functions similarly to the timekeeping circuit 31 .
[0050] The ROM 42 is a nonvolatile memory in which data cannot be rewritten. The ROM 42 stores various control programs, such as controlling program that executed by the CPU 41 and fixed values, and so forth. The RAM 43 is a volatile memory in which data can be rewritten. Various data such as an acquisition flag 43 a can be temporarily stored in the RAM 43 .
[0051] The acquisition flag 43 a may be set to “1” to indicate that a device monitoring program 44 a is acquiring easy logs from the printer 10 a , scanner 10 b and facsimile 10 c . (Hereinafter, the process of acquiring the easy logs will be called “easy-log acquiring process”.) when the device monitoring program 44 a starts the easy-log acquiring process, the acquisition flag 43 a is set to “1”. When the easy-log acquiring process is completed, the acquisition flag 43 a is set to “0.” Note that the acquisition flag 43 a is set to “0” as initial value when the power switch of the PC 11 is turned on.
[0052] The acquisition flag 43 a is referred to in the process performed by a log collecting program 44 b , which will be described later. The acquisition flag 43 a is used to prevent the device monitoring program 44 a and the log collecting program 44 b from performing one easy-log acquiring process and another easy-log acquiring process, respectively.
[0053] The HDD 44 is a nonvolatile memory in which data can be rewritten. The HDD 44 stores a device monitoring program 44 a , a log collecting program 44 b and an application program 44 c . These programs are executed by the CPU 41 . The HDD 44 also stores registry 44 d and a log folder 44 e.
[0054] The device monitoring program 44 a is a program that performs an easy-log acquiring process, i.e., a process of acquiring easy logs at regular intervals from all peripheral devices (i.e., the printer 10 a , scanner 10 b and facsimile 10 c ) that are connected to the PC 11 . As described above, the device monitoring program 44 a sets the value of the acquisition flag 43 a , either “1” or “0”, at the start or end of the easy-log acquiring process. The device monitoring program 44 a is activated when the power switch of the PC 11 is turned on. The CPU 41 keeps executing the device monitoring program 44 a until the power switch is turned off or the user inputs program-terminating instructions.
[0055] In the easy-log acquiring process, an easy log requesting command is transmitted to all peripheral devices, in order to acquire easy logs from the peripheral devices, respectively. At this point, the CPU 41 corrects the time described in each easy log, based on the time interval between the present time at the peripheral device, which has been transmitted along with the easy log, and the present time at the PC 11 , which has been acquired from the timekeeping circuit 45 . The time described in the easy log is thus adjusted to the time axis applied in the PC 11 . The easy logs of the peripheral device, thus corrected, are held in the sub-folders associated with the respective peripheral devices and provided in the log folder 44 e . The log folder 44 e will be described later.
[0056] The log collecting program 44 b is a program that compiles the PC log generated by the PC 11 and stored in the log folder 44 e (described later), the easy logs and detail logs generated by the peripheral devices, and the necessary ones of the registries stored in the registry 44 d (later described). Compiling these logs, the log collecting program 44 b generates a collected log file. The log collecting program 44 b is activated and executed in response to the instructions by the user and is executed prior to the generation of the collected log file, acquiring the easy logs and the detail logs. The latest easy log and the latest detail log can be thereby acquired from each peripheral device.
[0057] If the acquisition flag 43 a is “1”, the easy-log acquiring process is being performed by the device monitoring program 44 a . Therefore, the log collecting program 44 b does not perform an easy-log acquiring process and remains in the standby state until the device monitoring program 44 a finishes the easy-log acquiring process. This prevents the easy-log acquiring process from being performed by both the device monitoring program 44 a and the log collecting program 44 b.
[0058] In the detail-log acquiring process, detail logs of all peripheral devices are copied, and the time data items described in the respective detail logs are corrected. (Hereinafter, the process of correcting the time data items will be called “detail-log time correcting process.”) The digital log of each peripheral device, which has been subjected to the detail-log time correcting process, is held in the sub-folder provided in the log folder 44 e and associated with the device.
[0059] In the detail-log time correcting process, an easy log may be acquired from any peripheral device whose detail log has been copied. If this is the case, the time described in the detail log of the same identification number as the identification number described in the easy log is replaced by the time described in the easy log having the same identification number. Thus, the time described in the warning log item and error log item, both contained in the easy log, as well as in the detail log, can be adjusted to the time axis applied in the PC 11 . Because the detail log describes identification numbers, each incremented by one with respect to the immediately preceding one, the time the information log was generated with respect to the time axis applied in the PC 11 can be inferred from the time that has been replaced for the warning log item and error log item.
[0060] In the detail-log time correcting process, the easy log may not be acquired from any peripheral device whose detail log has been copied. In this case, a marker is added to the detail log, showing all time data items described in the detail log are used in the peripheral device. By using this marker, anyone who refers to the log can recognize that the time data items described in the detail log are those used in the peripheral device.
[0061] The application program 44 c is a program that the CPU 41 may execute to perform a specific process. When a control signal or data is supplied and received to and from each peripheral device, by using the application program 44 c , the application program 44 c (more precisely, the CPU 11 ) generates a log. The log (PC log) generated by the application program 44 c contains the information about the control signals and data transmitted and received to and from the peripheral device, the information about the results of operation in the peripheral device and the information about operation errors (The information about the results of operation represents, for example, the success or failure of the operation.) Each of the PC log describes the time data acquired from the timekeeping circuit 45 when the log was generated by using the application program 44 c , the logotype data identifying the type of the log (information log, warning log, or error log) and a character train representing the contents of the log. The application program 44 c adds the PC log to the PC log file provided for the peripheral device and held in the log folder 44 e.
[0062] The registry 44 d is a database that stores the setting data about the operation system (OS) of the PC 11 and the application program 44 c . The registry 44 d describes the names, vendor names, port numbers, IP addresses and node names of the peripheral devices connected to the PC 11 . From the information described in the registry 44 d , the device monitoring program 44 a and the log collecting program 44 b can acquire the information about any peripheral device, from which a easy log or a detail log should be acquired.
[0063] The log folder 44 e stores the PC logs generated by the application program 44 c and the easy and detail logs acquired from the peripheral devices by the device monitoring program 44 a and log collecting program 44 b . The configuration of the log folder 44 e will be described with reference to FIG. 2( c ). FIG. 2( c ) is a schematic diagram showing the configuration of the log folder “log” (hereinafter called “log” folder).
[0064] As shown in FIG. 2( c ), the “log” folder includes a PC log folder “PC log” (hereinafter called “PC log” folder) and a device log folder “Device log” folder (hereinafter called “Device log” folder). The “PC log” folder holds a PC log. The “Device log” folder holds the easy and detail logs each peripheral device has generated. Further, the “Device log” folder includes sub-holders provided for the respective peripheral devices. The sub-holders have names identical to the peripheral devices (or trade numbers) associated to them. That is, the sub-folder associated with the printer 10 a is named “Printer” is called “Printer” folder, the sub-folder associated with the scanner 10 b that is named “Scanner” is called “Scanner” folder, and the sub-folder associated with the facsimile 10 c that is named “Fax” is called “Fax” folder.
[0065] The “PC log” folder stores the PC log files prepared for each of the peripheral devices. More specifically, the “PC log” folder stores a “Printer. log” file, a “Scanner. log” file and a “Fax. log” file. The “Printer. log” file stores the PC log generated in the process the application program 44 c has performed on the printer 10 a . The “Scanner. log” file stores the PC log generated in the process the application program 44 c has performed on the scanner 10 b . The “Fax. log” file stores the PC log generated in the process the application program 44 c has performed on the facsimile 10 c . Further, in the “Pinter” folder, the “Scanner” folder and the “Fax” folder, an easy log file “easy.log” and a detail log file “Detail.log” are stored. The easy log file “easy.log” holds the easy log acquired from the associated peripheral device. The detail log file “Detail.log” holds the detail log acquired from the associated peripheral device.
[0066] The “log” folders are compressed and encrypted into a collected log file by the log collecting program 44 b , each preserving the folder configuration, together with the necessary registry information.
[0067] Next, the sequences that the log collecting system 1 operates in the normal operating mode and in the log-collecting mode will be described with reference to FIGS. 2( d )- 2 ( e ). FIG. 2( d ) is a sequence chart showing the sequence of operation the log collecting system 1 performs in normal operating mode. FIG. 2( e ) is a sequence chart showing the sequence of operation the log collecting system 1 performs in the log-collecting mode. In the normal operating mode, after the power source of the PC 11 and the printer 10 a is turned on, the system 1 performs ordinary processes. In the log-collecting mode, the PC 11 is started and executes the log collecting program 44 b . In FIGS. 2( d ) and 2 ( e ), only one peripheral device, i.e., printer 10 a is illustrated. Because similar processes are performed in the scanner 10 b and facsimile 10 c , display and explanation of the scanner 10 b and facsimile 10 c have been omitted.
[0068] In the normal operating mode, as shown in FIG. 2( d ), the PC 11 executes the process of the application program 44 c , transmitting and receiving control signals and data to and from the peripheral devices, and generates a PC log. The PC log is added to the PC log files prepared for the peripheral devices, respectively (1). Meanwhile, in the printer 10 a , the log-creating program 21 a generates a log about the operation of the printer 10 a . The entire log generated is stored, as detail log, in the detail log area 23 a (2). Moreover, the warning log and error log included in the detail log are stored, as easy log, in the easy log area 22 a (3).
[0069] The device monitoring program 44 a in the PC 11 transmits an easy-log requesting command to the printer 10 a (4). On receiving the easy-log requesting command from the PC 11 , the easy-log transmitting program 21 b reads an easy log from the easy log area 22 a (5). The program 21 b then acquires the present-time data of the printer 10 a from the timekeeping circuit 31 (6). Further, the program 21 b transmits the easy log, together with the present-time data, to the PC 11 (7).
[0070] On receiving the easy log and the present-time data, the device monitoring program 44 a in the PC 11 adjusts the time described in the easy log to the time axis applied in the PC 11 . Then, the device monitoring program 44 a stores the easy log describing the time corrected, in the sub-folder included in the log folder 44 e that is provided for the peripheral device ( 8 ).
[0071] Thus, in the normal operating mode, the log generated by the application program 44 c and the easy log generated in the printer 10 a are stored in the log folder 44 e.
[0072] In the log-collecting mode, as shown in FIG. 2( e ), the log collecting program 44 b determines the value of the acquisition flag 43 a (11). If the acquisition flag 43 a is “1”, the device monitoring program is performing the easy-log acquiring process. In this case, the log collecting program 44 b does not perform the easy-log acquiring process and remains in the standby state until the device monitoring program 44 a finishes the easy-log acquiring process. When the easy-log acquiring process is completed, the process ( 17 ) is performed.
[0073] If the acquisition flag 43 a is “0,” the log collecting program 44 b transmits an easy-log requesting command to the printer 10 a (12). On receiving the easy-log requesting command, the easy-log transmitting program 21 b in PC 11 performs processes similar to those (5) to (8) performed in the normal operating mode shown in FIG. 2( d ), in the steps (13) to (16), respectively. In this case, the latest easy log describing the time corrected is stored in the sub-folder included in the log folder 44 e that is provided for the peripheral device.
[0074] Next, the log collecting program 44 b copies the detail log from the detail log area 23 a in the printer 10 a (17). The log collecting program 44 b further corrects the time, which is described in the warning log and error log included in the detail log, to the time axis applied in the PC and stores the warning log and error log in the log folder 44 e (18). The log generated in the PC 11 and the easy and detail logs generated in the printer 13 a are stored in the log folder 44 e . Then, the log collecting program 44 b compresses and encrypts the contents of the log folder 44 e , generating one collected-log file. The collected-log file is output, with the folder configuration of the contents preserved (20). Therefore, the user or the vendor can easily identify the cause of a trouble in any process the PC 11 performs by analyzing this collected-log file.
[0075] Next, a log preparing process executed by the CPU 20 of the printer 10 a will be described with reference to FIG. 3 . FIG. 3 is a flowchart explaining the log preparing process performed in the printer 10 a . The CPU 20 performs this process by activating the log-creating program 21 a , when an event that should be logged takes place in the printer 10 a.
[0076] In this process, the CPU 20 acquires an identification number from the identification number counter 23 b (S 101 ). Then, the CPU 20 generates a log character string from the nature of the event that has taken place in the printer 10 a (S 102 ). As shown in FIG. 2( a ), the log character string represents an identification number 61 b , type 61 c and content 61 d . Further, the CPU 20 acquires the present-time data is acquired from the timekeeping circuit 31 , and adds the time data 61 a to the head of the log character string generated in S 102 (S 103 ). Then, the CPU 20 adds the log character string obtained in S 103 , as detail log 61 , and stores this log character string in the detail log area 23 a (S 104 ). The data about the event that has occurred in the printer 10 a is thereby stored in detail log area 23 a.
[0077] Then the CPU 20 increments the count of the identification number counter 23 b by “1” (S 105 ). The identification number 61 b described in the detail log 61 generated to prepare is therefore incremented by “1”. Hence, the detail log can be identified by referring to the identification number 61 b.
[0078] Next, the CPU 20 determines whether the type 61 c of the log character string acquired in S 103 is a warning log “WRN” or an error log “ERR” (S 106 ). If the type 61 c is neither a warning log “WRN” nor an error log “ERR” (No in S 106 ), the process is terminated. If the type 61 c is a warning log “WPN” or an error log “ERR” (Yes in S 106 ), the CPU 20 advances to S 107 .
[0079] The process from S 107 to S 110 is a process of storing the log character string acquired in S 103 in the easy log area 22 a . First, in S 107 , the CPU 20 acquires the vacant part of the easy log area 22 a . In S 108 , the CPU 20 determines whether the volume of the vacant part is large enough to store the log character string. If the volume of the vacant part is not large enough to store the log character string is determined (No in S 108 ), the CPU 20 deletes the easy log G 2 , which has been stored longer in the easy log area 22 a than any other data items (S 109 ). The CPU 20 repeats the process of S 107 through S 109 while the volume of the vacant part of the easy log area 22 a is smaller than the volume of the log character string. A storage area can thereby be provided in the easy log area 22 a , for the log character string acquired in S 103 .
[0080] When the CPU 20 determines the volume of the vacant part is found to be large enough to store the log character string (Yes in S 108 ), in S 110 the CPU 20 adds the log character string acquired in S 103 and stores this log character string as easy log 62 in the easy log area 22 a . Then, the CPU 20 ends the process. Thus, the log is stored as easy log 62 in the easy log area 22 a if the problem that has occurred in the printer 10 a may be serious in the future or may result in a grave consequence. More precisely, if the type 61 c included in the detail log 61 is a warning log “WRN” or an error log “ERR”, the type 61 c will be stored as easy log 62 . In this process, the same log character string acquired in S 103 is stored in the detail log 61 and the easy log 62 , therefore, the identification numbers given at the same incidence are the same in the detail log 61 and the easy log 62 By using this identification number, checking the detail log 61 and the easy log 62 can be easily executed.
[0081] Next, an easy-log transmitting process executed by the CPU 20 of the printer 10 a will be described with reference to FIG. 4 . FIG. 4 is a flowchart showing the easy-log transmitting process. This process is performed when the CPU 20 starts the easy-log transmitting program 21 b when the printer 10 a receives an easy-log requesting command transmitted from the PC 11 .
[0082] In the easy-log transmitting process, the CPU 20 determines whether an easy log exists in the easy log area 22 a (S 150 ). If an easy log exists in the easy log area 22 a (Yes in S 150 ), the CPU 20 acquires the present-time data from the timekeeping circuit 31 (S 151 ). Next, the CPU 20 transmits the present-time data acquired in S 151 and the easy log stored in the easy log area 22 a to the PC 11 (S 152 ) and ends this process. Because the present-time data and the easy log are transmitted to the PC 11 , the PC 11 can perform the easy-log acquiring process, adjusting the time described in the easy log to the time axis applied in the PC 11 .
[0083] If no easy logs are found to exist in the easy log area 22 a (if No in 5150 ), the CPU 20 transmits null data “Null” (hereinafter referred to as “Null” data) to the PC 11 (S 153 ) and ends this process. As a result, the PC 11 can determine that no easy logs exist in the printer 10 a.
[0084] Next, the device monitoring process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 5 . FIG. 5 is a flowchart showing the device monitoring process. This process is initiated when the CPU 41 starts the device monitoring program 44 a as the PC 11 is turned on.
[0085] In this process, the CPU 41 extracts the device name of a peripheral device the PC 11 should monitor, based on the device names or vendor names of the peripheral devices, which are described in the registry 44 d (S 201 ). The CPU 41 then acquires the easy log or detail log of any peripheral device that should be monitored. Further, the CPU 41 acquires data items about the peripheral device to monitor, such as the device name, port number, IP address and node name, from the registry 44 d . The easy log or detail log and the data items, all pertaining to the peripheral device to monitor, are stored in the RAM 42 . At this point, serial numbers, starting with “0”, are assigned to the peripheral devices to monitor. Thereafter, the easy-log acquiring process and the detail-log acquiring process will be performed on the peripheral devices, one after another, in accordance with the serial numbers assigned to the peripheral devices.
[0086] Subsequently, the CPU 41 counts the number of the extracted peripheral devices and stores this number in the RAM 42 (S 202 ). The count N stored will be used in the process of acquiring the easy logs or detail logs from all peripheral devices that are monitored.
[0087] Next, by using the timekeeping circuit 45 , the CPU 41 starts measuring time (S 203 ). Then the CPU 41 determines whether the time measured by the timekeeping circuit 45 has reached a prescribed time or not (S 204 ). If the time measured has not reached the prescribed value (No in S 204 ), the CPU 41 repeats the process of S 204 until the time measured reaches the prescribed value. If the time measured has reached the prescribed value (Yes in S 204 ), the CPU 41 advances to S 205 . As a result, before S 205 , the CPU 41 can creates prescribed time counted by the timekeeping circuit 45 . Thus, the CPU 41 can execute the easy-log acquiring process at regular intervals.
[0088] In S 205 , the CPU 41 set the acquisition flag 43 a to “1”. Then, the CPU 41 executes the easy-log acquiring process described later acquiring the easy log from each peripheral device (S 206 ). When the easy-log acquiring process (S 206 ) is completed, the CPU 41 sets the acquisition flag 43 a to “0” (S 207 ). As a result, the acquisition flag 43 a therefore indicates that the easy-log acquiring process proceeds during the device is being monitored. Thus, the acquisition flag 43 a prevents the log collecting program 44 b form performing another easy-log acquiring process.
[0089] The CPU 41 determines whether the PC 11 has been turned off, or the instruction to end the device monitoring program 44 a is input by the user (S 208 ). It the user has instructed to end the device monitoring program 44 a (Yes in S 208 ), the CPU 41 ends this process. If the user has not instructed to end the device monitoring program 44 a (No in S 208 ), the CPU 41 returns to S 203 and repeats the process of S 203 through S 208 until the CPU 41 detects the instruction to end the process. As a result, the easy-log acquiring process can therefore be performed at regular intervals, whereby the easy logs are acquired from the respective peripheral devices.
[0090] Next, the easy-log acquiring process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 6 . FIG. 6 is a flowchart showing the easy-log acquiring process. This is a process of acquiring an easy log from any peripheral device to monitor and is executed by the CPU 41 during the device monitoring process that has been described above or during the log collecting process that will be described later.
[0091] In this process, the CPU 41 sets a counter M is set in the RAM 43 at first and sets count of the counter M to “0” (S 301 ). The counter M is a counter for counting loops of the process of acquiring easy logs from all peripheral devices that are monitored during the easy-log acquiring process.
[0092] Subsequently, the CPU 41 determines whether the count of the counter M is smaller than the number N of peripheral devices, which is held in the RAM 43 during the device monitoring process (S 302 ). S 302 is a process of determining whether the process loop of acquiring easy logs from the peripheral devices has been completed. If the count of the counter M is equal to or larger than the number N (No in S 302 ), the CPU 41 determines the process of acquiring easy logs from the peripheral devices has been completed, and ends this process.
[0093] If the count of the counter M is smaller than the number N (Yes in S 302 ), the CPU 41 advances to S 303 . S 303 to S 315 are equivalent to the process of acquiring easy logs from the respective peripheral devices. First, in S 303 , of the information concerning the peripheral devices and held in the RAM 43 during the device monitoring process, the CPU 41 reads out the data about the peripheral device of the serial number identical to the count of the counter M, and transmits an easy-log requesting command to this peripheral device. Next, by using the timekeeping circuit 45 , the CPU 41 starts time-out counting (S 304 ). The time-out counting is initiated in order to determine whether each peripheral device gives a returned value within a prescribed time, in response to the easy-log requesting command transmitted in S 303 .
[0094] Next, the CPU 41 determines whether the peripheral device has given a returned value in response to the easy-log requesting command in S 305 . If the peripheral device has given no returned values (No in S 305 ), the CPU 41 determines whether the time-out counting has ended (S 306 ). If the time-out counting has not ended (No in S 306 ), the CPU 41 returns to S 305 , and determines whether the peripheral device has given a returned value again. If the time-out counting has ended (in S 306 ), the CPU 41 determines the peripheral device is unable to transmit the returned value. In this case, the CPU 41 advances to S 315 , so that an easy log may be acquired from another peripheral device. Note that any peripheral device cannot transmit the returned value when the peripheral device has been turned off or when a trouble has developed in the communications path between the PC 11 and the peripheral device.
[0095] If the peripheral device is found to have given the returned value in response to the easy-log requesting command (Yes in S 305 ), the CPU 41 ends the time-out counting (S 307 ). Then, the CPU 41 determines whether the returned value is “Null” data and if the returned value is “Null” data (Yes in S 308 ), the CPU 41 determines the peripheral device has no easy logs. In this case, the CPU 41 advances to S 315 in order to acquire an easy log from another peripheral device. If the returned value may not be “Null” data (No in S 308 ), the CPU 41 determines the returned value contains the present-time data and an easy log. Then, the CPU 41 extracts an easy-log time correcting process described later (S 309 ), and adjusts the time described in the easy log to the time axis applied in the PC 11 , based on the present-time data set in the peripheral device and the present-time data set in the PC 11 .
[0096] Subsequently, the CPU 41 determines whether “Device log” folder in the log folder 44 e includes a sub-folder whose name is identical to the name of a peripheral device that has acquired an easy log (S 310 ). The easy log, for which the time has been corrected, is stored in the subs folder whose name is identical to the name of the peripheral device. If “Device log” folder includes a sub-folder whose name is identical to the name of the peripheral device (Yes in S 310 ), the CPU 41 advances to S 312 . If “Device log” folder does not include such a sub-folder (No in S 310 ), the CPU 41 creates a sub-folder whose name is identical to that of the peripheral device is formed in the “Device log” folder (S 311 ) and then advances to S 312 .
[0097] In S 312 , the CPU 41 determines whether an “easy. log” file, which is an easy log file, exists in the sub-folder whose name is identical to the name of the peripheral device. If an “easy. log” file exists in the sub-folder (Yes in S 312 ), the CPU 41 merges the content of the easy log with the “easy. log” file (S 313 ). At this point, the identification number of the easy log which is stored in the “easy.log” file is compared with the identification number of the easy log included in the returned value acquired in S 305 . If an easy log having the same identification number exists, this easy log is regarded as one once acquired in the past and is not merged with the “easy. log” file. As a result, this can prevent identical easy logs, if any, from being described together in the “easy.log” file. When S 313 is completed, the CPU 41 advances to S 315 .
[0098] If an “easy.log” file is not found to exist, in S 312 (No in S 312 ), the CPU 41 creates an “easy. log” file in the sub-file whose name is identical to that of the peripheral device which has acquired the easy log, and copies the content of the easy log corrected in terms of time in the “easy.log” file (S 314 ). Then, the CPU 41 advances to S 315 .
[0099] In S 315 , the CPU 41 increments the count of the counter M by “1” and returns to S 302 . As a result, the CPU 41 can execute the process of acquiring an easy log from any other peripheral device.
[0100] Next, the easy-log time correcting process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 7 . FIG. 7 is a flowchart showing the easy-log time correcting process. This process is performed by the CPU 41 during the easy-log acquiring process described above, when the time data described in the easy log is adjusted to the time axis applied in the PC 11 .
[0101] In this process, the CPU 41 acquires the present-time data from the timekeeping circuit 45 (S 401 ). Next, the CPU 41 acquires the present-time at the peripheral device from the returned value acquired for the peripheral device during the easy-log acquiring process (S 402 ). The CPU 41 calculates the time interval between the present time at the PC 11 and the present time at the peripheral device (S 403 ). The CPU 41 adds the time interval thus calculated to the time data described in the easy log, thus correcting the time data, and overwrites the time data thus corrected in the easy log (S 404 ). Then, the CPU 41 ends this process. As a results, this can adjust the time data described in the easy log to the time axis applied in the PC 11 . The order can therefore be reliably recognized, in which the easy log and the log described in the PC log file generated by the application program 44 c in the PC 11 are generated. The load of analyzing the cause of any trouble can therefore be reduced.
[0102] Next, the log collecting process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 8 . FIG. 8 is a flowchart showing the log collecting process. This process is performed when the CPU 41 starts the log collecting program 44 b in response to the instructions the user has input.
[0103] In this log collecting process, first, the CPU 41 executes the process of acquiring the easy log from any peripheral device that should be monitored. In S 501 , the CPU 41 determines whether the acquisition flag 43 a is “1” (S 501 ). If the acquisition flag 43 a is “1” (Yes in S 501 ), the CPU 41 advances to S 502 because the easy-log acquiring process has been performed as determined in the device monitoring process. In S 502 , the CPU 41 determines whether the acquisition flag 43 a has changed to “0”. If the acquisition flag 43 a remains “1” (No in S 502 ), the CPU 41 repeats S 502 is repeated. If the acquisition flag 43 a has changed to “0” (Yes in S 502 ), the CPU 41 determines whether the easy log has been completed during the device monitoring process and then advances to S 504 . In 5501 , if the acquisition flag 43 a is “0” (No in S 501 ), the CPU 41 executes the easy-log acquiring process (S 502 ), and advances to S 504 .
[0104] In the easy-log acquiring process, the easy log is acquired from the peripheral device being monitored. The easy log file of any peripheral device, which is stored in a sub-folder included in the “Device log” folder and whose name is identical to that of the peripheral device, is updated to the latest state. Further, if the easy-log acquiring process proceeds during the device monitoring process, another easy-log acquiring process can be prevented from being performed unnecessarily.
[0105] In S 504 , the CPU 41 executes a detailed-log acquiring process described later. As a result, detail logs are thereby copied from all peripheral devices to monitor. The detail logs thus acquired are stored in the sub-files whose names are identical to those of the peripheral devices in the “Device log” folder.
[0106] Next, the CPU 41 creates a work folder in which to form collection files in the HDD 44 (S 505 ). The CPU 41 reads out the value of a registry 44 d that should be collected as a log and stores the value thus read is made into a text file in the work folder (S 506 ). Subsequently, the CPU 41 copies the log folder 44 e (i.e., ‘log’ folder) in untouched configuration, in the work folder (S 507 ).
[0107] In S 508 , the CPU 41 copies the collection folder and stores this collection folder in the work folder. In S 509 , the CPU 41 creates a collection log file by compressing and encrypting the work folder. That is, in S 509 , the CPU 41 creates one collection log file by compressing and encrypting the work folder in which the value of the registry 44 d and the work folder holding the “log” folder is stored with folder configuration untouched, and copies the collection log file in the desktop folder provided in the HDD 44 by using the OS. In S 510 , the CPU 41 deletes unnecessary work folder and ends this process.
[0108] Thus, the log collecting process is performed, merely by inputting from the user the instruction for the execution of the log collecting program 44 b . Therefore, a detail log can be acquired from each peripheral device and a collected log file can be immediately generated. The user may analyze the collected log file generated in the log collecting process, to confirm the value of the registry 44 d and various log files, which are stored in the collected log file. The user can therefore identify the cause of any trouble that has occurred while the PC 11 is executing processes. Moreover, since the configuration of the “log” folder is preserved in the collected log file, the name of any peripheral device, from which an easy log and a detail log have been acquired, is associated with both the easy log and detail log. Hence, the peripheral device that has generated the easy log and detail log can be easily identified.
[0109] Next, the detail-log acquiring process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 9( a ). FIG. 9( a ) is a flowchart showing this process. This process is executed to acquire a detail log from any peripheral device corresponding to the monitoring target. The CPU 41 executes this process during the log collecting process described above.
[0110] In this process, a counter M is provided in the RAM 43 . First, the CPU 41 calculates by substituting “0” as an initial value for the counter M (S 601 ). The counter M counts loops of the process of acquiring detail logs from all peripheral devices that are monitored during the detail-log acquiring process.
[0111] Subsequently, the CPU 41 determines whether the count of the counter M is smaller than the number N of peripheral devices which is held in the RAM 43 during the device monitoring process (S 602 ). In S 602 , the CPU 41 determines whether the process loop of acquiring detail logs from the peripheral devices has been completed. If the count of the counter M is equal to or greater than the number N (No in S 602 ), the CPU 41 determines detail logs have been acquired from all peripheral devices to monitor. In this case, the detail-log acquiring process is terminated.
[0112] If the count of the counter M is smaller than the number N (Yes in S 602 ), the CPU 41 advances to S 603 . S 603 to S 610 are equivalent to the process of acquiring detail logs from the respective peripheral devices. First, in S 603 , of the information concerning the peripheral devices and held in the RAM 43 during the device monitoring process, the CPU 41 reads out the data about the peripheral device of the serial number identical to the count of the counter M. Then, the CPU 41 copies the detail log from the detail log area 23 a that is a removable storage area of the peripheral device.
[0113] Next, the CPU 41 executes the detail-log time correcting process described later (S 604 ). That is, the time data items described in the warning log and error log, both included in the detail log, are adjusted to the time axis applied in the PC 11 . Then, the CPU 41 determines whether the “Device log” folder in the log folder 44 e includes a sub-folder whose name is identical to the name of the peripheral device that has copied the detail log (S 605 ). The detail log describing the time corrected is stored in the sub-folder whose name is identical to the name of the peripheral device. If such a sub-folder exists (Yes in S 605 ), the CPU 41 advances to S 607 . If such a sub-folder does not exist (No in S 605 ), the CPU 41 creates a sub-folder whose name is identical to that of the peripheral device is formed in the “Device log” folder (S 606 ). In this case, the CPU 41 advances to S 607 .
[0114] In S 607 , the CPU 41 determines whether the sub-folder whose name is identical to the name of the peripheral device includes the “detail.log” file. Here, detail log is stored in the “Detail.log” folder. If such a “detail.log” file exists (Yes in S 607 ), the CPU 41 merges the “detail.log” file with the content of the detail log corrected in terms of time and then stores them (S 608 ). At this point, the identification number of the detail log, which is stored in the “detail-log” file is compared with the identification number of the detail log copied in S 603 . If a detail log that has the same identification number exists, this detail log is regarded as one acquired in the past, and is not merged with the “detail. log” file. As a result, this can prevent identical detail logs, if any, from being described together in the “detail.log” file. When S 608 is completed, the CPU 41 advances to S 610 .
[0115] If a “detail.log” file is not found to exist, in S 607 (No in 5607 ), the CPU 41 creates a “detail.log” file is formed in the sub-file whose name is identical to that of the peripheral device which has copied the detail log, and copies the content of the detail log corrected in terms of time in the “detail.log” file (S 609 ). Then, the CPU 41 advances to S 610 .
[0116] In S 610 , the CPU 41 increments the count of the counter M by “1”. The CPU 41 then returns to S 602 . Thus, any other peripheral device can acquire a detail log.
[0117] Next, the detail-log time correcting process executed by the CPU 41 of the PC 11 will be described with reference to FIG. 9( b ). FIG. 9( b ) is a flowchart showing the detail-log time correcting process. This is a process of adjusting the time data items described in the warning log and error log, both included in the detail log, to the time axis applied in the PC 11 .
[0118] First, the CPU 41 determines whether the “Device log” folder in the log folder 44 e includes a sub-folder whose name is identical to the name of the peripheral device that has copied the detail log (S 650 ). If such a sub-folder exists (Yes in S 650 ), the CPU 41 advances to S 651 . In S 651 , the CPU 41 determines whether the sub-folder whose name is identical to the name of the peripheral device includes an “easy.log” file, i.e., easy log file. Whether an easy log has been acquired from the peripheral device that has copied the detail log can thereby be determined.
[0119] If an “easy.log” file exists (Yes in S 651 ), that is, an easy log has been acquired from the peripheral device, the CPU 41 substitutes the time data described in the detail log having the identification number same as the identification number described in the “easy.log” file by the time described in the easy log having the same identification number (S 652 ).
[0120] If the “Device log” folder in the log folder 44 e may not include a sub-folder whose name is identical to the name of the peripheral device that has copied the detail log (No in S 650 ) and the sub-folder does not include an “easy.log” file (No in S 651 ), the CPU 41 does not acquire easy logs have been acquired from the peripheral device. Therefore, the CPU 41 adds a marker to the detail log, showing all time data items described in the detail log are used in the peripheral device (S 653 ). By using this marker, anyone who refers to the log can recognize that the time data items described in the detail log are those used in the peripheral device.
[0121] As described above, the easy log corresponds to the warning log and error log included in the detail log. Any logs having the same identification number have been generated at the same event in the same peripheral device. The time described in the easy log held in the “easy.log” file is one adjusted to the time axis applied in the PC 11 in the easy-log time correcting process. The time data items described in the warning log and error log included in the detail log in S 652 can therefore be adjusted to the time axis applied in the PC 11 . Hence, which log has been generated earlier, the warning and error logs included in the detail log or the PC log generated by the application program 44 c of the PC 11 and described in the PC log file, can be determined. This helps to reduce the load of analyzing the cause of any trouble. Further, the time data items described in associated easy log and detail log can be adjusted to the same value. Which log precedes the other, the information log or the PC log, can be determined, too.
[0122] As has been described, in the log collecting system 1 according to this embodiment, detail logs are acquired at regular intervals from all peripheral devices (i.e., printer 10 a , scanner 10 b and facsimile 10 c ) in the log collecting process performed as the PC 11 executes the log collecting program 44 b . Then, the detail logs concerning the operations of the peripheral devices (i.e., printer 10 a , scanner 10 b and facsimile 10 c ) and the PC logs concerning the operations the PC 11 has performed on the peripheral devices are compiled, generating a collected log file. Based on the collected log file, the user can confirm both the log generated in each peripheral device and the log generated in the PC 11 . The cause of any trouble in any process performed by the PC 11 can therefore be easily identified.
[0123] The warning log and the error log influencing the operation of the peripheral device included in the detail log are acquired as easy logs at all times or at intervals during the device monitoring process performed as the PC 11 executes the device monitoring program 44 a . The collected log file includes the easy logs thus acquired. Therefore, even if no detail logs have been acquired at a prescribed time, the cause of a trouble, if any, can be determined, to some extent, from the easy logs acquired at all times or at intervals and the PC log.
[0124] The data amount of the easy log acquired at all times or at intervals during the device monitoring process is smaller than the data amount of the detail log acquired at the prescribed timing during the log collecting process. As a result, this can suppress the load of communication between the PC 11 and each peripheral device. Therefore, logs for easily identifying the cause of a trouble that has developed in the process performed by the PC 11 can be collected, while suppressing the increase in the load of communication between the PC 11 and each peripheral device.
[0125] While the invention has been described in detail with reference to the embodiments thereof, it would be apparent to those skilled in the art that various changes and modifications may be made therein without departing from the spirit of the invention.
[0126] In the embodiment described above, the detail-log time correcting process is performed as illustrated in the flowchart of FIG. 9( b ). Instead, the detail-log time correcting process may be performed in the same manner as the easy-log time correcting process shown in FIG. 7 . In this case, the present-time data of the peripheral device may be acquired, too, from the timekeeping circuit 31 provided in the peripheral device, in order to copy the detail log from the detail log area 23 a.
[0127] If the detail-log correcting process is performed in the same manner as the easy-log time correcting process shown in FIG. 7 , which log has been generate earlier, the PC log in the PC 11 or the detail log, can be reliably determined. As a result, this can reduce the load of analyzing the cause of a trouble. Further, if the detail-log time correcting process is performed in the same manner as the easy-log time correcting process shown in FIG. 7 , part of the detail log (e.g., warning log and error log) may be corrected in terms of the time described. Then, the process time can be reduced even if many detail logs exist.
[0128] In the embodiment described above, the easy log area 22 a is provided in the RAM 22 that is a volatile memory, and the detail log area 23 a is provided in the EEPROM 23 that is a nonvolatile memory. Instead, these areas may be provided in whichever memory, a volatile one or a nonvolatile one. Moreover, the nonvolatile memory may be a flash memory or a hard disk, not the EEPROM 23 .
[0129] In the embodiment described above, the easy log area 22 a cannot be directly accessed from the PC 11 , while the detail log area 23 a can be directly accessed from the PC 11 . The invention is not limited to this configuration, nevertheless. The easy log area 22 a may be directly accessed from the PC 11 , and the detail log area 23 a may not be directly accessed from the PC 11 . If the easy log area 22 a can be directly accessible from the PC 11 , any easy log may be copied directly from the easy log area 22 a . In this case, the present-time data described in the peripheral device may be acquired from the timekeeping circuit 31 incorporated in the peripheral device, at the same time the easy log is copied, in order to perform the easy-log time correcting process. The detail log area 23 a may be rendered not directly accessible from the PC 11 . In this case, a detail-log requesting command is transmitted to each peripheral device. On receiving the detail-log requesting command, each peripheral device transmits the detail log to the PC 11 , in the same manner as in the easy-log transmitting process.
[0130] In the embodiment described above, the HDD 44 stores the log collecting program 44 b . Instead, the log collecting program 44 b may be stored in a compact disk, read only memory (CD-ROM) or a floppy disk (registered trademark), and may be activated from such a storage medium.
[0131] In the embodiment described above, easy logs are acquired from each peripheral device at regular intervals during the device monitoring process Instead, each peripheral device may be monitored at all times, and an easy log may be acquired at the time the easy log is generated in the peripheral device.
[0132] In the embodiment described above, a printer 10 a , a scanner 10 b and a facsimile device 10 c are exemplified as peripheral devices. Other devices that can be connected to the PC 11 , such as a camera and an external ODD, can be incorporated in a log collecting system according to this invention.
[0133] In the embodiment described above, one application program 44 c collects the PC logs generated from the respective peripheral devices in the log collecting program 44 b . Instead, a plurality of application programs may be executed so that the log collecting program 44 b may collect the PC logs generated in the respective peripheral devices. If two or more application programs are executed to collect the PC logs, the cause of a trouble, if any, can be more easily identified than otherwise.
[0134] In this case, the application programs that the PC log files have generated for the peripheral devices, respectively, are used in each of the application programs. The PC log file for each peripheral device may describe the identification information of the application program that has generated a PC log. And, PC log files may be generated for the peripheral devices, respectively, and a sub-folder whose name can identify the associated application program may be provided in the “PC log” folder, so that the PC log file generated by the application program may be stored in the sub-folder. Furthermore, the name of the PC log file of each peripheral device, which has been generated by the associated application program, may be one that can identify the associated application program. In either case, the application program that has generated the PC log file can be identified, and the load of analyzing the cause of any trouble can therefore be reduced.
[0135] Moreover, a log about the activation, termination and setting change of each application program, and a log concerning the communication with the OS may be generated, instead of the PC log generated in the above-described embodiment, and may be stored in the “PC log” folder and collected by the log collecting program. In this case, the cause of a trouble, if any, can be more easily identified than otherwise.
[0136] In the embodiment described above, the easy log 62 and detail log 61 generated for each peripheral device are stored in the sub-folder provided in the “Device log” folder and associated with each peripheral device. Instead, an easy log file and a detail log file are provided in the “Device log” folder, and the name of each of these log files may contain information that can identify the associated peripheral device. Alternatively, an easy log file and a detail log file that store the easy logs 62 and detail logs 61 generated in all peripheral devices, respectively, may be provided in the “Device log” folder, and may store the easy logs 62 and detail logs 61 , respectively, together with the identification information about the peripheral devices that have generated the logs. In either case, the peripheral device that has generated an easy log 62 and a detail log 61 can be easily identified.
[0137] In the embodiment described above, the identification number 61 b is described in both the easy log 62 and the detail log 61 . Instead, the time data 61 a may serve as identification number. In this case, the time data 61 a is described in so minute units as milliseconds, and the time data 61 a described in one log should not overlap the time data described in any other log. | A log collecting system includes a computer apparatus and at least one peripheral apparatus connected to the computer apparatus, the computer apparatus collecting a log that records operation of the at least one peripheral apparatus. The peripheral apparatus includes, a first log memory controlling section that stores a first log relating to all operation of the at least one peripheral apparatus in a first log memory region, and a second log memory controlling section that stores, in a second log memory region, a second log indicative of any influence on the operation of the at least one peripheral apparatus among the first logs. The computer apparatus includes, a third log memory controlling section that stores, in a third log memory region, a third log relating to the operation of the computer apparatus concerning the at least one peripheral apparatus, a fourth log memory controlling section that continuously or discontinuously acquires the second log stored in the second log memory region, and stores the second log in a fourth log memory region, a first log acquiring section that acquires, at a predetermined timing, the first log stored in the first log memory region and a log information creating section that creates one log information with the acquired first log, the third log stored in the third log memory region, and the second log stored in the fourth log memory region when the first log acquiring section acquires the first log. | 6 |
FIELD OF THE INVENTION
[0001] The present invention relates to copy protection generally and, more particularly, to a method and/or apparatus for video watermarking and steganography using simulated film grain.
BACKGROUND OF THE INVENTION
[0002] Watermarking and data hiding have been extensively researched (e.g., IEEE ICIP, ISCAS, ICMCS, ICASSP, and SPIE special sessions and conferences for the past two decades). Due to the significant broadband consumer electronics applications, such watermarking provides an underlying enabling technology for digital rights management, steganography, watermarking, copy protection, copyright protection, traitor tracing, and/or IP protection.
[0003] Conventional watermarking extraction techniques include (i) taking a large number (e.g., 1000) of the highest amplitude discrete cosine transform (DCT) coefficients in an image (or video frame), (ii) averaging 8×8 blocks of an image (essentially the equivalent to taking the DC 8×8 transform coefficients), (iii) subtracting the original copy and projecting the remaining copy onto a subspace, and (iv) finding salient points and Delaunay triangulating the salient points for representation as a graph.
[0004] Among conventional watermarking extraction techniques, working directly on a compressed video stream is effective computationally. Inserting a robust watermark into a compressed video stream involves subtle manipulation of standard high bitrate syntax elements of a stream. Information may be directly inserted into a video in the pixel domain prior to compression. However, by inserting video in the pixel domain prior to compression, a much higher data processing rate (typically 50 to 100 times higher) is needed. A compression process that follows inserting video in the pixel domain is inefficient since the information quality weakens. It is computationally efficient to insert the information into the compressed stream after all easily accessible sources of redundancy have been removed from the data.
[0005] Typically, when the bitrate is high and the syntax element that is in use includes less perceptually visible distortion, more information can be inserted into the compressed stream. This approach has led to the preference shown in the past towards inserting information into transform coefficients, particularly the low-frequency (the lowest frequency of which is the DC coefficients).
[0006] Conventional approaches including using transform coefficients that are quite complex and need processing of the majority of an entire compressed bitstream to effectively insert information. In addition, with conventional approaches, robustness, security, and imperceptibility could be improved.
[0007] Watermark/fingerprint insertion and extraction processes are computationally demanding. Watermarks and fingerprints inserted for traitor tracing should be robust, secure, and imperceptible and should not be removable without distorting the video. Conventional approaches mainly differ from each other by the models used to control fidelity, robustness, bitrate, and error rates.
[0008] It would be desirable to provide a method and/or apparatus for video watermarking and steganography that improves robustness, security, and imperceptibility of the watermarking insertion and extraction process.
SUMMARY OF THE INVENTION
[0009] The present invention concerns an apparatus comprising a first circuit, a second circuit, and a watermark detection circuit. The first circuit may be configured to generate a bitstream. The bitstream may comprise compressed video data and a watermark message which represents hidden information. The second circuit may be configured to (i) simulate film grain in response to one or more predetermined values on the watermark message and (ii) generate a video output. The watermark detection circuit may be configured to extract hidden information from the video output.
[0010] The objects, features and advantages of the present invention include providing a method and/or apparatus for video watermarking and steganography using simulated film grain that may (i) lower the complexity of watermark insertion, (ii) add a minimized bitrate to a compressed bitstream (e.g., that is extremely efficient) and/or (iii) remain competitive with other methods.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] These and other objects, features and advantages of the present invention will be apparent from the following detailed description and the appended claims and drawings in which:
[0012] FIG. 1 is a block diagram illustrating various components of video watermarking using simulated film grain in accordance with a preferred embodiment of the present invention;
[0013] FIG. 2 is a block diagram illustrating various components of video watermarking using simulated film grain in accordance with a preferred embodiment of the present invention;
[0014] FIG. 3 is a more detailed block diagram illustrating an example content provider in accordance with a preferred embodiment of the present invention; and
[0015] FIG. 4 is a more detailed block diagram illustrating an example decoder in accordance with a preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] Simulated film grain may be represented by extremely efficient syntax as described in H.264/MPEG4-AVC and “Film Grain Simulation for HD DVD Systems” by SMPTE, published Nov. 22, 2004, version 2, which is hereby incorporated by reference in its entirety. A high bitrate portion of a compressed video data stream may be modified (e.g., the film grain) by manipulating an extremely small portion of the video syntax. The leverage that is now available through simulated film grain may be effectively exploited for watermarking and/or fingerprinting. Simulated film grain may provide characteristics that are ideal for watermarking and/or fingerprinting applications.
[0017] Film grain is very visible and is specified in a bit-accurate way as described in “The Film Grain Technology Specification” by SMPTE, published May 5, 2005 as a registered design document (RDD), version 1.0, which is hereby incorporated by reference in its entirety Generally, any modification to the film grain characteristic is easily detectible. The film grain syntax permits specifying unique film grain characteristics on a picture-by-picture basis. Information may be embedded not only within the frequency and correlation characteristics of the specified film grain, but also within the temporal variation in the film grain patterns.
[0018] Typically, the rendered data rate of the film grain portion of decompressed video is extremely high. The effective compression ratio of the compressed simulated film grain may be many orders of magnitude higher than that of the underlying video sequence from which film grain has been removed through pre-processing. Generally, the film grain syntax is substantially more ‘leveraged’ than any other bitstream syntax elements.
[0019] Referring to FIG. 1 , a block diagram of a system 100 in accordance with a preferred embodiment of the present invention is shown. The system 100 generally comprises a block (or circuit) 102 , a block (or circuit) 106 , a block (or circuit) 110 , a block (or circuit) 114 , and a block (or circuit) 116 . The block 102 may be implemented as a content provider. The block 106 may be implemented as a transmission medium (or disc). The block 110 may be implemented as a decoder. The block 114 may be implemented as a display. The block 116 may be implemented as a watermark detection circuit. In general, the content provider 102 presents video image data, audio data or other data that is compressed and transmitted in a bitstream 104 to an input of the transmission medium 106 . The video image, audio and/or other data (e.g., a sequence of still images, etc.) in the data bitstream 104 generally comprises an encoded video or audio signal and a watermark. The encoded data on the bitstream 104 may be encoded by one or more encoding standards (e.g., MPEG-1, MPEG-2, MPEG-4, WMV, VC-9, VC-1, H.262, H.263, H.264/JVC/AVC/MPEG-4 part 10, AVS 1.0′, Real Networks, DIVX Networks, and any other open or proprietary methods for compression of audio-video data). The transmission medium 106 generally presents the compressed data stream 108 to an input of the decoder 110 .
[0020] In one example, the content provider 102 may comprise a video broadcast, DVD, or any other source of video data stream. The transmission medium 106 may comprise, for example, a broadcast, cable, satellite, or data network, a DVD, a hard drive, or any other medium implemented to carry, transfer, and/or store a compressed bit stream. In one example, the decoder 110 may be implemented as a separate system. The decoder 110 generally decompresses (decodes) the data bit stream and presents the data via a link 112 to the display 114 . The decoder 110 may also simulate a film grain in response to decoding the watermark. The watermark detection circuit 116 may extract the watermark from the simulated film grain. The watermark detection circuit 116 may be used for forensic (or other) purposes.
[0021] Referring to FIG. 2 , a block diagram of a system 100 ′ is shown in accordance with another embodiment of the present invention. A recorder 118 may encode the decompressed video output which includes the watermark. The recorder 118 may produce a bitstream on an output 115 . The recorder 118 may record the video output to produce an illegal (e.g., unlicensed) copy of the video. The illegal copy of the video may be saved to a disc 120 . A decoder 110 ′ generally provides simulated film grain with the watermark. The watermark detection circuit 116 ′ may extract the watermark from the disc 120 . The watermark may identify the disc (e.g., transmission medium 106 ′), the device and/or a playback session where the illegal copy originated. The watermark detection circuit 116 ′ may identify the disc 120 and/or playback session on a signal (e.g., INFO).
[0022] Generally, the video image may be encoded by the content provider 102 ′ with the watermark, stored on the transmission medium 106 ′ and sent to a user. The bitstream may be decoded by the decoder 110 ′ and presented as video, which may be presented to the display 114 . The output may also be presented to the recorder/encoder 118 where the user may perform illegal copying in contradiction to the rights of the owner of the work. From there, the disc 120 (or discs) may be distributed illegally. The decoder 122 may provide simulated film grain with the watermark. Later, the watermark may be extracted by the watermark detection circuit 116 ′ from the raw video of an illegally distributed copy 120 to identify the distributed disc, and to ban the misbehaving user.
[0023] The system 100 ′ may be adapted to the following example. A studio may create and distribute secure recordings for pre-release screening of Hollywood films. Generally, in addition to encryption, watermarking is necessary for security. Forensically-traceable watermarks are needed on all video outputs to identify which distributed copy was pirated. Also, it may be desirable to determine where the pirated copy was played.
[0024] The video image may be encoded by the content provider 102 ′ (optionally with a watermark) to identify the individual disc (or transmission medium 106 ′). The disc 106 ′ may be sent to a user. The user may decode the video image from the disc 106 ′ with the decoder 110 ′. The decoder 110 ′ may be a secure device which (i) modifies (or generates) the film grain from the original given by the content provider 102 ′ and (ii) indicates in the watermark and which playback session the particular output video was generated from (e.g., the time/date/player-id-number and conditional access module id number). The disc 120 may be copied illegally (e.g., a camcorder in a studio, or an analog copy taken of the video signal). The watermark may be extracted from the illegal copy 120 (e.g., by LSI or the FBI) with the watermark detection circuit 116 ′ to identify not only the disc/transmission, but also which device(s) and playback session(s) the copy came from.
[0025] The current HD-DVD standard discloses that each video frame needs to be checked for bit-accuracy at the decoder 122 by a CRC (cyclical redundancy code). The system 100 ′ needs to include a mechanism to get an exact measure of the decoded video (e.g., the CRC) for verification of bit-accuracy. In one example, a DVD player manufacturer could use a similar mechanism (e.g., a serial port on an HD-DVD player box, or possibly a firewire, SATA, or PCI bus) to present the extracted watermark information for whatever purpose the manufacturer chooses. In one example, a watermark detection system may be a DVD-player which may playback the pirated copy and extract the watermark information (e.g., session and disc origin of information for the recording).
[0026] Referring to FIG. 3 , a more detailed block diagram is shown illustrating an example implementation of the content provider 102 in FIG. 1 . The content provider 102 generally comprises a block (or circuit) 150 , a block (or circuit) 152 , a block (or circuit) 154 , a block (or circuit) 156 and a block (or circuit) 160 . The block 152 may be implemented as a watermark generator. The watermark generator 152 may produce watermarks (or hidden information). The block 154 may be implemented as an encoder. The block 156 may be implemented as a film grain modeler circuit. The block 158 may be implemented as a multiplexer. The source 150 may present a signal (e.g., VIDEO) to the encoder 154 . The encoder 154 may present a signal (e.g., COMPRESSED) to the multiplexer 158 . The watermark generator 152 may present the signal INFO to the film grain modeler circuit 154 . The film grain modeler circuit 156 may present a signal (e.g., SEI) to the multiplexer 158 . The film grain modeler circuit 156 may present a signal (e.g., A) to the encoder 154 . The signal SEI may comprise one or more syntax elements. The multiplexer 160 may present a signal (e.g., BITSTREAM).
[0027] In general, the content provider 102 may embed watermarks into the compressed bitstream using simulated film grain syntax. The content provider 102 may embed the watermarks in the bitstream with temporal and/or spatial characteristics of the film grain. The content provider 102 generally manipulates film grain intensity and film grain pattern (e.g., size and shape) by using film grain that is characterized by a frequency filtering type and inserted with additive blending. The watermark may be embedded by manipulating various parameters of a H.264/MPEG4-AVC Film Grain Supplemental Enhancement Information (SEI) message. The parameters of the SEI message (or watermark message) generally comprises a parameter log2_scale_factor and a parameter comp_model_value (e.g., film grain intensity in the different color bands and vertical and horizontal high cut frequency of the film grain).
[0028] In one example, the content provider 102 may present a watermark that may be independent of the original video provided by the source 150 . The film grain modeler 156 generates the signal SEI in response to receiving the watermark. The signal SEI may include various parameters of the SEI message. The parameter of the SEI message may vary depending on the watermark. The film grain modeler 156 may present the signal SEI to the multiplexer 158 .
[0029] In one example, the content provider 102 may present a watermark that may be dependent on the video and/or audio generated by the source 150 (e.g., embedded into the original video/audio). Generally, the film grain modeler 156 may be modified to insert the watermark generated by the watermark generator 152 . The watermark generator 152 may present the watermark on the signal A to the encoder 154 . The encoder 154 may generate the core film grain model with the original video/audio and the watermark. The encoder 154 may (i) estimate the original film grain generated by the original input source 150 , (ii) remove the original film grain, (iii) model the SEI message and (iv) produce a compact bitstream so that the original film grain may be reinserted by a decoder to emulate the original video film grain appearance. The signal COMPRESSED generally comprises compressed video/audio data and the SEI message.
[0030] The multiplexer 158 may present the embedded watermark and compressed video data (e.g., via the signal COMPRESSED) on the signal BITSTREAM if the watermark is dependent on original video/audio (or original video). The multiplexer 158 may present the watermark (e.g., via the signal SEI) on the signal BITSTREAM if the watermark is independent of the original video.
[0031] The syntax elements on the signal COMPRESSED and/or the signal SEI may be manipulated at a multiple of picture frequencies. The parameters of the SEI message are generally compliant with the ITU-T Rec. H.264/ISO/IEC 14496-10 standard. In general, the syntax elements may be generated by adjusting the following parameters of the SEI message: (i) log scale_factor, (ii) comp_mode_value[c] [i] [ 0 ], (iii) comp_model_value[c] [i] [1] and (iv) comp_model_value[c] [i] [2]. The parameter log_scale_factor generally specifies the logarithmic scale factor which is used to represent the film grain parameter in the SEI message. The parameter log_scale_factor may generally be in the range [2,7] to ensure the film grain simulator (e.g., to ensure the film grain simulation process may be performed by using 16-bit arithmetic). The parameter comp_model_value[c] [i] [0] generally specifies a film grain intensity for a color component c and an intensity interval i. Generally for all values c and i, the parameter comp_model_value[c] [i] [0] may be in the range [0,255] to ensure the film grain simulation may be performed using 16-bit arithmetic. The parameter comp_model_value[c] [i] [1] generally specifies the horizontal high cut frequency that characterizes a film grain shape for the color component C and the intensity interval i. Generally for all values c and i, the parameter comp_model_value [c] [i] [2] may be in the range [2,14] which generally includes all of the needed grain patterns. The parameter comp_model_value[c] [i] [2] generally specifies the vertical high cut frequency that characterizes the film grain shape for the color component c and the intensity interval i. For all values c and i, the parameter comp_model_value [c] [i] [2] may be in the range [2,14] which generally includes all of the needed grain patterns.
[0032] Each of the parameters log2_scale_factor, comp_model_value[c] [i] [0], comp_model_value[c] [i] [1], the comp_model_value[c] [i] [ 2 ] may be manipulated to present watermarking information generated by the watermark generator 152 . The SEI message comprises a parameter model_id and a parameter blending_mode_id. The parameter model_id may be set to 0 to identify that the film grain simulation model as frequency filtering. The parameter blending_model_id may be set to 0 to indicate an additive blending mode to blend the simulated film grain with the decoded frame.
[0033] Referring to FIG. 4 , a more detailed block diagram is shown illustrating an example implementation of the decoder 110 in FIG. 1 . The decoder 110 generally comprises a block (or circuit) 170 , a block (or circuit) 172 , a block (or circuit) 174 , and a block (or circuit) 176 . The block 170 may be implemented as a demultiplexer. The block 174 may be implemented as an H.264 decoder. The block 172 may be implemented as a film grain simulator circuit. The block 176 may be implemented as an adder circuit.
[0034] The demultiplexer 170 generally receives the bitstream from the transmission medium 106 . The demultiplexer 170 may present the signal COMPRESSED to the decoder 174 if the inserted watermark is dependent on the original video/audio generated from the source 150 . The decoder 174 may present the SEI message on a signal (e.g., B) to the film grain simulator 172 . The film grain simulator circuit 174 may generate film grain (e.g., which is representative of the watermark) on the signal FILM based on the values of the parameters in the message SEI generated by the encoder 154 . The film grain simulator 172 generally presents film grain on a signal (e.g., FILM) to the adder circuit 176 . The adder circuit 176 generally combines the film grain to the decompressed video to produce a video output on a signal (e.g., DECOMPRESSED). The watermark detection circuit 116 may receive the signal DECOMPRESSED to extract the watermark. The watermark detection circuit 116 may determine the watermark by estimating the intensity and the horizontal and vertical cut frequency of the film grain.
[0035] If the inserted watermark is independent of the original video/audio generated from the source 150 , the demultiplexer 170 may present the signal SEI to the film grain simulator circuit 172 . The film grain simulator circuit 174 may generate film grain on the signal FILM based on the values of the parameters SEI on message. The watermark detection circuit 116 may receive the signal FILM to extract the watermark. The watermark detection circuit 116 may be coupled to the outputs of the film grain simulator circuit 174 and the adder circuit 176 . In one example, the watermark detection circuit 116 may detect the watermark using a combination of the output of the film grain simulator circuit 172 (e.g., via the signal FILM) and the output of the adder circuit 176 (e.g., via the signal DECOMPRESSED). CRC values may be checked to ensure that (i) the film grain is accurately represented and (ii) the film grain in the video complies with existing technology. In general, decoders may need to be checked by the video at the output of the film grain simulator circuit 172 and/or the output of the adder circuit 176 for the purpose of HD-DVD conformance checking. By detecting the watermark at the output of the watermark simulator circuit 172 and at the output of the adder circuit 176 , watermark detection may take place with a minimum amount of changes to current hardware/architectures.
[0036] With film grain simulation, 13 different horizontal high cut frequencies and 13 different vertical high cut frequencies result in 169 unique film grain patterns. Adjacent cuts off values may result in extremely similar film grain appearance. A superior perceptual effect due to slightly increased randomness may be produced by modifying specific cutoffs in a pseudo-random fashion with film grain simulation to embed hidden information. In one example, 255 different film grain intensities may be used.
[0037] The watermark detection circuit 116 may extract the watermark from rendered/decompressed video stream (i) through the temporal and/or spatial characteristics of the film grain, (ii) by estimating the intensity and horizontal and vertical cut frequency of each frame, and detecting a signature pattern in the variation of these patterns, (iii) by estimating either the absolute or the relative frequency distribution of the film grain and the overall video signal, making the detection mechanism robust to attack, and/or (iv) by estimating the relative or absolute intensities of the film grain and the overall video signal.
[0038] The watermark detection circuit 116 may estimate the intensity and horizontal/vertical cutoff frequency of each frame and/or estimate the absolute or relative frequency distribution by various methods used for spectral estimation. These methods may include the classical periodogram, blackman-tukey, and/or a correlation method. More modern techniques of parametric modeling, autogressive and/or moving average estimation, and minimum variance estimation may also be used. Additionally, an ad hoc method may be used which may include a low-complexity approximation of one of the above mentioned techniques.
[0039] The watermark detection circuit 116 may also extract the film grain hidden information by (i) frequency filtering horizontally or vertically to change the horizontal and/or vertical cutoff frequencies of the film grain, (ii) modifying the intensity of the film grain of the combined video, the film grain video, or the underlying video without film grain, and/or (iii) removing the simulated film from the rendered/decompressed video. The present invention may involve synchronizing the rendered compressed video, and discover the underlying phase of the film grain insertion process, followed by removal of the simulated film grain.
[0040] Frequency filtering may modify the cutoff frequency by attenuating specific frequencies in the watermarked video stream. Frequency filtering may have the undesirable effect of attenuating frequencies both in the film grain and in the underlying video signal. Therefore, any attack should not be capable of significantly increasing the watermark error rate (e.g., decreasing the information rate of the watermark). If the cut-frequency signal levels are chosen to be separated sufficiently to cause such an attack, and to significantly degrade the visual quality of the video, a successful attack should remove the watermark or significantly reduce the watermark information rate without visible video degradation.
[0041] The underlying phase of the film grain may be linked to the picture order count (or picture display order) as defined in the H.264 standard. Without access to the bitstream syntax of the watermarked video, discovery of the underlying phase of the film grain can only be done with knowledge of the particular watermarking method that is generally in use. For example, a signature must be embedded into the watermark which enables the receiver to synchronize with the watermark (e.g., if a detection method uses synchronization). A typical example of a synchronization method may be a “start-code”. With the start code, a particular extracted pattern of information by the watermark detector can be used to indicate a starting point in the video stream. The starting point may be used for the initialization or synchronization of the detector.
[0042] Conventional watermarking techniques try to attain minimum distortion of the original signal by remaining below the perception level of most observers. In one example, a conventional method of inserting a watermark in the LSBs of a video signal (or the transform coefficients of the video) is (i) severely hampered in terms of the amount of information that can be transmitted in the watermark and (ii) very fragile to an attack that involves removing or inserting noise into the LSBs of the video (i.e., on the transform coefficients of the video) to destroy the watermark without significantly impairing video quality. The present invention may provide a watermark that may be strong enough to be clearly visible to observers. The aim of the film grain (or the SEI message) is to simulate traditional film grain to give the video the look-and-feel of traditional cinematography.
[0043] The present invention may provide watermark signal power (e.g., in both the pixel and frequency domains) that may be an order of magnitude or more stronger than traditional watermarks, since the watermark is meant to be visible. Many conventional watermark attacks such as noise addition or removal, and/or recompression, may be much less effective against a watermark that is intended to be visible by users. The present invention may provide a strong deterrent to attacks since the strength of these attacks must be increased and be strong as to have an effect that is visible to an observer to be effective. In effect, the present invention provides visible watermarking techniques that are robust against attack. The present invention may provide the primary advantage of conventional invisible watermarking techniques, which is the insertion of the watermark that is not discernable to an observer. The present invention, generally overcomes a significant barrier that has, to date, hampered all watermarking techniques from becoming commercially successful. Invisible watermarks are strongly desired, but to date watermarks have been to vulnerable to the typical operations that users typically subject watermarks to (e.g., recompression, noise introduction, and/or cropping).
[0044] The present invention provides an extraction process that may be resistant to translation, rotation, scaling, and general affine skew by making the detection process relative to rendered video local or global orientation/scale/contrast/etc. In general, film grain is random in its appearance. Due to random appearance of film grain, there may be a great deal of latitude in how the film grain may be modified while still being visibly acceptable.
[0045] The present invention may also preserve the integrity of the hidden information through the encoding and decoding process. Digital video is generally only available in unencrypted form in
[0046] The present invention may also preserve the integrity of the hidden information through the encoding and decoding process. Digital video is generally only available in unencrypted form in the analog domain. Therefore, not only is the film grain syntax unassailable as long as the new cryptography of HD DVD remains secure. In general, the only domain in which the rendered film grain may be attacked is in the pixel domain. It is difficult to attack film grain in the pixel domain since completely removing all film grain may noticeably blur the video. In particular, high texture areas with irregular motion cannot normally be cleaned with motion compensated filtering. In general, the nature and characteristics of the film grain and any signature data or hidden information for watermarking is embedded in the film grain is robust against attack in the analog domain.
[0047] Since film grain may be extremely difficult to perfectly remove in the analog domain without damaging the underlying video, it will be extremely difficult to remove the embedded hidden information from the film grain. Removing grain is particularly difficult in the lower frequencies of the film grain. Also, modifying the intensity of the film grain relative to the intensity of the underlying video in highly textured video regions may be extremely difficult without modifying the underlying video. Due to the random nature of the film grain, it may be difficult to synchronize any rendered natural (non-test pattern) video to the underlying film grain patterns that are being used, and thereby determine the precise film grain in order to do perfect film grain extraction.
[0048] The present invention may provide (i) an extremely low-complexity watermark insertion process which includes lower complexity than alternative methods, (ii) a low-complexity extraction process, (iii) a secure and robust implementation for inserting and extracting watermarking that are comparable to existing techniques and (iv) a completely orthogonal method to existing methods. The present invention may be implemented in future and alternative video standards. For example, the present invention may be implemented with VC-1 in a similar manner once a syntax is specified for film grain.
[0049] While the invention has been particularly shown and described with reference to the preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made without departing from the spirit and scope of the invention. | An apparatus comprising a first circuit, a second circuit, and a watermark detection circuit. The first circuit may be configured to generate a bitstream, wherein the bitstream comprises a watermark message which represents hidden information. The second circuit may be configured to (i) simulate film grain in response to one or more predetermined values on the watermark message and (ii) generate a video output. The watermark detection circuit may be configured to extract hidden information from the decoded video output. | 7 |
BACKGROUND OF THE INVENTION
The present invention relates to an improved method for making platinum-phosphine complexes and to certain platinum-phosphine-vinylsiloxane complexes.
The term platinum-phosphine complexes and platinum-phosphine-vinylsiloxane complexes, as used herein refers to complexes wherein the platinum atom in the complex has a formal oxidation state of zero.
Platinum-phosphine complexes have been known for many years. For example, Malatesta et al., Journal of the Chemical Society, 1957, 1186, disclose the synthesis of platinum-phosphine complexes.
Exemplary of known methods for making platinum-phosphine complexes is the reduction of a phosphine-complexed platinous chloride, said reduction being performed by a mixture of hydrazine, alcoholic potassium hydroxide, and an excess of non-complexed phosphine. Another known method, suitable for making trialkylphosphine complexes of platinum, is the displacement of boroallyl ligands on platinum by phosphines.
Another known method uses platinum-phosphine-olefin complexes as starting materials. An example of this method is the work of Fitch et al., as disclosed in the Journal of Organometallic Chemistry, 1978, 160, 477. Fitch et al. reacted vinylsilanes with platinum-phosphine-olefin complexes wherein the vinylsilanes have the general formula CH 2 ═CHSi(CH 3 ) y (OC 2 H 5 ) 3-y , y having a value of 0, 1, 2 or 3.
Each of these known methods of making platinum-phosphine complexes is fraught with difficulty: yields are low; starting materials are difficult to synthesize, difficult to handle and difficult to obtain; and the reactions are prone to side reactions in the presence of small amounts of contaminants. For example, small amounts of water can hydrolyze and cause condensation of the ethoxy-substituted vinylsilanes of Fitch et al., thus rendering Fitch et al's complexes either less useful, or totally useless.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a new and improved method for making platinum-phosphine complexes. It is a further object to provide a method for making platinum-phosphine-vinylsiloxane complexes. It is another object to provide novel platinum-phosphine-vinylsiloxane complexes. It is yet another object to provide curable silicone compositions that have enhanced stability at room temperature.
These objects and others are attained by the method and complexes of the present invention. The method of the present invention comprises contacting certain phosphines and platinum-vinylsiloxane complexes with one another in an oxygen-free environment. The complexes of the present invention are certain platinum-phosphine-vinylsiloxane complexes.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a method for making platinum complexes, said method comprising contacting a platinum-vinylsiloxane complex with a phosphine selected from the group consisting of R 3 P molecules and R 2 P(CH 2 ) m PR 2 molecules wherein each R is selected from the group consisting of monovalent hydrocarbon radicals free of aliphatic unsaturation and m has a value of 1, 2, or 3, said contacting being accomplished in a substantially oxygen-free environment.
The present invention further relates to platinum complexes having the general formula
T a PtQ b , wherein in said general formula
T is a phosphine selected from the group consisting of phosphines having the formula R 3 P and phosphines having the formula R 2 P(CH 2 ) m PR 2 , each R being a monovalent hydrocarbon radical free of aliphatic unsaturation and m having a value of 1, 2, or 3;
a has a value of 1 or 2;
Q is a vinylsiloxane; and
b has a value of 1 or 2.
The method of the present invention comprises contacting a platinum-vinylsiloxane complex with a phosphine.
Platinum-vinylsiloxane complexes are well known. Platinum-vinylsiloxane complexes are the result of reacting hexachloroplatinic acid with a vinylsiloxane having the general unit formula
R n 'SiO.sub.(4-n)/2, wherein each R' is a monovalent hydrocarbon radical; each n has a value of 1, 2, or 3; there is at least one R' unit in said vinylsiloxane having the formula CH 2 ═CH--, and there is at least one SiOSi linkage present in said vinylsiloxane.
Platinum-vinylsiloxane compounds have been described in U.S. Pat. No. 3,419,593, issued Dec. 31, 1968 to David N. Willing, the specification of which patent is hereby incorporated herein to further teach a method for making suitable platinum-vinylsiloxane complexes. U.S. Pat. No. 3,775,452, issued Nov. 27, 1973 to Karstedt also discloses methods for making suitable platinum-vinylsiloxane complexes.
In general, platinum-vinylsiloxane complexes are made by contacting a vinylsiloxane with a suitable platinum compound such as hexachloroplatinic acid. Hexachloroplatinic acid is well known and widely available commercially.
R' in the above general unit formula for the vinylsiloxane is a monovalent hydrocarbon radical. Thus, R' can be an alkyl radical, such as methyl, ethyl, propyl or butyl; an aryl radical such as phenyl or naphthyl; a cycloalkyl radical, such as cyclohexyl, cycloheptyl, and the like; an alkenyl radical, such as vinyl or allyl; or a cycloalkenyl radical, such as cyclohexenyl, cycloheptenyl and the like. At least one R' of each vinylsiloxane, on average, must be a vinyl radical.
The vinylsiloxane can be linear, branched or cyclic in structure. Examples of appropriate vinylsiloxanes include the following. The term Vi in the following examples of vinylsiloxanes and in this specification represents the CH 2 ═CH-- radical; the term Me represents the CH 3 -- radical.
ViMe 2 SiOSiMe 2 Vi; ##STR1## (MeViSiO) 3 ; (MeViSiO) 4 , the last two formulae representing cyclosiloxanes; and other structures.
Phosphines suitable for use in the method of the present invention are selected from those phosphines having the formula R 3 P, and those phosphines having the formula R 2 P(CH 2 ) m PR 2 , m having a value of 1, 2, or 3.
R in each of the above formulae is a monovalent hydrocarbon radical free of aliphatic unsaturation. Thus, R can be an alkyl radical, such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tertiary butyl, hexyl, heptyl, and the like. R can also be a cycloalkyl radicals, such as cyclopentyl, cyclohexyl, cycloheptyl, and the like. R can also be an aryl radical, such as phenyl, naphthyl and the like. R can also be an alkaryl radical, such as tolyl, xylyl, or mesityl. R can also be an aralkyl radical, such as betaphenylethyl, beta-phenylpropyl and the like.
Phosphines as above described are well known and widely available. Moreover, their synthesis is well known in the organic chemistry art.
Especially preferred phosphines for the method of the present invention are those in which R is selected from the group consisting of phenyl, cyclohexyl, and tertiary butyl radicals.
The contacting referred to in performing the method of the present invention is done by simply exposing the two reactants to one another as by simply mixing. Mixing can be accomplished manually, by placing the two reactants in a single vessel and swirling or shaking. More preferably, mixing is accomplished with a mechanical stirrer or mixer.
The method of the present invention comprises contacting the phosphine, as described above, with the platinum vinylsiloxane, as described above, in a substantially oxygen-free environment.
By substantially oxygen-free environment it is meant herein no more than 20 or 30 parts per million by weight of the environment in which the method of the present invention is being performed can be O 2 , molecular oxygen. Preferably, the O 2 concentration is less than 20 parts per million.
While not required, it is most convenient to perform the method of the present invention in an enclosed vessel, equipped with a stirrer, under a blanket of inert gas. Examples of commonly used inert gasses include nitrogen, helium, and argon. It is also frequently convenient to perform the method of the present invention with the two reactants dissolved in a suitable solvent.
Suitable solvents for use in the method of the present invention are those that will dissolve the two reactants, and will not appreciably react with either of the two reactants. Many common industrial solvents are suitable. For example, hexane, heptane, octane, toluene, benzene, xylene, acetone, and methyl-ethyl ketone are all suitable. Selection of the solvent, if a solvent is used, is not critical.
The method of the present invention can be performed at room temperature, or the temperature can be elevated. If the temperature is elevated, it is necessary to limit the temperature to avoid thermal decomposition of any of the reactants. If a solvent is used, it is desirable to provide a condenser for solvent vapors, and means to return the condensed solvent vapors to the enclosed vessel.
The reactants to be contacted with one another are combined in approximately, i.e. ±10%, stoichiometric amounts. Thus, if it is desired to produce the complex Pt(PPh 3 ) 3 , wherein Ph represents the phenyl radical, approximately three moles of PPh 3 are added to each mole of Pt present in the platinum-vinylsiloxane complex. If it is desired to produce the complex PtP(tBu) 3 (Me 2 ViSi) 2 O, wherein tBu represents the tertiary butyl radical and Vi represents the vinyl radical, and Me represents the methyl radical, then approximately one mole of P(tBu) 3 are added to each mole of Pt present in a platinum-vinylsiloxane complex wherein the vinylsiloxane is (Me 2 ViSi) 2 O.
The reaction in the method of the present invention is fairly rapid, and is generally completed in less than an hour. Simple routine experimentation can be used to determine optimum reaction conditions or reaction times, if such are desired.
If it is desired that platinum-phosphine-vinylsiloxane complexes be produced in the method of the present invention, phosphines having relatively sterically large groups should be used, e.g. tertiary butyl or cyclohexyl groups. Conversely, if a platinum-phosphine complex is desired, phosphines substituted with relatively sterically small groups should be used, e.g. methyl or ethyl.
Compositions of the present invention have the general formula
T a PtQ b , wherein
T is a phosphine selected from the group consisting of phosphines having the formula R 3 P and phosphines having the formula R 2 P(CH 2 ) m PR 2 , each R being a monovalent hydrocarbon radical free of aliphatic unsaturation and m having a value of 1, 2, or 3;
a has a value of 1 or 2;
Q is a vinylsiloxane; and
b has a value of 1 or 2.
The platinum in the above general formula will have either 3 or 4 complexation sites. Since the phosphine can be a monodentate ligand of the form R 3 P or a bidentate ligand of the form R 2 P(CH 2 ) m PR 2 , and the vinylsiloxane can also be a monodentate or a multidentate ligand, it will be noted that the sum of a plus b can have a value of 2, 3, or 4.
Particularly preferred complexes of the present invention are
Pt(P(C 6 H 5 ) 3 ) 3 ;
Pt((C 6 H 5 ) 2 PCH 2 CH 2 P(C 6 H 5 ) 2 ) 2 ;
Pt(C 6 H 11 ) 3 P((CH 2 ═CH)(CH 3 ) 2 Si) 2 O; and
PtC(CH 3 ) 3 P((CH 2 ═CH)(CH 3 ) 2 Si) 2 O.
The platinum complexes of the present invention are useful as catalysts for hydrosilylation reactions; as catalysts for hydrogenation of unsaturated organic compounds or polymers; as catalysts for the isomerization of olefins; as catalysts for the oligomerization of acetylene and other alkynes; and in many other applications which require a platinum catalyst.
The platinum complexes of the present invention resulting from the method of the present invention are especially useful as curing catalysts for curable silicone compositions comprising
(1) a silicone polymer having at least one unit selected from the group consisting of CH 2 ═CH--Si.tbd. units and .tbd.SiOH units;
(2) a silicone polymer having at least one .tbd.SiH unit; and
(3) a platinum complex formed by contacting a phosphine with a platinum-vinylsiloxane complex.
A curable silicone composition as described above is made by simply mixing the appropriate polymers and platinum complex together. Simple mixing is accomplished by mixers, such as Myers® mixers, sigmoid blade mixers, three-roll mills, two-roll mills, Baker Perkins® type mixers, and other known mixers.
Generally from 1 to 99 parts by weight of Component (1), from 1 to 99 parts by weight of Component (2), and a catalytically effective amount of the platinum complex are used. By catalytically effective amount it is meant herein an amount sufficient to allow the curable composition to be cured in a reasonable amount of time, such as an hour or less, at a reasonable elevated temperature, such as 35° C. or higher.
Catalytically effective amounts of the platinum-complex of the present invention vary from 1 part per million by weight of platinum metal to 0.1% by weight of platinum metal.
More preferably, the amounts of Components (1) and (2) are selected so that approximately equimolar amounts of .tbd.SiH on the one hand and .tbd.SiCH═CH 2 or .tbd.SiOH on the other hand are used.
A curable composition as described above is a useful coating material, such as a paper release coating. If a reinforcing filler, such as amorphous silica, is added to the curable composition, a useful elastomer will result upon cure.
The platinum complexes produced by the method are useful catalysts for both filled an unfilled curable silicone compositions.
The following Examples are here presented to further teach the method of the present invention and the use of the products of the present invention. All parts and percentages in the Examples are by weight unless otherwise specified.
CHARACTERIZATION METHODS
The products of the method of the present invention were characterized by the following methods:
Yield: Yields were determined by dividing the weight of the product actually obtained by the weight of product which would result from complete reaction and recovery of product, and multiplying the result of this division by 100%.
Elemental Analysis: Carbon and hyrogen percentages were determined by the combustion method. The complexes being analyzed were quantitatively burned in oxygen, and the resulting weights of CO 2 and H 2 O were determined. These weights were used to calculate the percentages of carbon and hydrogen originally present in the complex.
Phosphorous, platinum and silicon analyses reported herein were done by atomic absorption spectroscopy, which is a well known method for determining these elements quantitatively.
Yields reported herein were calculated on the basis of the amounts of phosphine in the reaction mixture.
The following test procedures were used to evaluate cured films in the following examples.
Smear--Smear of a coating was evaluated by lightly rubbing the cured coating with a finger. A wholly cured coating will not change in appearance upon rubbing. No change in the appearance in the smear test is recorded in the following examples as "no smear."
Rub-off--Rub-off of a coating was evaluated by vigorously rubbing the cured coating with a finger. The result "no ruboff" indicates that the coating could not be removed in this manner. The result "ruboff" indicates that the coating was easily removed.
Migration--Migration was evaluated herein by: first, adhering a strip of standard adhesive-coated tape to the cured coating by firmly pressing the side coated with adhesive to the cured coating; second, removing the tape from the cured coating by peeling the tape up; third, doubling the removed tape back upon itself with the adhesive coated side adhering to itself; and fourth, comparing the force required to peel the doubled tape to the force required to peel a freshly prepared, similarly doubled tape which had never been adhered to the coating. If the force required is substantially the same, no migration of the coating or components thereof has occurred. This result is recorded as "no migration." Total loss of adherence indicates that migration of coating components has taken place. This result is recorded as "migration.
The following terms are assigned the following meanings in the Examples for the sake of brevity: ##STR2##
EXAMPLE 1
1.35 g of platinum -(Me 2 ViSi) 2 O complex mixture consisting of the complex dissolved in (Me 2 ViSi) 2 O and higher oligomers consisting of (Me 2 SiO) units and Me 2 ViSiO 3/2 units, containing 4.02% platinum, were added to a solution consisting of 0.3 g of PPh 3 dissolved in 10 ml of pentane, all of the above ingredients being confined to a closed vessel under a nitrogen blanket. Yellow crystals rapidly precipitated. These yellow crystals were filtered, and washed with pentane. Residual pentane was removed by exposing the yellow crystals to reduce pressure for several minutes. The calculated yield was 84.7%.
Elemental analysis for carbon and hydrogen was consistent with the structure
______________________________________Pt(PPh.sub.3).sub.3 theory found______________________________________% carbon 66.06 66.34% hydrogen 4.59 5.03______________________________________
EXAMPLE 2
1.35 g of the platinum-vinylsiloxane complex mixture used in Example 1 were added to a solution consisting of 0.24 g of Ph 2 PCH 2 CH 2 PPh 2 dissolved in 10 ml of toluene. Said addition was accomplished in an enclosed vessel under a nitrogen blanket. The above reactants were mechanically mixed for 30 minutes, after which time the toluene was removed under reduced pressure. The residue was a yellow solid. This yellow solid was dissolved in pentane, then isolated by the procedure of Example 1. Yield was 72.4%. Elemental analysis was consistent with the structure
______________________________________Pt(Ph.sub.2 PCH.sub.2 CH.sub.2 PPh.sub.2).sub.2 theory found______________________________________% carbon 62.90 61.29% hydrogen 4.80 5.40______________________________________
COMPARISON TO EXAMPLE 2
The same reactants used in Example 2 were reacted together, in acetone, with no steps being taken to exclude oxygen from the reaction environment.
The resulting product had a melting point of 269° C.-270° C., as compared to a published value of 273° C.-274° C. for the compound
Ph.sub.2 P(O)CH.sub.2 CH.sub.2 P(O)Ph.sub.2
Elemental analysis was consistent with this structure:
______________________________________ theory found______________________________________% carbon 72.50 71.40% hydrogen 5.60 5.76% phosphorous 14.40 14.40______________________________________
Thus it is seen that failure to perform the method of the present invention in a substantially oxygen-free environment results in an oxidized phosphine rather than a platinum complex.
EXAMPLE 3
40 g of the platinum-vinylsiloxane complex mixture used in Example 1 and 1.80 g of P(tBu) 3 were heated together, with mixing, in an enclosed vessel, under a nitrogen blanket, to a temperature of 65° C. This temperature was maintained for 5 minutes, after which time the mixture was allowed to cool to room temperature.
A white solid separated, which solid was filtered, washed with (Me 2 ViSi) 2 O, and the residue was exposed to reduced pressure to remove volatile substances. The product was obtained in a yield of 79.4%, and had a melting point of 145° C.-147° C.
The product was subjected to X-ray structural analysis, which analysis proved the structure to be
PttBu.sub.3 P(Me.sub.2 ViSi).sub.2 O
Elemental analysis was consistent with the above structure:
______________________________________ theory found______________________________________% carbon 41.16 41.23% hydrogen 7.72 7.57% phosphorous 5.32 5.49% silicon 9.61 9.50% platinum 33.45 33.22______________________________________
EXAMPLE 4
80 g of the platinum-vinylsiloxane complex used in Example 1 were heated with 5.0 g of PCy 3 under a nitrogen blanket, with mixing. After a temperature of 85° C. had been attained and held for 5 minutes, the mixture was allowed to cool. A white solid separated, which solid was treated by the procedure of Example 3. The product was obtained at a yield of 63.2%, and had a melting point of 188° C.-189° C.
Elemental Analysis was consistent with the structure
______________________________________Pt(PCy.sub.3 (Me.sub.2 ViSi).sub.2 O) theory found______________________________________% carbon 47.20 48.20% hydrogen 7.72 7.95% phosphorous 4.60 4.50% silicon 8.47 8.75______________________________________
EXAMPLE 5
0.25 g of the complex produced in Example 4 were dissolved in sufficient toluene to produce a 0.71% platinum solution.
The following components were mixed together to form a curable silicone composition:
(1) 67.9 g of a polymer having the average formula ViMe 2 SiO(Me 2 SiO) 135 SiMe 2 Vi; and 0.63 g of methylvinylcyclosiloxanes;
(2) 3.22 g of a mixture consisting of
(a) 41.67 parts of a polymer having the average formula
Me.sub.3 SiO(MeHSiO).sub.35 SiMe.sub.3 ; and
(b) 58.33 parts of a (Me 2 SiO)/(MeHSiO) copolymer having a viscosity of 5 centistokes at 25° C.
(3) 1.29 g of the 0.71% platinum solution.
The viscosity of this mixture was monitored as a function of time. Additionally, the time required to cure a thin film at 130° C. was determined periodically. The criteria for cure were no smear, no ruboff, and no migration. See Table 1.
TABLE 1______________________________________Cure StabilityTime at 25° C. Viscosity Minimum Cure(hours) (Centistokes at 25° C.) Time at 130° C.______________________________________0 304 70 seconds5 308 --7.5 308 --24 344 75 seconds32 308 --64 420 --82 580 --154 gelled --______________________________________
COMPARISON TO EXAMPLE 5
The procedure of Example 5 was repeated with a platinum-vinylsiloxane complex instead of a complex of the present invention. This mixture gelled in 30 minutes.
The procedure of Example 5 was then repeated with a platinum-vinylsiloxane complex instead of a complex of the present invention. This time 2.44 parts of the inhibitor 3,5-dimethyl-1-hexyne-3-ol were included. The results of evaluation of this comparison are found in Table II.
TABLE 2______________________________________Cure StabilityTime at 25° C. Viscosity Minimum Cure(hours) (centistokes at 25° C.) Time at 82° C.______________________________________0 368 60 seconds5 476 --7 516 --12 gelled --______________________________________
Thus it is seen that the complexes of the present invention greatly enhance effective life of a curable silicone composition at room temperature without seriously compromising the ability to cure at elevated temperatures. | A new method for making platinum-phosphine complexes and novel platinum-phosphine-vinylsiloxane complexes are disclosed. These complexes can be used in curable silicone compositions, thus providing curable silicone compositions of greatly enhanced stability at room temperature. The ability of the compositions to cure at elevated temperatures is not significantly compromised. | 2 |
BACKGROUND
1. Technical Field
The present invention relates to an LED illumination apparatus that uses an LED (light emitting diode) attached to a socket of a fluorescent light fixture. The contents of the following patent application is incorporated herein by reference, NO. 2009-259493 filed on Nov. 13, 2009, and NO. 2010-028309 filed on Feb. 11, 2010.
2. Related Art
LED illumination apparatuses that use a white LED with high luminance, energy saving capability, and long life have already been developed to replace conventional illumination apparatuses such as fluorescent lamps.
Patent Document No. 1: Japanese Patent Application Publication No. 2001-351402 Patent Document No. 2: Japanese Patent No. 4156657 Patent Document No. 3: Japanese Utility Model Registration No. 3148176
Patent Document No. 1 proposes an LED illumination apparatus that can be attached to an already-installed fluorescent light fixture with ease.
Patent Document No. 2 proposes an LED illumination apparatus that is assembled efficiently.
FIG. 11 shows an internal structure of a conventional LED illumination apparatus. The LED illumination apparatus includes a main body 1 , a cap 3 , a print substrate 4 , a plurality of LEDs 5 , and an electric wire 7 , where the cap 3 holds a pair of pin terminals 2 attachable to an already-installed fluorescent light fixture and is joined to the main body 1 , the print substrate 4 is accommodated in the main body 1 and has an electric control circuitry mounted thereon, the plurality of LEDs 5 are mounted to the print substrate 4 , the electric wire 7 has one end connected to the print substrate 4 and the other end connected to the pair of pin terminals 2 , and the pair of pin terminals 2 and the electric terminal 7 are connected to each other by swaging or soldering. The connection by waging or soldering is not only difficult to work with, but also the electric wire, once connected, is structurally difficult to be removed, and the parts exchange is difficult to pursue.
Patent Document No. 3 proposes an LED illumination apparatus having an LED illumination section and/or the LED itself exchangeable. The structure of bringing the contacts into contact with each other has a possibility of causing outage and contact failure, which is not favorable as an illumination apparatus.
Wiring in some fluorescent light fixtures is such that only one pole of the pair of electrodes of the socket 8 is connected to the power source, as shown in FIG. 12 . Therefore, both of the pin terminals 2 should be connected to the print substrate 4 . One method to realize this is to connect both of the pin terminals 2 to the print substrate 4 via two electric wires, as shown in FIG. 11 . Another method is to connect a round terminal 9 a to one end of the electric wire 7 drawn from the print substrate 4 , to be connected to a pin terminal 2 using screw, as shown in FIGS. 13A and 13B . Note that the round terminal 9 a and a round terminal 9 b that is different from the round terminal 9 a are short circuited therebetween using a jumper line 10 , and the round terminal 9 b is connected to another pin terminal 2 using screw.
SUMMARY
In this way, with a conventional method, parts exchange and the like are difficult. Other problems also exist such as unfavorable operability and reliability, and necessitating additional parts.
So as to solve the above-stated problems, according to a first aspect of the innovations herein, provided is an LED illumination apparatus including: a cap having a terminal electrically coupled to a socket of a fluorescent light fixture; and a main body having an end coupled with the cap, where the main body includes: an LED; and a coupler to electrically couple the terminal to the LED, the terminal being fitted in the coupler.
In the above-stated LED illumination apparatus, the coupler may be removably coupled with the terminal. In the above-stated LED illumination apparatus, the coupler may include a lock section removably coupled with a groove formed on the terminal. The above-stated LED illumination apparatus may have such a structure that the lock section has flexibility or elasticity, and by means of the flexibility or the elasticity, the lock section removably couples the terminal to the coupler.
In the above-stated LED illumination apparatus, the coupler may be removably coupled with the cap. In the above-stated LED illumination apparatus, the coupler may include a lock section removably coupled with a lock engaging section formed on the cap. The above-stated LED illumination apparatus may have such a structure that the lock section has flexibility or elasticity, and by means of the flexibility or the elasticity, the lock section removably couples the cap to the coupler.
In the above-stated LED illumination apparatus, the cap may include a holding section to hold the coupler. In the above-stated LED illumination apparatus, the terminal may be electrically insulated from the cap. The above-stated LED illumination apparatus may have such a structure that the terminal is a pair of pin terminals, and the coupler is electrically coupled with both of the pair of pin terminals. In the above-stated LED illumination apparatus, the coupler may be an integrally formed metal plate.
In the above-stated LED illumination apparatus, the main body may further include an electric wire to electrically couple the coupler with the LED. The above-stated LED illumination apparatus may have such a structure that the main body further includes a print substrate provided with the LED and an electric control circuitry, and the electric wire has an end connected to the coupler and the other end connected to the print substrate.
The above structure allows to exchange the parts such as an LED illuminating section and/or the LED itself with ease.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded view of an LED illumination apparatus according to the present invention (Embodiment Example 1).
FIG. 2 is a sectional view of the LED illumination apparatus according to the present invention (Embodiment Example 1).
FIG. 3 is a sectional view of a cap 3 according to Embodiment Example 1.
FIG. 4 is an internal perspective view of the cap 3 according to Embodiment Example 1.
FIG. 5 is a perspective view of a connecting terminal 6 according to Embodiment Example 1.
FIG. 6 shows the state in which the cap 3 is assembled with the connecting terminal 6 according to Embodiment Example 1.
FIG. 7 shows a sectional view of the state in which the cap 3 is assembled with the connecting terminal 6 according to Embodiment Example 1.
FIG. 8 is a perspective view of a cap 3 and a connecting terminal 6 according to Embodiment Example 2.
FIG. 9 is a perspective view of a cap 3 and a connecting terminal 6 according to Embodiment Example 3.
FIG. 10 is an enlarged view of a lock section 6 d according to Embodiment Example 3.
FIG. 11 is an exploded sectional view of a conventional LED illumination apparatus.
FIG. 12 is a wiring diagram of a fluorescent light fixture.
FIGS. 13A and 13B are a connection diagram for a conventional LED illumination apparatus.
DESCRIPTION OF EXEMPLARY EMBODIMENTS
As shown in FIG. 1 and FIG. 2 , an LED illumination apparatus according to the present embodiment holds a main body 1 , a cap 3 , a print substrate 4 , an LED 5 , a connecting terminal 6 , and an electric wire 7 , where the cap 3 holds a pair of pin terminals 2 fitted to a socket 8 of a fluorescent light fixture and is joined to the main body 1 , the print substrate 4 is accommodated in the main body 1 and has an electric control circuitry mounted thereon, the LED 5 is mounted to the print substrate 4 , the connecting terminal 6 is for connection with the pair of pin terminals 2 , and the electric wire 7 has one end connected to the print substrate 4 and the other end connected to the connecting terminal 6 .
The pair of pin terminals 2 are electrically coupled to the socket 8 of the fluorescent light fixture. The connecting terminal 6 electrically couples the pair of pin terminals 2 and the LED 5 . The pair of pin terminals 2 are fitted into the connecting terminal 6 . The connecting terminal 6 is removably coupled to the pair of pin terminals 2 . The connecting terminal 6 may be an integrally formed metal plate. The pair of pin terminals 2 may be an example of a terminal connected to a socket of a fluorescent light fixture. The connecting terminal 6 may be an example of a coupler.
In the present embodiment, the pair of pin terminals 2 are provided through a cap. However, the pair of pin terminals 2 are not limited to this structure. The pair of pin terminals 2 may include a member fitted to a socket, and a member connected to the connecting terminal 6 , so that both of the member fitted to a socket and the member connected to the connecting terminal 6 be electrically coupled to each other.
The term “electrically coupled” or the derivatives thereof may refer to a case where the corresponding members are in contact with each other, and not limited to a case in which the members are electrically connected to each other. The term “electrically coupled” or the derivatives thereof may also include a case where the members form a part of the electric path.
Embodiment Example 1
The main body 1 is a combination between an optical diffusion section 1 a made of a transparent or semi-transparent resin (e.g. polycarbonate resin) and a heat dissipating section 1 b made of an aluminum alloy or the like, and has a cylindrical form. However, the heat dissipating section 1 b may be created as a heat sink having convex and concave portions. Note that the main body 1 is not limited to the described combination, and may be made of only a resin.
The cap 3 having a pair of pin terminals 2 made of a copper alloy sized to suit to an already installed fluorescent light fixture is joined to each end of the main body 1 , and has a structure removable from the main body 1 for internal maintenance. Although FIG. 3 shows a cap 3 integrally formed with a pair of pin terminals 2 using an insulation resin, the pair of pin terminals 2 may be attached to the cap 3 by press fit or swaging. In addition, as shown in FIG. 4 , a groove 3 b for assembling the connecting terminal 6 and a lock engaging section 3 a for engaging the lock section 6 c of the connecting terminal 6 are formed within the cap 3 . Note that the material of the cap 3 may be metal, not limited to an insulation resin, as long as the pin terminal 2 and the cap 3 are electrically insulated from each other for avoiding electric shock. The groove 3 b holds the connecting terminal 6 . The groove 3 b may be an example of a holding section.
An electric control circuitry for rectification and voltage control (not shown in the drawings) and a plurality of LEDs 5 are mounted to the print substrate 4 , and the electric wire 7 to which the connecting terminal 6 is attached is drawn from an end of the print substrate 4 . The print substrate 4 is accommodated in the main body 1 . The LEDs 5 in this example are surface-mounting white LEDs, but may be shell-type LEDs. The number of LEDs 5 is defined according to the specification of illumination.
The connecting terminal 6 is fabricated by press working a copper alloy, and is configured by a crimp section 6 a , pin terminal connecting sections 6 b , and a lock section 6 c as shown in FIG. 5 . The electric wire 7 is connected to the crimp section 6 a . There are two pin terminal connecting sections 6 b , to allow connection by inserting the pair of pin terminals 2 therethrough. As shown in FIG. 6 and FIG. 7 , the lock section 6 c has a U-shaped sectional form, and an end thereof is bent to be engaged with the lock engaging section 3 a of the cap 3 , to hold the connecting terminal 6 . Note that the elasticity of the lock section 6 c facilitates removal of the connecting terminal 6 from the cap 3 using a simple tool to cancel the lock. Moreover, by introducing the connecting terminal 6 into the groove 3 b of the cap 3 , the shock from the electric wire 7 is prevented. The above structure allows to exchange the parts such as an LED illuminating section and/or the LED itself with ease. The pin terminals 2 can be connected to the print substrate 4 with ease using only a single electric wire 7 and the connecting terminal 6 .
Embodiment Example 2
FIG. 8 shows a cap 3 and a connecting terminal 6 according to Embodiment Example 2. The only difference of the lock section 6 c in Embodiment Example 2 from its counterpart in Embodiment Example 1 is that the lock section 6 c in Embodiment Example 2 has a tongue-like shape. The lock section 6 c is bent to be engaged with the lock engaging section 3 a of the cap 3 , thereby holding the connecting terminal 6 . Note that the elasticity of the lock section 6 c facilitates removal of the connecting terminal 6 from the cap 3 using a simple tool to cancel the lock. This also allows the cap 3 to hold the connecting terminal 6 with a simple structure, without using any additional parts.
Embodiment Example 3
FIG. 9 shows a cap 3 and a connecting terminal 6 according to Embodiment Example 3. The following explains only the differences from Embodiment Example 1. Each pin terminals 2 according to Embodiment Example 3 is provided with a groove 2 a . A lock section 6 d is formed on the connecting terminal 6 . The lock section 6 d is provided in the vicinity of the pin terminal connecting section 6 b , so as to be engaged with the groove 2 a , and holds the connecting terminal 6 by being engaged with the groove 2 a by means of the elasticity of the lock section 6 d . As shown in FIG. 10 , by being provided with a protrusion 6 d ′, the lock section 6 d is assuredly engaged with the groove 2 a . Note that the elasticity of the lock section 6 d facilitates removal of the connecting terminal 6 from the cap 3 using a simple tool to cancel the lock. In this way, according to the configuration of Embodiment Example 3, the cap 3 is not necessarily provided with a lock engaging section 3 a , unlike in the case of Embodiment Example 1, and so Embodiment Example 3 advantageously simplify the structure of a mold for shaping the cap 3 .
The present invention is applicable to an LED illumination apparatus that uses an LED (light emitting diode) attached to a socket of a fluorescent light fixture. | Parts exchange or the like is not easy with an LED illumination apparatus that uses an LED attached to a socket of a conventional fluorescent light fixture. Other problems also exist such as unfavorable operability and reliability, and necessitating additional parts. Provided herewith is an LED illumination apparatus including a cap having a terminal electrically coupled to a socket of a fluorescent light fixture and a main body having an end coupled with the cap, where the main body includes an LED and a coupler to electrically couple the terminal to the LED, the terminal being fitted in the coupler. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the field of animal processing to provide meat food products. More specifically, it relates to methods for reducing leakage of and contamination by matter from the rectum vent of an animal by obstructing the rectum vent.
2. Discussion of the Related Art
Public attention has recently been focused on the microbiological safety of commercially processed meat. Although this country's meat supply has remained consistently safe for many years, with a low incidence of microbial contamination causing illness, governmental agencies responsible for regulation and on-site inspection of commercial meat processing appear to be moving towards a policy of zero tolerance for microbial contamination. Accordingly, sources of contamination, including sources of food-borne pathogens and food-spoilage microbes, and the effects of current processing on contamination have come under scrutiny.
Generally, the origin of microbial contamination in raw meat, such as raw poultry, is the live animal; not the processing facility. The number of microbes found in a retail product is heavily influenced by the microbiological condition of the live animal, which is usually reared in close proximity with many of its kind, making transmission of potentially pathogenic and spoilage microorganisms possible.
The fecal micro flora of animals for slaughter is by far the predominant source of zoonotic microbes such as Campylobacter and Salmonella. Therefore, it is a desideratum for an effective method for reducing gross fecal leakage and contamination during processing.
Modern commercial animal processing generally is a multi-step process employing semi-automated apparatus for transporting an animal sequentially through different stations at high rates. The processing stations are, preferably, physically isolated from one another to minimize contamination from human sources and cross-contamination between stations. For example, after arriving at a processing plant, poultry are hung by their feet, stunned and then transported through a number of work stations ending with a cleaned carcass being cut into parts suitable for cooking or with the entire carcass being preserved for cooking.
More particularly, in modem, semi-automated, commercial processing plants, poultry is conveyed through a plurality of consecutive work stations or areas at speeds of about seventy birds per minute. Typically, the work stations include a slaughtering station where the throat of an invertedly suspended bird is cut and blood is permitted to drain; a scalding station, where the carcass is submerged in heated water to facilitate de-feathering; a de-feathering station, where spinning rubber fingers impact the outside of the carcass to remove the feathers; a washing station, where the exterior of the bird is washed by spraying with an unheated aqueous solution; a hock-cutting station where the feet are removed; and an evisceration station where the internal organs are removed from the remainder of the carcass.
Various measures have been put into place to avoid contamination and cross-contamination of meats during processing and to eliminate microbes introduced by the live animal. However, microbe-free meats have not yet been achieved, a long standing problem being the contamination and cross-contamination of poultry and other meats by the leakage of fecal materials from the rectum vent of the animal during processing.
For example, the de-feathering step can be a major source of contamination of poultry carcasses. As the spinning rubber fingers move from one carcass to another, they may spread fecal material leaked from a few carcasses to many carcasses.
Another step that can be a major source of contamination is evisceration. During evisceration the digestive tract organs are sometimes cut or otherwise opened so that ingesta or fecal material or other contents of the intestine may be released.
One approach to the problem of fecal leakage is to remove fecal matter from the animal to be processed. For example, one method involves squeezing or kneading the large intestine and rectum or cloaca of a poultry animal to force any fecal material out from the poultry animal. This is usually done manually and cannot effectively be accomplished at a rate which is compatible with the desired rate of operation of the conveyors in modern poultry processing facilities.
Another example of this approach involves using a suction probe inserted into the vent of the poultry animal. Loose fecal matter within the vent is supposedly withdrawn by the suction applied to the probe. Suction probes have not been particularly satisfactory, however. The probes often cannot remove all the loose fecal material due to the absence of air within the vent to create an air flow for entraining the fecal matter into the suction probe. Efforts to overcome this problem by increasing the amount of suction can actually work to suck out part of the intestine itself, thereby, damaging the poultry animal and often causing fecal leakage instead of preventing it.
Another approach to the problem involves obstructing the opening of the rectum vent. For example, one method includes gluing the vent opening shut. Fecal matter within the vent is supposedly prevented from leaking out through the vent by the adhesive seal. Adhesives have not been particularly satisfactory, due to leakage resulting from, for example, incomplete seals or tearing of the vent opening or adjacent area of the intestine during processing of the carcass.
Another example of this second approach involves inserting neoprene balls into the rectum vent to supposedly block intestinal fluids from leaking. However, such balls have demonstrated themselves to be nonstationary during the subsequent processing of the carcasses. This has resulted in fecal leakage, contamination and cross-contamination of carcasses.
Still another example of this approach is taken with relatively large animals such as cows, pigs, and sheep. A circular cut generally circumscribing the vent opening is made in the carcass and the entire circumscribed vent area is pulled out, pulling a portion of the intestine through the vent cut. The dislodged intestine immediately adjacent the anus or vent opening tied with a string or other clamping means to prevent intestinal leakage during further process steps. One drawback to this approach is that it is only useful with relatively large carcasses. A second drawback is that, even when it is used, it is labor-intensive and not compatible with the desired rates of operation of conveyors used in automated or semi-automated processing facilities.
Therefore, it is a desideratum for a method for reducing fecal leakage and contamination that can simply and effectively be incorporated into the automated or semi-automated processing of slaughtered animals into meat food products. It is also a desideratum for a method that does not preliminarily require the removal or suction of fecal matter from the rectum or the tying of the intestine of the animals to be processed.
Thus, there remains a definite need for an effective method for reducing gross fecal leakage and contamination. There remains a further definite need for methods which may be integrated into modern meat processing facilities to provide reliable, safe and consistent prevention of fecal leakage and contamination. The present invention satisfies these and other needs and provides further related advantages.
SUMMARY OF THE INVENTION
Now in accordance with the invention, there has been found a method that can be integrated into automated or semi-automated processes for processing a live animal in order to substantially reduce fecal leakage and contamination. The method involves slaughtering the animal and then obstructing its rectum with a gelled material. In some embodiments, a plug of gelled material is inserted into the rectum. The plug can be coated with fine particles of an abrasive material, such as wet-milled corn bran, to increase the adhesion between the plug and the rectal wall. In other embodiments, a gellable material is inserted into the rectum of the slaughtered animal under conditions to gel the material to form the plug. Both embodiments are useful in the processing of cows, pigs, sheep and poultry, such as chickens, game hens, ostriches, ducks and turkeys. The rectum is preferably obstructed early during processing and, when the animal is a poultry animal, it is most preferably obstructed before the poultry carcass is scalded and de-feathered.
In a preferred embodiment, the gelled plug is made by combining a cold water swelling granular starch with an aqueous sugar syrup. The gelled plug swells when it comes into contact with the slaughter animal's intestinal fluids forming an obstruction conforming to and having sufficient tack to create a seal with the rectal wall, thereby substantially preventing fecal leakage past the plug.
In some embodiments, the gelled plug contains a bore extending from the distal end through a portion of the plug. The bore reduces the back pressure caused by intestinal fluid and fecal material as the a plug is inserted into the animal's rectum. In preferred embodiments, when the slaughtered animal is a poultry animal, the distal end of the plug is positioned from about 2.5 cm to about 8 cm from the slaughtered animal's rectum vent.
Further, there has been found a pre-eviscerated animal carcass having a plug of gelled material in its rectum conforming to and forming a seal with the rectal wall to form an obstruction that substantially prevents fecal leakage. Still further, there has been found an apparatus for processing a live poultry animal, the apparatus having a slaughtering station for providing a slaughtered carcass, an insertion station for inserting a gelled plug or a gellable material into the rectum of the slaughtered carcass, a scalding station for submerging the carcass in heated water, a de-feathering station for removing feathers from the carcass, and an evisceration station for removing the internal organs from the carcass.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following description may concentrate primarily on the processing of poultry, such as chickens and turkeys, into meat food products to exemplify a multi-step processing operation. It should be readily apparent to the skilled artisan that the description with little or no modification might also apply to processing of other animals, including those animals which are sources for other meat food products such as, for example, beef, pork, lamb, veal and the like.
The method in accordance with the invention is useful during the processing of any animal having a rectum or cloaca and a vent. Representative animals include cows, pigs, sheep and poultry, such as chickens, game hens, ostriches, ducks, and turkeys. The method has been found particularly effective in substantially reducing fecal leakage and contamination from poultry.
In accordance with the inventive method, the rectum is plugged by inserting a gelled or a gellable material through an animal's rectum vent and into its rectum. In those embodiments, where a plug of gelled material is inserted into the rectum, the plug is made from any gelled material that is compressible, i.e., can be squeezed through the rectum vent and is swellable and resilient, i.e., after insertion expands to conform to and create a seal with the mucosal surface of the rectal wall and then maintain the seal. Additionally, the material has sufficient tack, so that once the plug is in place, it is not dislodged during the subsequent processing of the animal.
In some embodiments, the plug is coated with fine particles of an abrasive material to increase the adhesion between the plug and the rectal wall. The material can be any material that is compatible with preparing an edible food product. Representative food-compatible, abrasive materials include wet-milled corn bran.
The gelled plug is of any shape at least a portion of which has a substantially circular cross section. Representative shapes include cylinders, spheres, cones and frustrums, with cylinders being preferred. The specific dimensions will depend on the particular animal to be processed and will be readily determinable by one skilled in the art.
In some embodiments, the plug contains a bore extending from the distal end through a portion of the plug. Upon insertion into the rectum, intestinal fluid and fecal material can fill the bore, this reducing back-pressure on the plug and enhancing its positional stability.
It is an advantage of this embodiment that the insertion step is readily incorporated into conventional, semi-automated processing lines. In some embodiments, the gelled plug is inserted at a fully automated insertion station. In other embodiments, the gelled plug is manually inserted at an insertion station using a rounded, plastic, tampon dispenser-type mechanism. The plug is advantageously inserted any time after the animal has been slaughtered or stunned and before it is eviscerated. To minimize fecal leakage and contamination, the plug is preferably inserted during one of the initial processing steps.
Upon insertion, the intestinal fluids contact the plug causing it to swell, typically increasing the diameter of the plug from about 0.3 cm to about 2.25 cm. The swollen plug blocks the lumen of the distal colon, thus preventing the escape of fecal matter. Typical dimensions are set forth in the following table:
______________________________________Animal Diameter(cm) Length(cm)______________________________________Chicken .25-1.5 1-3Game Hen .25-1.5 1-3Duck .3-2 1-4Turkey .3-2.25 1-5Cow 10-15 13-20Sheep 5-9 10-15Pig 5-9 10-15______________________________________
In those embodiments, where a sufficient amount of a gellable material is inserted into the rectum of the slaughtered animal under conditions to gel the material and form a plug, the gellable material is any material that gels when combined with water or other suitable liquid to form a plug that swells (or hydrates) when it comes into contact with intestinal fluids present in the rectum. The swollen plug conforms to and has sufficient tack to create a seal with the rectal wall that is not dislodged during subsequent processing of the animal.
For ease of use in high speed, automated or semi-automated processing plants, the material should gel within a period of less than about one minute, preferably within a period of from about five to fifteen seconds. Furthermore, it is desirable that the material gel without chilling or without heating the water or other suitable liquid to its boiling point. It is preferable that the material gel at temperatures of from about 100° to about 170° F., more preferably from about 105° to about 108° F.
It is also an advantage of the second embodiment that the insertion step is readily incorporated into automated or semi-automated processing lines. The gellable material is manually inserted at an insertion station using a big barrel syringe. For example, a cold water swelling starch is combined with an aqueous sugar syrup in the syringe and then injected into the rectum of the slaughtered animal. The mixture rapidly gels and swells to form a plug conforming to and forming a seal with the rectal wall.
Representative materials for use in both embodiments include starches, such as cold-water-swelling or pregelatinized starches, and gums, such as agar, gelatin, low methoxyl pectin and carrageenan gums. Cold-water swelling starches are preferred. Exemplary cold-water-swelling starches are granular starches that have been subjected to an alcohol process, as described in Eastman, U.S. Pat. No. 4,465,702 (which patent is herein incorporated by reference), or further modified by substitution, crosslinking or oxidation. Common reagents for substitution are propylene oxide and acetic anhydride and common cross-linking agents are phosphorous oxychloride and adipic acid. Such starches typically have a gel-forming capability represented by a gel strength of greater than about 90 grams, as measured by the Voland Stevens method at room temperature. Preferred examples of such starches include MIRA-GEL 463, Soft Set and MIRA-THIK 468 and 469 which are available from A. E. Staley Co., Inc. MIRA-GEL 463 is most preferred.
The rectum is advantageously obstructed any time after the animal has been slaughtered or stunned and before it is eviscerated. To minimize fecal leakage and contamination, the gelled plug or the gellable material are preferably inserted as one of the initial processing steps. When processing poultry, the insertion step most preferably occurs after stunning and bleeding, but before the animals have been scalded. The depth of insertion of the plug into the rectum of a particular animal is dependent on the animal to be processed and will be readily determinable by one skilled in the art. With turkey, for example, the plug is preferably inserted so that the distal end is positioned from about 2.5 cm to 8 cm from the rectum vent. It is a benefit of the method in accordance with the invention that fecal leakage and contamination can be substantially reduced or eliminated without having to vacuum or suction the rectum or tie the intestine.
A determination of whether an effective seal has been formed can be pre-tested by manually squeezing the rectum of the animal being processed so that gases or material contained therein press against the seal. By varying the squeeze pressure, one can qualitatively determine that the plug can withstand a considerable buildup of back pressure before becoming dislodged or before permitting leakage of fecal material from the vent.
Once the plug has formed, the animal carcass continues along the processing line. After evisceration, the plug is discarded along with the intestine.
While the invention has been described in detail with reference to certain preferred embodiments thereof, it will be understood that modifications and variations are within the spirit and scope of that which is described and claimed. | Disclosed is a method for processing live animals into meat food products involving slaughtering the animal, inserting a gelled or a gellable material into the rectum of the slaughtered animal to form a plug obstructing the rectum, and then eviscerating the animal. The method can be integrated into automatic or semi-automatic processes for processing a live animal in order to substantially reduce fecal leakage and contamination. | 0 |
BACKGROUND
Ad-hoc networks are becoming more widely used, especially for mobile wireless devices. An attractive feature of ad-hoc networks is that they do not require a network infrastructure of base stations/fixed gateway nodes to enable communications between wireless nodes. Instead, the wireless nodes are capable of acting as base stations/access points that relay communications for other wireless nodes in the network. Thus, each node can, at various times, act as a source of information, a drain for information, and a router for information.
Traditionally, the focus of ad-hoc networks has been communications between wireless nodes on the network. More sophisticated ad-hoc networks that provide for access to fixed, wired networks have also been proposed. This allows wireless devices to communicate with other types of wired networks, such as the PSTN and the Internet.
One shortcoming associated with known ad-hoc networks, including the more sophisticated ad-hoc networks discussed above, is that they are typically oriented toward enabling communication between nodes, with the direction of such communication being somewhat random. These networks are not as efficient as possible for other types of communication, such as Internet-oriented communication, in which the flow of data is strongly directional (i.e., from fixed gateway nodes downward to wireless nodes and vice versa).
What is needed is a network that can efficiently handle communications such as the Internet that are directionally oriented.
SUMMARY
The aforementioned issues are addressed to a great extent by an ad-hoc network with an internet-oriented, software-defined dynamic infrastructure. The ad-hoc network includes at least one fixed gateway node and a plurality of wireless nodes. As used herein, a fixed gateway node means a node that is in a fixed location and that acts as a gateway, or access point, between the ad-hoc network and another network such as the Internet. In some embodiments, all of the wireless nodes are mobile. In other embodiments, some of the wireless nodes are mobile and some are at fixed locations, which shall be referred to herein as “home nodes.” (As used herein, the term “home node” should be understood to refer to a wireless node that is in a fixed location and should not be understood to be limited to a fixed wireless node installed in a residence). At least some of the wireless nodes, and, in some embodiments, all of the wireless nodes, may perform a routing function for other wireless nodes. In embodiments with multiple fixed gateway nodes, the fixed gateway nodes may be connected to the other network via a central node or may be connected directly to the other network. In the latter case, the fixed gateway node serves as a central node.
This ad-hoc network is hierarchical based on distances, measured in hop counts, to fixed gateway nodes. Each of the wireless nodes in the network (which may be fixed wireless nodes or mobile wireless nodes) in the ad-hoc network has a hop count with respect to each fixed gateway node. Any given wireless node may have one or more neighborhood nodes with which the wireless node can communicate directly. The neighborhood nodes will be either upstream (i.e., closer, as measured by hop count, to the fixed gateway node), downstream (further away, as measured by hop count, from the gateway node), or at the same distance (referred to herein as a peer node).
Each wireless node in the network also has at least one of each of four tables that describe the node's neighborhood and that are used for routing and other functions: 1) a downstream neighbor table, 2) a downstream routing table, 3) an upstream routing table, and 4) a peer table. The upstream routing table lists each upstream node in the wireless node's neighborhood together with a hop count to the fixed gateway node. In embodiments with multiple fixed gateway nodes, there is a plurality of upstream routing tables and each upstream routing table pertains to a different fixed gateway node. The peer routing table lists each peer node in the node's neighborhood along with an associated hop count to the fixed gateway node and, in embodiments with multiple fixed gateway nodes, each node has a separate peer table for each fixed gateway node. The downstream neighborhood table lists each downstream neighbor with respect to a particular fixed gateway node (again, there is a separate downstream neighborhood table for each fixed gateway node in embodiments with multiple fixed gateway nodes). The downstream routing table lists each downstream node (including downstream neighborhood nodes) reachable from the node together with an associated hop count, and in embodiments with multiple fixed gateway nodes, there is a multiplicity of downstream routing tables and each downstream routing table pertains to a different fixed gateway node. The aforementioned tables define the connectivity for the network. A number of triggers are generated during routing and at other times to cause the update of these tables. The tables are also audited periodically, either on an individual node basis or for the tables as a whole.
BRIEF DESCRIPTION OF THE DRAWINGS
The aforementioned advantages and features will be more readily understood with reference to the following detailed description and the accompanying drawings in which:
FIG. 1 is a schematic diagram of a network with one fixed gateway node according to a first embodiment.
FIG. 2 is a schematic diagram of a network with two fixed gateway nodes according to a second embodiment.
FIGS. 3 a and 3 b are conceptual schematic diagrams illustrating two superimposed networks that together comprise the network of FIG. 2 .
FIG. 4 is a schematic diagram of a network with fixed gateway nodes routed through a central node according to a third embodiment.
FIG. 5 is a logic diagram illustrating a packet routing process.
FIG. 6 is a flowchart illustrating in further detail the processing associated with one of the steps of FIG. 5 .
FIG. 7 is a flowchart illustrating in further detail the processing associated with another of the steps of FIG. 5 .
FIG. 8 is a flowchart illustrating the processing associated with a downstream trigger D 1 .
FIG. 9 is a flowchart illustrating the processing associated with a downstream trigger D 2 .
FIG. 10 is a flowchart illustrating the processing associated with an upstream trigger U 1 .
FIG. 11 is a flowchart illustrating the processing associated with a trigger T 4 .
FIG. 12 is a logic diagram illustrating various processing of a trigger T 5 depending upon the difference in hop counts between the sending and receiving nodes.
FIG. 13 is a flowchart illustrating in greater detail the processing associated with one of the steps of FIG. 12 .
FIG. 14 is a flowchart illustrating in greater detail the processing associated with one of the steps of FIG. 12 .
FIG. 15 is a flowchart illustrating in greater detail the processing associated with one of the steps of FIG. 12 .
FIG. 16 is a flowchart illustrating in greater detail the processing associated with one of the steps of FIG. 12 .
FIG. 17 is a flowchart illustrating in greater detail the processing associated with one of the steps of FIG. 12 .
DETAILED DESCRIPTION
In the following detailed description, a plurality of specific details, such as numbers of nodes and hops, are set forth in order to provide a thorough understanding of the embodiments described herein. The details discussed in connection with the preferred embodiments should not be understood to limit the present invention. Furthermore, for ease of understanding, certain method steps are delineated as separate steps; however, these steps should not be construed as necessarily distinct nor order dependent in their performance.
An exemplary network 100 is illustrated in FIG. 1 . The network 100 includes a fixed gateway node A, a plurality of mobile wireless nodes 1 - 14 , and a home wireless node 15 . The fixed gateway node A is connected to an Internet backbone and has wireless transmission and reception capability that allows it to act as an access point for a plurality of wireless nodes. Mobile wireless nodes 1 - 14 and home wireless node 15 also have wireless transmission and reception capability that allow them to communicate with other wireless nodes in the network and with the fixed gateway node (provided that the fixed gateway node is within range of the wireless transmission and reception system). Each of the mobile nodes 1 - 14 have the ability to act as routers for other wireless nodes in the network. (In alternative embodiments, only a portion of the mobile nodes have this ability.) The home node 15 does not have the ability to act as a router for other subscriber nodes in the embodiment of FIG. 1 . Although only one home node 15 is illustrated in FIG. 1 , it should be understood that there may be a plurality of such home nodes in other embodiments and that some or all of such home nodes may have the ability to act as routers. It should also be understood that, in various embodiments, a particular wireless node, whether it be mobile or fixed, may be configured such that it only acts as a router, only act as a subscriber (i.e., a source or drain of information) or acts as both a router and a subscriber.
As discussed above, the network 100 is an Internet-oriented network. Accordingly, each of the wireless nodes 1 - 15 can be classified based on the number of hops, or hop count, measured with respect to the fixed gateway node A. Nodes 1 and 2 have a hop count of 1, nodes 3 - 6 have a hop count of 2, nodes 7 - 9 have a hop count of 3, nodes 10 - 13 have a hop count of 4, and nodes 14 and 15 have a hop count of 5.
Each wireless node may have one or more other wireless nodes with which it is directly connected. As used herein, a second node is “directly connected” to a first node when the first node can communicate with the second node using its wireless communication system without requiring any other node to relay messages between the first and second nodes. The set of nodes that are directly connected to a node form the neighborhood for that node. The neighborhood for any wireless node can include nodes with lower hop counts (upstream nodes), nodes with the same hop count (peer nodes), and nodes with lower hop counts (downstream nodes).
Each of the nodes of the network 100 have at least one neighborhood node.
For example, the neighborhood for node 5 includes upstream nodes 1 and 2 , peer nodes 4 and 6 , and downstream nodes 8 and 9 . Every node in the network 100 has at least one upstream node (which may be the fixed gateway node A or another wireless node), and some have a plurality of upstream nodes. At any given time in any particular network, a wireless node may have zero (in which case it is isolated), one or many upstream nodes and may have zero, one or many peer nodes and zero, one or many downstream nodes. Each node will have downstream neighborhood tables (DNTs) and peer tables (PTs) that list each downstream and peer neighbor, respectively, along with the corresponding hop count relative to the fixed gateway node.
Each wireless node will also have an upstream routing table (URT) which will include the fixed gateway node with which the URT is associated and all upstream nodes (nodes with lower hop counts) in that node's neighborhood. The URT will also include a hop count for each of the neighboring nodes listed in the URT. Exemplary URTs for nodes 1 , 5 , and 8 are provided in Tables 1, 2 and 3 below.
TABLE 1
URT for Node 1
Node
Hop Count
A
1
TABLE 2
URT for Node 5
Node
Hop Count
1
1
2
1
TABLE 3
URT for Node 8
Node
Hop Count
4
2
5
2
The PT for a node will have a format similar to that of the URT, but will list peer neighbors rather than upstream neighbors. A detailed discussion of how the URTs and PTs are utilized for routing packets is set forth below.
Each node also has a downstream routing table, or DRT, which the node will utilize in order to determine how to rout packets downstream. The DRT for a node includes each node that is reachable from a node by traveling in a purely downstream direction regardless of the number of hops. In other words, an other node is included in the DRT for a particular node if and only if a path exists from the particular node to the other node, and that path is purely downstream (i.e., each successive node on the path has a higher hop count than the previous node). One result of the foregoing is that routing will always be done through the shortest path as measured by hop count. Another consequence is that the DRT of a node with only upstream and/or peer neighbors will be empty.
Three different types of downstream routing tables may be utilized: DRTs indexed by destination node, DRTs indexed by downstream neighbors, and DRTs double-indexed by both destination node and by downstream neighbors. Examples of the first type of DRT for nodes 1 , 2 and 5 and fixed gateway node A are presented below in tables 4-7:
TABLE 4
DRT Indexed by Destination Node for Node 1
Through Downstream
Node
Hop Count
Neighbors
4
1
—
5
1
—
8
2
4, 5
9
2
5
10
3
5
11
3
4, 5
12
3
4, 5
13
3
4, 5
14
4
4, 5
TABLE 5
DRT Indexed by Destination Node for Node 2
Through Downstream
Node
Hop Count
Neighbors
3
1
—
5
1
—
6
1
—
7
2
3, 6
8
2
5
9
2
5, 6
10
3
3, 5, 6
11
3
5
12
3
5
13
3
5, 6
14
4
3, 5, 6
TABLE 6
DRT Indexed by Destination Node for Node 5
Through Downstream
Node
Hop Count
Neighbors
8
1
—
9
1
—
10
2
9
11
2
8
12
2
8
13
2
8, 9
14
3
8, 9
TABLE 7
DRT Indexed by Destination Node for Fixed Gateway Node A
Through Downstream
Node
Hop Count
Neighbors
1
1
—
2
1
—
3
2
2
4
2
1
5
2
1, 2
6
2
2
7
3
2
8
3
1, 2
9
3
1, 2
10
3
1, 2
11
4
1, 2
12
4
1, 2
13
4
1, 2
14
5
1, 2
15
5
1, 2
Certain aspects of the DRTs listed above are worth noting. First, for all nodes in the DRT that are not directly accessible, the third column of the DRT indicates the directly accessible neighboring nodes through which such non-directly accessible nodes can be reached.
A second aspect of the DRT tables is that not all nodes with higher hop counts that could possibly be reached from a given node are included in the DRT. For example, the DRT for node 2 does not include an entry for node 4 even though node 4 has a higher hop count (2, as compared to a hop count of 1 for note 2 ) and even though there is a path from node 2 to node 4 through node 5 that does not require any upstream travel. The reason why node 4 is not included in the DRT for node 2 is that the portion of the aforementioned path from node 5 to node 4 is not purely downstream because both node 4 and node 5 have a hop count of 2 (i.e., nodes 4 and 5 are peers). Similarly, node 8 is listed in the DRT for node 2 , but no path through node 6 is shown. Again, this ensures that packets will be routed upstream toward the fixed gateway node through the shortest path as measured by hop counts.
A third aspect of the DRT tables is that multiple paths are shown in some instances. For example, the DRT for node 1 shows that node 11 is reachable in three hops via either node 4 or node 5 . The choice between possible paths can be made by the node based on a random selection, relative loading of the multiple nodes, or any other technique.
A second type of DRT is indexed by downstream neighbors rather than by destination node. For each downstream neighboring node, the DRT includes a list of all nodes reachable through purely downstream paths along with an associated hop count. This type of DRT is advantageous because its construction is simple—the DRTs of downstream neighboring nodes are simply concatenated. However, this type of DRT requires a search of the DRT table in order to select a shortest path for a particular destination. Examples of this second type of DRT for nodes 2 , 3 and fixed gateway node A are set forth below in Tables 8-10 below:
TABLE 8
DRT Indexed By Downstream Neighbor for Node 2
Nodes Reachable
Nodes Reachable
Nodes Reachable
Through Node 3/HC
Through Node 5/HC
Through Node 6/HC
3/1
5/1
6/1
7/2
8/2
7/2
10/3
9/2
9/2
14/4
10/3
10/3
11/3
13/3
12/3
14/4
13/3
15/5
14/4
15/5
TABLE 9
DRT Indexed By Downstream Neighbor for Node 3
Nodes Reachable Through Node 7/HC
7/1
10/2
14/3
TABLE 10 DRT Indexed By Downstream Neighbor for Fixed Gateway node A Nodes Reachable Nodes Reachable Through Node 1/HC Through Node 2/HC 1/1 2/1 4/2 3/2 5/2 5/2 8/3 6/2 9/3 7/3 10/4 8/3 11/4 9/3 12/4 10/4 13/4 11/4 14/5 12/4 15/5 13/4 14/5 15/5
As alluded to above, an advantage of using DRTs indexed by downstream neighboring nodes is that they are easily constructed and updated using information from downstream nodes. Each column of the DRTs above represents the downstream cluster of the corresponding downstream neighbor. The downstream cluster for any particular node can be formed by simply forming the union of each of the columns of the DRT for that node, adding 1 to each of the hop counts in the union, and then adding the particular node along with a hop count of 0. Thus, for example, downstream cluster for node 2 (DC 2 ) is shown below in table 11:
TABLE 11
DC i for Node 2
2/0
Node 2 itself with HC = 0
3/1
5/1
6/1
7/2
8/2
9/2
union of columns of
10/3
{close oversize bracket}
DRT of node 2 with
11/3
associated hop counts
12/3
13/3
14/4
15/4
As will be discussed in further detail below, the DC for a node is sent by that node to its upstream neighbors in a trigger message.
The third type of DRT is double indexed by both destination and downstream neighbor. An example of this type of double-indexed DRT for node 2 is provided in Table 12 below (where “x” signifies that a route exists between the given node and the destination node corresponding to a row through the downstream neighbor corresponding to a column):
TABLE 12 Double-Indexed DRT for Node 2 Destination Nodes Reachable Nodes Reachable Nodes Reachable Node Thru Node 3/HC Thru Node 5/HC Thru Node 6/HC 3 x/1 5 x/1 6 x/1 7 x/2 x/2 8 x/2 9 x/2 x/2 10 x/3 x/3 x/3 11 x/3 12 x/3 13 x/3 x/3 14 x/4 x/4 x/4 15 x/4 x/4
Double-indexed DRT tables have the advantages of efficiency for both construction and routing. In preferred embodiments, the DRTs are represented as sparse matrices when used with large numbers of nodes.
In the network 100 of FIG. 1 , there is only a single fixed gateway node A. However, it will be readily apparent that networks sometimes include multiple fixed gateway nodes. An example of a network 200 with the same wireless nodes 1 - 15 and two fixed gateway nodes A and B is illustrated in FIG. 2 . As illustrated in FIGS. 3( a ) and 3 ( b ), the network 200 can be thought of as the superimposition of the two networks 300 , 400 , one with fixed gateway node A and one with fixed gateway node B. Thus, the methods set forth above with respect to the network 100 of FIG. 1 can be extended to the two fixed gateway node network 200 of FIG. 2 by creating URTs, PTs, and DRTs for each node for each of the individual networks illustrated in FIGS. 3( a ) and 3 ( b ).
Some nodes (e.g., node 1 ) will have only a single URT because only one fixed gateway node is upstream of that node. Other nodes (e.g., node 3 ) will have multiple URTs for multiple fixed gateway nodes, but one URT will have a shorter route than the other (node 3 is one hop from fixed gateway node B but is two hops from fixed gateway node A). In this case, the URT corresponding to the shortest distance (smallest number of hops) is designated as the primary URT and the other URT is designated as the secondary URT. The secondary URTs can be used in cases where the path to the primary fixed gateway node associated with the primary URT is blocked. Finally, still other nodes will have multiple URTs with the same minimum distance/hop count. In such cases, both URTs will be designated as primary and both will used for routing purposes. The choice of which of the multiple URTs to use can be based on load balancing, random selection, or some other process.
Maintaining multiple node associations (through primary and secondary URTs or multiple primary URTs as well as in a single URT) is useful and important for three reasons: 1) as a vehicle moves, it may drop its principal association with one fixed gateway node and move to a new one; 2) a failure in part of the network may be recovered by using alternate routing through alternate nodes; and 3) alternate paths may be used for load balancing purposes.
In the network 200 illustrated in FIG. 2 , node 3 is only associated with fixed gateway node B and node 1 is only associated with fixed gateway node A. Also, node 3 is not in either the DRT or the URT for node 1 , and vice-versa. One way in which to effect communications between these nodes is via the Internet. However, in other embodiments of the invention, the fixed gateway nodes are linked to a central node which is then connected to the Internet. An example of such a network 400 with fixed gateway nodes A and B linked to central node 410 is illustrated in FIG. 4 . In such an embodiment, the central node 410 has a downstream routing table for each of the fixed gateway nodes and each of the wireless nodes in the network. Exemplary DRTs are set forth in Tables 13 and 14 below (although not shown below, double-indexed DRTs are also possible):
TABLE 13
Central Node DRT with Indexing by Downstream Neighbors
Through Downstream
Target Node
Hop Count
Neighbors
A
1
B
1
1
2
A
2
2
A, B
3
2
B
4
3
A
5
3
A, B
6
3
A, B
7
3
B
8
4
A, B
9
4
A, B
10
4
A, B
11
5
A, B
12
5
A, B
13
5
A, B
14
5
A
15
6
A, B
TABLE 14
Central Node DRT with Indexing by Destination Nodes
Nodes Reachable
Nodes Reachable
Through A/HC
Through B/HC
A/1
B/1
1/2
2/2
2/2
3/2
4/3
5/3
5/3
6/3
6/3
7/3
8/4
8/4
9/4
9/4
11/5
10/4
12/5
11/5
13/5
12/5
15/6
13/5
14/5
15/6
A node associated with multiple fixed gateway nodes A, B, C, etc. will have one set of the URT, PT, DNT and DRT for each of the corresponding fixed gateway nodes A, B, C, etc., respectively.
The routing algorithm from the internet to a subscriber (downstream routing) uses the DRTs to select one of several possible shortest routes to the subscriber. The routing algorithm from a subscriber to the Internet uses the URTs to select one of several possible shortest routes to the Internet. Subscriber to subscriber routing will use both DRTs and URTs. Alternate routing through upstream and downstream neighbors may be chosen in the case of routing failure, for “handover” from one fixed gateway node to another, or for load balancing.
The creation of the routing tables, and hence the network, will now be discussed. The process begins by constructing upstream routing tables. Initially, all wireless nodes have an infinite hop count, no neighbors, and empty URTs, and fixed gateway nodes have a zero hop count, no downstream neighbors and empty DRTs. As wireless nodes detect other nodes (which may be accomplished through periodic broadcast polling messages), the other wireless nodes are registered into that node's PT with an equal infinite hop count. As the fixed gateway nodes detect directly connected wireless nodes, those wireless nodes are assigned a hop count of 1. The wireless nodes detected by the fixed gateway node then propagate the information concerning the fixed gateway node to other nodes they have previously detected as peers and to new wireless nodes detected thereafter (the techniques by which this information is propagated will be discussed in further detail below). In this manner, the upstream hierarchy is established.
The DRT construction process can be triggered in either of two ways: 1) when the process of URT construction reaches nodes without downstream neighbors; or 2) when a node modifies its URT. In addition, events encountered during packet routing operations will also trigger modifications to the routing tables as discussed in further detail below.
Use of the routing tables to perform routing operations will now be discussed with reference to the logic diagram 500 of FIG. 5 . The process begins when the next packet arrives at step 510 . If the packet is intended for the node at which it is received at step 520 , the process is complete and step 510 is repeated. Otherwise, the direction of routing required—upstream, downstream, or subscriber-to-subscriber—is determined. There are several ways in which the routing direction of a packet can be determined. In some embodiments, each node can have separate buffers for upstream, downstream and subscriber-to-subscriber packets. In other embodiments, the routing process determines the direction based on the destination. In still other embodiments, the packets include a flag that indicates the direction. Other techniques will be readily apparent to those of skill in the art and are within the purview of the invention.
If downstream routing is required, subroutine 530 is performed. If upstream routing is required, subroutine 540 is performed. Finally, if subscriber-to-subscriber routing is required, subroutine 550 is performed.
The downstream routing subroutine 530 of FIG. 5 is illustrated in further detail in the flowchart 600 of FIG. 6 . A downstream neighbor is selected from the DRT at step 531 . If the destination node is a downstream neighbor, the packet is transmitted directly to that node. If a destination node is not a downstream neighbor (i.e., is not directly connected) but there is only a single path to that node available, the downstream neighbor node associated with that path is chosen. Otherwise, if multiple paths to the destination node are available, a choice between the available paths is made. The choice can be made any number of ways, including random selection from among the available paths, selection of the first available path found in the routing tables, selection of the least loaded downstream neighbor, etc. As will be discussed further below, peer routing is also possible.
If the selection of a downstream neighbor at step 531 was successful (i.e., a downstream neighbor was found in the routing tables) at step 532 , an attempt to transmit the packet to the selected downstream neighbor is made at step 533 . If the packet was successfully transmitted to the selected downstream neighbor at step 534 , the downstream routing subroutine ends and control returns to step 510 of FIG. 5 for processing of the next packet.
If the attempt at step 533 to transmit the packet to the selected downstream neighbor was unsuccessful at step 534 , then a trigger D 1 is generated at step 536 and a routing failure procedure is initiated at step 537 . Triggers, including the trigger D 1 , are messages that trigger a routing table update process upon the occurrence of some event. Triggers and the updating of routing tables will be discussed in further detail below. The routing failure procedure of step 637 may be handled in a number of ways. One possibility is that the packet is simply dropped, which will result in the sender failing to receive an acknowledgment from the destination node. Another possibility is to send a failure message to the sending node. This will allow the sending node to send another packet as soon as possible (i.e., without waiting for a timeout for an acknowledgment message). This may be desirable for time-sensitive applications, but there is a performance penalty associated with sending such failure messages. Other possibilities will be apparent to those of skill in the art.
In addition to the trigger D 1 of step 536 , a second trigger D 2 will be generated at step 538 if no downstream neighbor could be located in the DRT at step 531 . The D 2 trigger occurs because the upstream neighbor's DRT indicated that a path to the destination node was available through a node but that node's DRT does not include the destination node. The processing of the D 2 and other triggers will be discussed in further detail below.
The upstream routing subroutine 540 of FIG. 5 is illustrated in further detail in the flowchart 700 of FIG. 7 . An upstream neighbor is selected from the URT at step 541 . If the destination node is the upstream neighbor, the packet is transmitted directly to that node. If a destination node is not a an upstream neighbor (i.e., is not directly connected) but there is only a single path to that node available, the upstream neighbor node associated with that path is chosen. (Note that this will be the case where the hop count of the receiving node is 1, because the only upstream neighbor that will be fixed gateway node.) Otherwise, if multiple paths to the destination node are available, a choice between the nodes in the URT (excluding the fixed gateway node, which cannot be directly connected if multiple paths exist) is made. As discussed above in connection with the downstream routing process of FIG. 6 , the choice can be made any number of ways, including random selection from among the available paths, selection of the first available path found in the routing tables, selection of the least loaded upstream neighbor, etc. Again, peer routing is also possible.
If the selection of an upstream neighbor at step 541 was successful (i.e., an upstream neighbor was found in the routing tables) at step 542 , an attempt to transmit the packet to the selected upstream neighbor is made at step 543 . If the packet was successfully transmitted to the selected upstream neighbor at step 544 , the upstream routing subroutine ends and control returns to step 510 of FIG. 5 for processing of the next packet.
If the attempt at step 543 to transmit the packet to the selected downstream neighbor was unsuccessful at step 544 , then a trigger U 1 is generated at step 546 . Again, the processing of triggers will be discussed in further detail below. After the U 1 trigger is generated at step 546 , or if an upstream neighbor could not be located at step 542 , a routing failure procedure is initiated at step 546 . Like the downstream routing failure procedure, the upstream routing failure procedure of step 546 may be handled in a number of ways. One possibility is that the packet is simply dropped, which will result in the sender failing to receive an acknowledgment from the destination node. A second possibility is to send a failure message to the sending node.
The subscriber-to-subscriber routing subroutine 550 of FIG. 5 functions by utilizing a combination of the upstream and downstream routing procedures. When a subscriber node wishes to send a packet to another subscriber node that is not in that node's DRT, the packet is sent using the upstream routing subroutine 540 described above in connection with the flowchart 700 of FIG. 7 . When the packet reaches the central node, the central node will send the packet downstream using the downstream routing subroutine 530 described above in connection with the flowchart 600 of FIG. 6 .
The routing algorithms discussed above do not use the nodes in the PTs to route packets to peers. Thus, the PTs are only used in the event of changes to the routing tables (e.g., through trigger messages as will be discussed in further detail below). However, as alluded to above, the routing algorithms may be modified to use the PTs. In some embodiments, the PTs are used as alternate upstream routes. In other embodiments, the PTs may be used for downstream routing. In such cases, because peer neighbors do not necessarily include the same subscribers in their DRTs, the construction of the DRTs is modified to include the DRTs of peers as well. This allows for the use of alternate downstream routes through peers whenever available and useful without modification of the downstream routing process.
Triggers will now be discussed in greater detail. As mentioned above, triggers are messages that are generated upon the occurrence of some event that trigger the updating of routing tables at the receiving node. The processing of triggers is handled locally by the node receiving the trigger, and the processing of a trigger may generate another trigger of the same type or of a different type. As discussed above, three triggers—D 1 , D 2 and U 1 —are generated by the routing algorithms. The processing of these triggers will be discussed in detail.
Trigger D 1 occurs when a packet cannot be sent successfully to a downstream neighbor in a node's DRT. The processing of trigger D 1 is shown in the flowchart 800 of FIG. 8 . Upon receipt of a D 1 trigger, the downstream neighbor N k to which the packet could not be sent is taken out of the downstream neighborhood table at step 810 . If the DRT is of the type indexed by downstream neighbor, the column of the DRT corresponding to the unavailable downstream neighbor is updated at step 820 . (In embodiments in which the DRTs are indexed by destination node or are double indexed by destination node and downstream neighbor, appropriate modifications to the network tables are made.) The downstream cluster is then computed at step 830 by calculating the union of the columns of the DRT and adding the node N i and its hop count 0 (represented symbolically as {Ni, 0} in FIG. 8 ) as discussed above. Next, a T 4 trigger message including the downstream cluster is sent to upstream neighbors at step 840 (and to peers in embodiments in which peer routing is implemented) so that these neighbors can update their routing tables. The process is then complete.
Trigger D 2 occurs when a packet directed to a destination node is received at a node that does not have the destination node in its DRT. The processing of trigger D 2 is shown in the flowchart 900 of FIG. 9 . Upon receipt of a D 2 trigger, the downstream cluster of the receiving node is calculated at step 910 and a new T 4 trigger message including the downstream cluster is sent to upstream neighbors at step 920 to trigger the update of the routing tables of the upstream node that sent the packet. The process is then complete.
Trigger U 1 occurs when a packet cannot be sent successfully to an upstream neighbor in a node's URT. The processing of trigger U 1 is shown in the flowchart 1000 of FIG. 10 . The process begins by removing the upstream neighbor to which the packet could not be sent from the URT for that node at step 1010 . If the URT is not empty at step 1020 (meaning there is another upstream neighbor through whom packets can be sent), the process ends. If the URT is empty at step 1020 , node tables are re-computed at step 1030 as follows: the peer table becomes the upstream routing table, and the downstream neighborhood table becomes the peer table. The downstream neighborhood table and downstream routing tables are then empty. If the URT is still empty at step 1040 , the hop count for that node is set to infinity at step 1050 and processing ends. If the URT is not empty at step 1040 , the downstream cluster for the node is set to {N i +0} at step 1060 and a T 4 trigger message including the downstream cluster is sent to the upstream neighbors in the URT at step 1070 and processing ends.
The T 4 trigger is generated during the processing of the routing triggers as discussed above. The purpose of the T 4 trigger is to propagate downstream connectivity changes to upstream nodes in order to update their DRTs. The processing of a T 4 trigger is illustrated by the flowchart 1100 of FIG. 11 . The process begins at step 1110 with increasing by 1 the hop counts of the nodes in the received Trigger T 4 and updating the downstream routing table which, in embodiments with DRTs indexed by downstream neighbor, involves replacing the corresponding column in the DRT with the new column received in the T 4 trigger message. If the hop count for the node is zero at step 1120 (signifying that the highest level node has been reached), the process ends as there are no further upstream nodes. If the hop count is not zero at step 1120 (signifying that there is an upstream neighbor), the downstream cluster is calculated at step 1130 and sent to all upstream nodes in the URT in a new T 4 trigger message at step 1140 and the process is complete.
In addition to triggers T 1 -T 4 , there is a trigger T 5 . The T 5 trigger is generated by a periodic broadcast. That is, each node periodically broadcasts its node ID and hop count to inform neighboring nodes of its presence. When a broadcast message from another node is received that indicates a change of some kind, the T 5 trigger is the mechanism that propagates the change through the network.
T 5 trigger processing is illustrated by the flowchart 1200 of FIG. 12 . Processing begins at step 1201 , where the hop count of the node receiving the T5 trigger message (HC i ) is compared to the hop count (HC k ) of the node that sent the T 5 trigger message. If the hop count of the receiving node is more than 2 hops downstream of the sending node, the processing at step 1210 is performed. If the hop count of the receiving node is exactly 2 hops downstream of the sending node, the processing of step 1220 is performed. If the hop count of the receiving node is exactly 1 hop downstream of the sending node, the processing of step 1230 is performed. If the hop counts are equal, the processing of step 1250 is performed. Finally, if the receiving node is upstream of the sending node (the hop count of the sending node is greater than or equal to the hop count of the receiving node plus one), the processing of step 1270 is performed.
The processing of step 1210 is illustrated in the flowchart of FIG. 13 . The process begins at step 1211 , where the DNT, URT and PT of the receiving node are searched to determine whether the node ID (N k ) of the sending node is listed in any of those tables as being in the neighborhood of the receiving node. If so, the node is taken out of the corresponding table at step 1212 . Then, or if the sending node was not in any of the neighborhood tables at step 1211 , all nodes in the URT and PT for the receiving node are removed from those tables and added to the downstream neighborhood table DNT and the hop counts in the DNT are set to hop count of the sending node plus 2 at step 1213 . The sending node is entered in the URT of the receiving node at step 1214 , and the hop count for the receiving nose is set to the hop count of the sending node plus 1 at step 1215 . Finally, the node ID and hop count of the receiving node are sent to other nodes in the receiving node's neighborhood in a new T 5 trigger message at step 1216 and the process is complete. In other embodiments, the sending of the new T 5 trigger message at step 1216 is delayed until the next periodic broadcast. It is also possible to not update the hop counts at step 1213 but rather update them upon receipt of a periodic broadcast message from the neighboring nodes, which will contain the updated hop count after the T 5 trigger message is sent to the neighboring nodes at step 1216 .
The processing of step 1220 is illustrated in the flowchart of FIG. 14 . The process begins at step 1221 , where the DNT, URT and PT of the receiving node is searched to determine whether the node ID (N k ) of the sending node is listed in any of those tables as being in the neighborhood of the receiving node. If so, the node is taken out of the corresponding table at step 1222 . Next, the PT, DNT and URT are updated at step 1223 . The nodes previously listed in the peer table PT are added to the downstream neighbor table DNT, the nodes previously listed in the URT are moved to the PT, and the hop counts are appropriately modified. The sending node is entered in the URT of the receiving node at step 1224 , and the hop count for the receiving nose is set to the hop count of the sending node plus 1 at step 1225 . Finally, the node ID and hop count of the receiving node are sent to other nodes in the receiving node's neighborhood in a new T 5 trigger message at step 1226 and the process is complete. The alternative embodiments and methods discussed above in connection with FIG. 13 are applicable to the processing of FIG. 14 as well.
The processing of step 1230 (the hop count of the receiving node is one greater than the hop count of the sending node) is illustrated in the flowchart of FIG. 15 . If the sending node is listed in the URT of the receiving node at step 1231 , then processing is complete as there has been no change in the relative position of the sending and receiving nodes. If the sending node is not in the URT of the receiving node, then the DNT and PT of the receiving node are checked at step 1232 to determine if the sending node is listed in either of those tables. If so, the sending node is taken out of the corresponding table at step 1233 . Next, or if the sending node was not in any of the neighborhood tables at step 1232 , the sending node is added to the URT of the receiving node at step 1234 as the sending node has a lower hop count than the receiving node. The downstream cluster of the receiving node is computed at step 1235 . Next, a check is made at step 1236 to determine if the sending node was previously listed in the downstream neighborhood table of the receiving node. If so, a T 4 trigger message including the downstream cluster is sent to the sending node at step 1237 and processing is complete. If the sending node was not previously listed in the receiving node's downstream neighborhood table at step 1236 , the T 4 trigger message with the downstream cluster calculated at step 1235 is sent to the nodes in the receiving node's upstream routing table at step 1238 and processing is complete.
The processing of step 1250 is illustrated in the flowchart of FIG. 16 . If the sending node (whose hop count is equal to the receiving node's hop count) is already listed in the peer table of the receiving node at step 1251 , then processing is complete as there has been no change in the relative position of the sending and receiving nodes and nothing more need be done. If the sending node is not in the PT of the receiving node at step 1251 , then the DNT and URT of the receiving node are checked at step 1252 to determine if the sending node is listed in either of those tables. If so, the sending node is taken out of the corresponding table at step 1253 . Next, or if the sending node was not in the peer table at step 1252 , the sending node is added to the PT of the receiving node at step 1254 . Next, if the URT is not empty at step 1255 , processing is complete.
If the URT is empty at step 1255 (meaning that there is no upstream node and hence no way to reach the fixed gateway node), then the three neighborhood tables are re-computed at step 1256 . First, the nodes listed in the PT are moved to the URT (i.e., since no upstream node is available, packets destined for the fixed gateway node will be routed through a peer). Then, nodes listed in the downstream neighborhood table are moved to the peer table, and the downstream neighborhood table and downstream routing table are left empty. If the URT is still empty at step 1257 (i.e., there were no peers in the PT), then no path to the fixed gateway node is available and the hop count for the receiving node is set to infinity at step 1258 and processing is complete. If, however, the URT was not empty at step 1257 , the downstream cluster is calculated at step 1259 and sent to the upstream neighbors at step 1260 and processing is complete.
The T 5 trigger discussed above will generally propagate downstream because it is initiated by a new RF association with a fixed gateway node. This downstream propagation will work even when nodes are isolated (i.e., have an infinite hop count) because the comparison between an infinite hop count with a finite hop count will select the processing of step 1210 .
The processing of step 1270 (the hop count of the sending node is at least one greater than the hop count of the receiving node) is illustrated in the flowchart of FIG. 17 . If the sending node is already listed in the downstream neighbor table of the receiving node at step 1271 , then the hop count of the sending node is set equal to the hop count of the receiving node plus one at step 1272 and a new T 5 trigger message including the hop count of the receiving node is sent to the sending node at step 1273 and processing is complete. If the sending node is not in the DNT of the receiving node at step 1271 , then the PT and URT of the receiving node are checked at step 1274 to determine if the sending node is listed in either of those tables. If so, the sending node is taken out of the corresponding table at step 1275 . Next, or if the sending node was not in the peer table or URT at step 1274 , the sending node is added to the downstream neighbor table of the receiving node at step 1276 . The hop count of the sending node is set equal to the hop count of the receiving node plus one at step 1277 . Next, if the URT is not empty at step 1278 , the node identification and hop count of the receiving node are sent to the sending node at step 1273 and processing is complete. It should be noted that, in alternative embodiments, it is also possible to wait for the next periodic broadcast from neighboring nodes to update the hop counts rather than updating the hop counts at step 1256 .
If the URT is empty at step 1278 (meaning that there is no upstream node and hence no way to reach the fixed gateway node), then the three neighborhood tables are re-computed at step 1279 . First, the nodes listed in the PT are moved to the URT (i.e., since no upstream node is available, packets destined for the fixed gateway node will be routed through a peer). Then, nodes listed in the downstream neighborhood table are moved to the peer table, and the downstream neighborhood table and downstream network table are left empty. If the URT is still empty at step 1280 (i.e., there were no peers in the PT), then no path to the fixed gateway node is available and the hop count for the receiving node is set to infinity at step 1281 and step 1273 is performed. If, however, the URT was not empty at step 1280 , the downstream cluster is calculated at step 1282 and sent to the upstream neighbors in a T 4 trigger message at step 1283 . Then, the node identification and hop count of the receiving node are sent to the sending node at step 1273 and processing is complete. It should be noted that the alternatives discussed above in connection with FIG. 13 (i.e., not updating the hop counts at step 1279 and waiting until the next periodic broadcast to send the hop counts and node IDs rather than sending them at step 1273 ) are also applicable to this processing.
In addition to the triggers described above, a mechanism to remove obsolete links from the upstream routing table, peer table and downstream network table is necessary. This mechanism can take the form of periodic audits in which all of the nodes in the aforementioned tables are checked periodically. Alternatively, an activity watchdog for each neighbor node can be set up to trigger action if the neighbor node has been idle for too long.
The first mechanism involves periodically auditing the entries for the URT, PT and DNT. In the URT audit, the time since each node in the URT has been heard from is checked. If a node has been silent for more than a threshold period of time, the node is removed from the URT and the processing associated with a T 3 trigger (steps 1010 - 1070 of FIG. 10 ) is performed. If a peer node in the PT has been inactive for more than a threshold period of time, it is simply removed from the peer table. Finally, in the DRT audit, the time since each node in the DRT has been heard from is checked. If a downstream node in the DRT has been inactive for more than a threshold period of time, the processing associated with a T 1 trigger (steps 810 - 840 of FIG. 8 ) is performed.
The processing of the second mechanism, activity watchdogs, works in the same fashion described above in connection with the periodic audits whenever an activity watchdog indicates that a node has been idle for more than a threshold period of time.
Any given mobile node will be associated with a growing number of fixed gateway nodes over time as that mobile node moves around. As a practical matter, preferred embodiments maintain only a limited number of associations (e.g., 3) with fixed gateway nodes. In such embodiments, the maintained associations are referred to as principal associations. One way that this can be accomplished is by having a new association replace an old association and trigger its elimination in the neighborhood tables. If a principal association with a fixed gateway node becomes “broken” (i.e., communications with the fixed gateway node become impossible), the association becomes inactive but is still maintained (i.e., it is not dropped as in the case where a new association replaces an old one) as a peer node. It is important to continue maintaining inactive associations because they may become active again (e.g., a mobile unit makes a U-turn or goes around a curve in the road).
In the embodiments described above, a correction in a DRT is immediately propagated upward. Since URT corrections propagate downward, this will create successive waves of DRT update propagation upward as the URT corrections propagate downward. In this manner, infrastructure updates are propagated immediately, which results in fewer mishandled packets. However, this requires more CPU resources. Alternatively, the algorithms discussed herein can be modified so that any upstream propagation of DRT updates only occurs when a node that has modified its DRT has no downstream neighbors. This would delay infrastructure updates, but would be computationally more economical.
Obviously, numerous other modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the appended claims, the invention may be practiced otherwise than as specifically described herein. | A hierarchical directional internet-oriented ad-hoc network, defined by a software infrastructure, is composed of fixed gateway nodes and a plurality of wireless nodes, which may be fixed or mobile, and which may act as subscribers, routers, or both. The infrastructure hierarchy is defined by the hop count of each node (distance of that node to a fixed gateway node). The software infrastructure includes two tables associated with each node in the network: the upstream routing table which provides shortest routes to fixed gateway nodes through upstream neighbors, and the downstream routing table which provides shortest routes to subscribers through downstream neighbors. These two tables are used by routing algorithms. A peer table can also be used for alternate routes. The maintenance of the aforementioned tables is performed by autonomous algorithms operating locally on each node by receiving and processing signals from their neighbors. | 7 |
This is a division of application Ser. No. 821,604, filed Jan. 23, 1986, now U.S. Pat. No. 4,726,941.
BACKGROUND OF THE INVENTION
This invention was made in part with the assistance of grants from the Veterans Administration. The government has certain rights in this invention.
The alcohol sensitizing drugs disulfiram (tetraethylthiuram disulfide; Antabuse®) and carbimide (citrated calcium carbimide; Temposil®) increase blood acetaldehyde concentrations in the presence of ethanol by inhibiting the oxidation of acetaldehyde to acetic acid by aldehyde dehydrogenase (AlDH), thereby producing physiological effects that deter further drinking by alcoholics.
The absorption of calcium carbimide following oral administration is extremely rapid, causing nausea, headache and vomiting. In an attempt to reduce the rate of absorption, calcium carbimide is formulated as a slow release tablet, and to prevent its decomposition to ammonia, it is prepared in the citrated form (1 part drug to 2 parts citric acid). In the gastric juices, calcium carbimide is hydrolyzed to carbimide (cyanamide, H 2 NCN) which is rapidly absorbed into the portal circulation. Data from animal experiments indicate that the drug is rapidly absorbed, metabolized and eliminated, and in view of the rapid onset and short duration of the calcium carbimide-ethanol reaction (CER), it is likely that absorption, metabolism and elimination are also rapid in humans. Cyanamide itself does not inhibit AlDH, but must be enzymatically activated by catalase to an as-yet unidentified active metabolite.
Disulfiram continues to be widely used in alcoholism treatment; however, there has been concern that its repeated use may induce toxicity. The use of calcium carbimide is not approved in the United States. In Canada and other countries, calcium carbimide has not been widely used because of its short duration of activity, which lasts approximately 24 hours. This is due to its facile conversion in vivo to an acetylated derivative, viz. acetylcyanamide (AC), which is rapidly excreted in the urine. At least 94% of the administered cyanamide is eliminated within 6 hours via this route by the rat. Like cyanamide, AC is devoid of AlDH inhibitory activity in vitro.
Therefore a continuing need exists for alcohol sensitizing and deterrent drugs which can substantially elevate blood acetaldehyde levels in the presence of ethanol for a prolonged period following oral administration.
SUMMARY OF THE INVENTION
The present invention is directed to a series of cyanamide derivatives of general structure RCONHCN, which are prepared by substituting the amino nitrogen atom of cyanamide with lipophilic acyl and N-substituted-(α-aminoacyl) groups. In vivo, the enzymatic cleavage of these acyl groups (RCO) results in the gradual release of cyanamide. Thus, the preferred compounds of the present invention are superior to cyanamide or its salts with respect to (a) the elevation of blood acetaldehyde levels after ethanol administration, and/or (b) the duration of action. Therefore, the present invention is also directed to a method of deterring ethanol intake comprising raising the blood acetaldehyde level of a human following ethanol intake by administering an effective amount of one of the compounds of the present invention.
The present alcohol sensitizing composition includes compounds of the formula I: ##STR1## wherein R is C 3 -C 30 (alkyl), aryl, or cycloalkyl group; preferably a C 12 -C 22 alkyl or a C 5 -C 12 cycloalkyl group; said alkyl group comprising from 0-3 double bonds. Therefore, the RCO acyl group is preferably derived from a saturated or unsaturated fatty acid such as an alkanoic, alkenoic, dienoic or trienoic acid. Such acids include lauric, oleic, palmitic, linoleic, linolenic, stearic, eleastearic, palmitic, palmitoleic, petroselenic, vaccenic, erucic acid and the like. Other preferred R groups include propyl, butyl and branched alkyl groups such as t-butyl (from pivalic acid) or cycloalkyl groups comprising 1-4 rings, such as cyclohexyl, cyclopropylmethyl, norbornyl, cyclopentyl, adamantyl and the like. Preferred aryl groups include phenyl, benzyl, benzyloxy, tolyl and variously-substituted aryl groups including heteroaryl groups.
The R groups of the compounds of formula I may also be represented by the formula (R 2 )NHCH(R 1 ) wherein R 1 is H, benzyl, or a C 3 -C 6 alkyl group, and R 2 is benzoyl, (N-carbobenzyloxy) or (L-pyroglutamyl). Thus, the RCO moiety of the compounds of formula I can be derived from an (N-protected)-α-amino acid or from an N-[N-protected)-(α-amino)acyl]-α-amino acid. Preferably R 1 is benzyl or i-butyl. Preferred RCO groups of this type include hippuryl (C 6 H 5 CONHCH 2 CO), N-benzoyl-L-leucyl, (N-carbobenzyloxy) glycol-L-leucyl, (L-pyroglutamyl)-L-Leucyl and (L-pyroglutamyl)-L-phenylalanyl. RCO may also be the moiety N-carbobenzyloxy-L-pyroglutamyl.
Especially preferred acylated cyanamides of the present invention, due to their ability to rapidly elevate blood acetaldehyde levels to alcohol-deterrent levels and/or their ability to elevate blood acetaldehyde levels for a prolonged period, include n-butyrylcyanamide, palmitoylcyanamide (R=C 15 -n-alkyl), stearoylcyanamide (R=C 17 -n-alkyl), N-benzoyl-L-leucyl-cyanamide, hippuryl cyanamide, N-carbobenzyloxy-glycyl-L-leucylcyanamide and L-pyroglutamyl-L-phenylalanyl-cyanamide, and the pharmaceutically acceptable salts thereof.
The present invention also is directed to a method of discouraging ethanol intake and abuse by a human comprising raising the blood acetaldehyde level of a human following ethanol intake by administering an effective amount of one of the compounds of the present invention. Other compounds which can be used in this method are acetylcyanamide and propionylcyanamide. Therefore, the present invention can also include the pharmaceutically-acceptable salts of these acylated cyanamides, together with a pharmaceutically-acceptable carrier for administration in an effective non-toxic dose form. Pharmaceutically-acceptable amide salts may include metal salts, such as the alkali and alkaline earth metal salts, e.g., sodium, potassium, lithium and the like.
These physiologically acceptable salts are prepared by methods known in the art. Metal salts can be prepared by reacting a controlled amount of a metal hydroxide with the free cyanamide. Examples of metal salts which can be prepared in this way are salts containing Li, Na, K, Ca, Mg, Zn, Mn and Ba. A less soluble metal salt can be precipitated from a solution of a more soluble salt by addition of a suitable metal compound. Thus for examples, Zn, Mg and Mn salts can be prepared from the corresponding sodium salts. The metal ions of a given metal salt can be exchanged by hydrogen ions, other metal ions, ammonium ion, guanidium ion and ammonium and guanidinium ions substituted by one or more organic radicals by using a suitable cation exchanger.
BRIEF DESCRIPTION OF THE FIGURES
FIGS. 1-4 graphically depict the effectiveness of certain of the compositions of the invention in elevating blood acetaldehyde (AcH) following ethanol administration in rats.
FIG. 5 is a graphic depiction of the effectiveness of four of the compositions of the invention in elevating blood AcH following ethanol administration in rats over a 72 hour time course (0.5 mmol/kg i.p. dose).
FIG. 6 is a graphic depiction of the effectiveness of palmitoylcyanamide and N-benzoyl-L-leucylcyanamide, administered orally, in elevating blood AcH following ethanol administration in rats over a 72 hour time course.
The following abbreviations appear in the figures: CBZ=carbobenzyloxy; Gly=glycyl; and pGlu=pyroglutamyl.
DETAILED DESCRIPTION OF THE INVENTION
Acylated cyanamides of the general formula I, wherein R is a C 3 -C 30 (alkyl), aryl (e.g. phenyl) or cycloalkyl group can be readily prepared by acylation of an alkali metal cyanamide salt, such as monosodium cyanamide, with the acid chloride RCOCl. The reaction can be carried out at about -5° C. to 30° C. in an inert solvent such as tetrahydrofuran for about 10-80 hours. Following partition of the reaction mixture between water and an organic solvent such as ethyl acetate, the aqueous phase containing the sodium salt of the product is acidified with dilute mineral acid, extracted with an organic solvent such as chloroform and the solvent removed to yield the crude product. The product can be purified by crystallization and/or thin layer- or column-chromatographic techniques. Variations of this procedure are set forth in Examples hereinbelow.
In the case where the desired acid chloride is not commercially available, it can be prepared from the corresponding carboxylic acid by reaction of the acid with thionyl chloride in the presence of triethyl amine or with (COCl) 2 or PCl 3 . See, Compendium of Organic Synthetic Methods, I. T. Harrison et al., eds., Wiley-Intersciences, Pub., New York (1971) at pages 22-24, the disclosure of which is incorporated by reference herein.
Acylated cyanamides of formula I wherein R is R 2 CONHCH(R 1 )--, wherein R 1 and R 2 are defined as hereinabove or wherein RCO is (N-carbobenzyloxy-L-pyroglutamyl-) can be derived from the corresponding (N-protected)-α-(amino)acid or from the corresponding N-[(N-protected)-(α-amino)-acyl]-α-amino acid (a protected dipeptide) by conversion of the free CO 2 H mostly to the corresponding activated N-hydroxysuccinimide ester by reaction with N-hydroxysuccinimide in the presence of dicyclohexylcarbodiimide (DCC). The activated ester readily reacts with cyanamide in the presence of an alkali metal hydroxide to yield the protected, acylated cyanamide of formula R 2 CONHCH(R 1 )CONHCN following acidification. N-protected-α-amino acids can also be converted to the corresponding activated N-hydroxysuccinimide esters and reacted with a second α-amino(benzyl)ester to provide the dipeptide starting materials employed in the present invention, (R 2 CONHCH(R 1 )CO 2 H), following removal of the benzyl ester by hydrogenolysis. See L. F. Fieser et al., Reagents for Organic Synthesis, John Wiley and Sons, Inc., New York (1967) at pages 485 and 487, the disclosure of which is incorporated by reference herein.
Other activated intermediates can be employed, such as the mixed anhydride i-BuOCOCOR which is formed by reaction of the amino acid (RCO 2 H) with i-BuOCOCl in the presence of (N-methyl)morpholine. Amino protecting groups are selected from those which are base stable, such as the t-butoxycarbonyl and carbobenzyloxy groups. Pyroglutamic acid is a self-protected cyclic amide of glutamic acid.
In clinical practice, acylated cyanamides or the salts thereof will normally be administered orally in the form of a pharmaceutical unit dosage form comprising the active ingredient in combination with a pharmaceutically-acceptable carrier which may be a solid, semi-solid or liquid diluent or an ingestible capsule. A unit dosage of the compound or its salt may also be administered without a carrier material. As examples of pharmaceutical preparations may be mentioned tablets, capsules, aqueous solutions, suspensions, liposomes, and other slow-release formulations. Usually the active substance will comprise between about 0.05 and 99%, or between 0.1 and 95% by weight of the unit dosage form, for example, between about 0.1 and 50% of preparations intended for oral administration.
The amount of the acylated cyanamide administered and the frequency of administration to a given human patient will depend upon a variety of variables related to the patient's psychological profile and physical condition. For evaluations of these factors, see J. E. Peachey, A Review of the Clinical Use of Disulfiram and Calcium Carbimide in Alcoholism Treatment, J. Clinical Psychopharmacology, 1, 368 (1981), J. F. Brien et al., Europ. J. Clinn. Pharmacol., 14, 133 (1978), and Physicians' Desk Reference, Charles E. Baker, Jr., Pub., Medical Economics Co., Oradell, NJ (34th ed., 1980) at page 591-592. Generally, although the initial unit dose of the present compounds may be similar to that administered in the case of calcium cyanamide, e.g., 0.5-1.0 mg/kg, the unit dose preferably need not be readministered for 24-96 hours, versus about 8-12 hours in the case of calcium cyanamide.
The invention will be further described by reference to the following detailed examples.
I. SYNTHESIS OF ACYLATED CYANAMIDES
EXAMPLE 1. Sodium Acetylcyanamide (1)
Sodium acetylcyanamide was prepared by the acetylation of sodium cyanamide (Fluka Chemical Corp., Hauppauge, N.Y.) by the method of F. N. Shirota et al., Drug Metab. Disp., 12, 337 (1984), the disclosure of which is incorporated by reference herein.
EXAMPLE 2. Benzoylcyanamide (2)
Benzoylcyanamide was prepared by the addition of benzoyl chloride (6.33 g, 0.045 mol) in 100 ml of diethyl ether to a suspension of monosodium cyanamide (5.76 g, 0.090 mol) in 100 ml of ether at 4° C. The reaction was stirred overnight at room temperature and the pale yellow solid which formed was collected and dissolved in water. On acidification of the solution to pH 1, a precipitate formed which was collected and recrystallized from ethyl acetate (EtOAc)/petroleum ether (30°-60° C.) to give 2 (5.89 g, 89.7% yield), mp 140°-142° C. [reported mp 139°-140° C.]. Anal. Calcd for C 8 H 6 H 2 O: C, 65.75; H, 4.11; N, 19.18. Found: C, 65.79; H, 4.35; N, 19.04.
EXAMPLE 3. Pivaloylcyanamide (3)
Pivaloyl chloride (2.41 g, 2.46 ml, 0.020 mol) in 50 ml of tetrahydrofuran (THF) was added drop-wise to a suspension of sodium cyanamide (3.84 g, 0.060 mol) in 100 mol of THF at ice bath temperature with stirring. The reaction was allowed to proceed at 25° C. overnight. The reaction mixture was then extracted with ethyl acetate (2×50 ml). The aqueous layer (pH 10.5) was separated, acidified to pH 1.5 with 10% aqueous HCl, and extracted with chloroform (3×50 ml). The chloroform extract was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated in vacuo to give 2.15 g (85.2% yield) of crude product. This was crystallized from ethyl acetate and petroleum ether (b.p. range 30°-60° C.) to yield 1.4 g of white crystalline 3, mp 112°-118° C. TLC: R f =0.56 in ethyl acetate/petroleum ether/acetic acid (AcOH) (50:100:1), detected by orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3180 (NH), 2240 (C.tbd.N), 1730 (C═O); NMR (Silanor C, δ from TMS) 1.26 (s, (CH 3 ) 3 C--). Anal. Calcd for C 6 H 10 N 2 O: C, 57.12; H, 7.99; N, 22.20. Found: C, 56.98; H, 7.93; N, 22.12.
EXAMPLE 4. 1-Adamantanecarbonyl Cyanamide (1-Adamantoylcyanamide) (4)
1-Adamantanecarbonyl chloride (1.99 g, 0.010 mol) in 50 ml of THF was added drop-wise to a suspension of sodium cyanamide (1.92 g, 0.030 mol) in 100 ml of THF with stirring at ice bath temperature. The reaction was allowed to proceed at 25° C. for 15 hours. The reaction mixture was then extracted with ethyl acetate (100 ml). The separated aqueous portion (pH 10.5) was acidified to pH 1.5 with 10% HCl and extracted with ethyl acetate (3×60 ml). The ethyl acetate extract was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated in vacuo to dryness. The resulting white solid residue was triturated in a minimal amount of distilled water, filtered, and air-dried to give 1.74 g (85.2% yield) of crude 4 as white solid. This was recrystallized from ethyl acetate and petroleum ether to give 0.55 g (crop 1) of white crystalline powder. The filtrate was concentrated when further crystallization occurred to give 0.49 g (crop 2) of additional product giving a total yield of 50.9%, mp 168°-170° C. TLC: R.sub. f =0.58 in EtOAc/petroleum ether/AcOH (50:100:1), detected by UV quenching (weak) and reddish orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ), 3210 (NH), 2230 (C.tbd.N), 1710 (C═O); NMR (Silanor C, δ from TMS) 1.62-2.2 (m, aliphatic CH's). Anal. Calcd for C 12 H 16 N 2 O: C, 70.56; H, 7.90; N, 13.71. Found: C, 70.59; H, 8.04; N, 13.66.
EXAMPLE 5. n-Butyrylcyanamide (5)
n-Butyryl chloride (3.2 g, 3.12 ml, 0.030 mol) in 50 ml of freshly distilled dry THF was added drop-wise to a suspension of sodium cyanamide (5.76 g, 0.090 mol) in 100 ml of freshly distilled dry THF at ice bath temperature. The reaction was allowed to proceed at room temperature for 24 hours and then the mixture evaporated to dryness in vacuo. The resulting yellow solid residue was dissolved in distilled water (50 ml) and the alkaline soluton was adjusted to pH 6.5 with 10% HCl. The mixture was then extracted with ethyl acetate (2×50 ml). The aqueous portion (pH 7.8 was acidified to pH 1.5 with 10% HCl and extracted with methylene chloride (3×30 ml). The organic layer was separated, dried over anhydrous sodium sulfate and evaporated in vacuo to give 3.33 g (99.0% yield) of the crude product as a pale yellow liquid. A portion of the crude 5 (2.00 g, 0.0178 mol) was applied to a dry silica gel column (22×2.5 cm, 230-400 mesh, EM reagent) in EtOAc/petroleum ether (1:3) and eluted with the same solvent by flash chromatography at 15 psi. A total of 32×20 ml fractions were collected. The fractions containing the desired compound were pooled and evaporated in vacuo to give 1.77 g (total yield, 87.6%) of pure 5 as a clear colorless liquid. This compound decomposes on standing even at 5° C. after prolonged periods. TLC: R f =0.6 in EtOAc/petroleum ether/AcOH (50:100:1), detected by UV quenching and orange color with ferricyanide spray reagent; IR (neat, cm -1 ) 3100-3250 (NH), 2860-2960 (alkyl), 2260 (C.tbd.N), 1725 (C═O); NMR (Silanor C, δ from TMS) 8.2-8.5 (broad, NH), 2.3-2.6 (t, --CH 2 --CH 2 --C═O), 1.5-1.9 (sextet, CH 3 --CH 2 --CH 2 --), 0.8-1.1 (t, CH 3 --CH 2 --); CI-MS (NH 3 : positive) m/z (rel. intensity) 147 (12.6, [(M+1)+2NH 3 ]), 130 (100.0) [(M+1)+NH 3 ], 105 (5.2) [(M+1)+2NH 3 --H 2 NCN]; CI-MS (NH 3 : negative) m/z (rel. intensity) 111 (100.0) [M-1], 68 (2.0) [(M-1)--CH 3 CH 2 CH 2 ], 41 (16.7) [(M-1)--CH 3 CH 2 CH═C═O].
EXAMPLE 6. Palmitoylcyanamide (6)
A solution of palmitoyl chloride (5.5 g, 0.020 mol) in 50 mol of freshly distilled dry THF was added drop-wise to a suspension of sodium cyanamide (3.84 g. 0.060 mol) in 150 ml of freshly distilled by THF at ice bath temperature. After the addition, the ice bath was removed and the reaction was allowed to proceed at 25° C. for 43 hours. The solids that formed was filtered to yield 8.48 g of waxy solid residue. The residue was ground to a fine powder and stirred in 150 ml of distilled water at ice bath temperature. The resulting soapy suspension (pH 11) was acidified to pH 2 with 10% HCl, then filtered and air-dried to give 5.4 g (96.3% yield) of crude 6 as a white solid. This was dissolved in warm THF and the mixture filtered. The filtrate was concentrated in vacuo until the solution became slightly turbid. This material was crystallized from THF/petroleum ether to yield 3.6 g (crop 1) of white powder. The filtrate was concentrated and crystallized in the same fashion to yield additional 0.6 g (crop 2) of white powder (74.8% total yield), mp 62°-65° C. TLC: R f =0.68 in ethyl acetate/petroleum ether/glacial acetic acid (10:20:1); IR (Nujol, cm -1 ) 3230 (NH), 2250 (C.tbd.N), 1740 (C═O); NMR (Silanor C, δ from TMS (1.3-1.6 (t, --CH 2 --CH 2 --C═O), 1-1.8 L (m, --(CH 2 ) 13 --), 0.8-1 (t, CH 3 --CH 2 --); Anal. Calcd for C 17 H 32 N 2 O: C, 72.81; H, 11.50; N, 9.99. Found: C, 72.69; H, 11.65; N, 9.68.
EXAMPLE 7. Stearoylcyanamide (7)
Stearoyl chloride (3.03 g, 0.010 mol) in 50 ml of freshly distilled dry THF was added drop-wise to a suspension of sodium cyanamide (1.92 g, 0.030 mol) in 100 ml of freshly distilled dry THF with vigorous stirring. The reaction was allowed to proceed at 25° C. for 63 hours. The solids which formed were collected by filtration and the solid cake was suspended in 200 ml of distilled water. The resulting soapy suspension (pH 10.5) was acidified to pH 1.5 with 10% HCl, filtered, and air-dried to give 2.85 g (92.4% yield) of crude 7. This was dissolved in THF and the solution decolorized with activated charcoal. The filtrate was concentrated until the solution became turbid. Addition of petroleum ether gave 2.29 g (crop 1) of white waxy 7. The filtrate was concentrated and petroleum ether added to give 0.28 g (crop 2) of additional product giving a total yield of 83.3%, mp 74°- 75° C. TLC: R f =0.69 in EtOAc/petroleum ether/AcOH (50:100:1), detected by UV quenching (weak) and no color reaction with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3210 (NH), 2250 (C.tbd.N), 1735 (C═O); NMR (Silanor C, δ from TMS) 2.3-2.6 (t, --CH 2 --CH 2 --C═O), 1.0-1.8 (fused s, (CH 2 ) 14 ), 0.8-0.9 (t, CH 3 --CH 2 --); Anal. Calcd for C 19 H 36 N 2 O: C, 73.97; H, 11.76; N, 9.08. Found: C, 73.88; H, 11.50; N, 9.09.
EXAMPLE 8. N-Carbobenzoxycyanamide, Sodium Salt (8)
To a stirred solution of cyanamide (6.3 g, 0.15 mol) in 60 ml of distilled water, were added carbobenzoxy chloride (8.5 g, 0.050 mol) and 10% NaOH (40 ml, 0.10 mol) drop-wise via separate funnels at ice batch temperature. The reaction was allowed to proceed at this temperature for 3 hours. The reaction mixture (pH 10.1) was extracted with ethyl acetate (2×50 ml) and diethyl ether (2×50 ml), then the aqueous layer was acidified with 10% HCl to pH 1.5 and extraction with diethyl ether (4×50 ml). The ether extract was dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated in vacuo to give a pale pink clear liquid. The liquid was dissolved in 50 ml of methanol at ice bath temperature. The methanolic solution (pH 1.8) was titrated with 5% methanolic NaOH to pH 5.9, the solution filtered, and the filtrate was evaporated in vacuo to near dryness to give a pale yellow liquid. Diethyl ether (100 ml) was added to the liquid with occasional shaking. After some scratching with a glass rod, a white solid cake formed. The collected white solid was washed with diethyl ether to give 5.17 g (52.2% yield) of pure 8 as a white powder, mp 216°-217° C. TLC: R f =0.56 in CH 2 Cl 2 /CH 3 OH (5:1); detected by UV quenching and orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3100-3040 (C 6 H 5 ), 2150 (--N═C═N--Na), 1640 (--O 2 C--N); NMR (Silanor D 2 O/DSS, δ from DSS), 7.38 (s, C 6 H 5 ), 5.03 (s, C 6 H 5 --CH 2 --O--). Anal. Calcd for C 9 H 6 N 2 O 2 .Na: C, 54.55; H, 3.56; N, 14.14. Found: C, 54.57; H, 3.79; N, 14.26.
EXAMPLE 9. N-Carbobenzoxyglycine N-Hydroxysuccinimide Ester
Acetonitrile (100 ml) was added to a reaction vessel containing N-carbobenzoxyglycine (4.18 g, 0.020 mol), dicyclohexyl carbodiimide (4.13 g, 0.020 mol), and N-hydroxysuccinimide (2.3 g, 0.020 mol) were stirred in 100 ml of acetonitrile at ice bath temperature for 5 hours. The reaction mixture was filtered to remove 4.12 g of white crystalline dicyclohexyl urea (DCU) as by-product. The filtrate was evaporated in vacuo to give a semi-solid residue which was recrystallized from chloroform/petroleum ether (bp range: 60°-70° C.) to give 4.99 g (81.5% yield) of white, crystalline N-carbobenzoxyglycine N-hydroxysuccinimide ester, mp 111° C. IR (Nujol, cm -1 ) 3300 (NH), 3020 and 3060 (C 6 H 5 ), 1820, 1780, 1740, and 1690 (C═O). Anal. Calcd for C 14 H 14 N 2 O 6 : C, 54.90; H, 4.61; N, 9.15. Found: C, 54.15; H, 4.63; N, 8.75.
EXAMPLE 10. N-Carbobenzoxyglycylcyanamide (9)
A solution of N-carbobenzoxyglycine N-hydroxysuccinimide ester (1.53 g, 5.0 mol) in 50 ml of THF and 10% NaOH (4 ml, 0.4 g, 0.010 mol) were added drop-wise, simultaneously via separate channels, to a reaction vessel containing cyanamide (0.63 g, 0.015 mol) in 100 ml of distilled water, with stirring at ice bath temperature. The reaction was allowed to proceed overnight at room temperature. The raction mixture (pH 9.5) was extracted with ethyl acetate (2×50 ml). The ether was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated in vacuo to give 1.0 g (86% yield) of crude product as a white solid residue. It was recrystallized from THF/petroleum ether (bp range: 60°-70° C.) to give 0.50 g (43% yield) of white, crystalline 9, mp 198° C. dec. IR (Nujol, cm -1 ) 3300, 3100 (NH), 2250 (C N), 1725 and 1680 (C═O). Anal. Calcd for C 11 H 11 N 3 O 3 : C, 56.65; H, 4.75; N, 18.02. Found: C, 56.77; H, 4.53; N, 17.95.
EXAMPLE 11. N-Benzoylglycylcyanamide (Hippurylcyanamide) (10)
Hippuric acid (3.58 g, 0.020 mol), DCC (4.13 g, 0.020 mol), and N-hydroxysuccinimide (2.3 g, 0.020 mol) were stirred in 100 ml of acetonitrile at ice bath temperature for 2 hours. The reaction mixture was filtered to remove the bulk of by-product DCU. The filtrate was evaporated in vacuo to dryness, the residue was redissolved in THF and the mixture was filtered to remove any residual DCU. The filtrate (70 ml) was added drop-wise to a solution of sodium cyanamide (3.84 g, 0.060 mol) in 100 ml of distilled water with vigorous stirring at ice bath temperature. The reaction was allowed to proceed at room temperature overnight. The reaction mixture (pH 11) was extracted with ethyl acetate (2×60 ml) and the separated aqueous layer was acidified to pH 1.5 with 10% HCl. The resulting solid suspension was filtered to give 2.28 g (56.1% yield) of white crystalline 10. It was recrystallized from THF/acetonitrile/petroleum ether to yield 0.78 g (crop 1) of white crystalline product. The filtrate was concentrated to yield 0.9 g (crop 2) of additional crystals. Mp dec. >155° C. (turns to brown oil at 160° C.); TLC: R f =0.36 in EtOAc/AcOH (100:1), detected by UV quenching and orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3400 (NH), 3080 (C 6 H 5 ), 2220 (C.tbd.N), 1710 and 1620 (C═O); NMR (Silanor C and DMSO (1:1), δ from TMS) 8.2-8.4 (broad, NH); 7.3-8.0 (m, C 6 H 5 --), 4.1-4.2 (d, --NH--CH 2 --CO). Anal. Calcd for C 10 H 9 N 3 O 2 : C, 59.11; H, 4.46; N, 20.68. Found: C, 59.26; H, 4.46; N, 20.84 (crop 1) and C, 59.03; H, 4.20; N, 20.80 (crop 2).
EXAMPLE 12. N-Benzoyl-L-leucine
Benzoyl chloride (4.22 g, 0.030 mol) and 10% NaOH (12 ml, 0.030 mol) were added separately with vigorous stirring to a solution of L-leucine (3.94 g, 0.030 mol) in 150 ml of distilled water at ice bath temperature. The reaction was allowed to proceed at this temperature until the reaction mixture became clear (30 minutes); it was then extracted with ethyl acetate (2×100 ml). The aqueous layer was separated, acidified to pH 2 with 10% HCl, and extracted with ethyl acetate (3×50 ml). The ethyl acetate extract was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated in vacuo to yield quantitative amount of N-benzoyl-L-leucine as a semi-solid which was used directly for the following step.
EXAMPLE 13. N-Benzoyl-L-leucylcyanamide (11)
DCC (2.41 g, 0.0117 mol) and N-hydroxysuccinimide (1.35 g, 0.0117 mol) were added to a solution of N-benzoyl-L-leucine (2.75 g, 0.0117 mol) in 100 ml of acetonitrile at ice bath temperature. The raction was allowed to proceed at this temperature for 2 hours. The reaction mixture was filtered to remove the bulk of the DCU and the filtrate was evaporated in vacuo to dryness. The resulting semi-solid residue was redissolved in THF and the mixture filtered to remove any residual DCU. The filtrate was evaporated in vacuo to give crude N-benzoyl-L-leucine N-hydroxysuccinimide ester as a foamy residue. IR (neat, cm -1 ) 3340 (NH), 3060 (C 6 H 5 ), 1820, 1790, 1740 and 1650 (C═O); NMR (Silanor C, δ from TMS) 7.3-7.9 (m, C 6 H 5 ), 5.1-5.3 (m, --NH--CH--C═O), 2.8 (s, cycl. --CH 2 --CH 2 --), 1.6-2.2 (m, CH--CH 2 --), 0.9-1.1 (d, (CH 3 ) 3 CH). This was dissolved in 100 ml of THF and added drop-wise to a solution of sodium cyanamide (1.50 g, 0.0234 mol) in 100 ml of distilled water at ice bath temperature. The reaction was allowed to proceed at room temperature for 24 hours. The reaction mixture was then concentrated in vacuo to half its original volume and filtered. The filtrate (pH 9) was extracted with ethyl acetate (2×50 ml). The aqueous layer was separated, acidified to pH 1.5 with 10% HCl, and extracted with methylene chloride (3×50 ml). The methylene chloride extract was dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated in vacuo to give 2.80 g (92.4% yield) of crude product as a tacky white solid. This was triturated with diethyl ether and collected to give 1.30 g (42.9% yield of white powdery 11, mp 136°-137° C. [α] D 23 +0.7° (c 1.0, CH 3 OH); TLC: R f =0.93 in EtOAc/petroleum ether/THF/CH 2 Cl 2 /AcOH (50:50:10:50:4) and 0.24 in EtOAc/petroleum ether/AcOH (50:100:1), detected by UV quenching and orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3300, 3100 (NH), 2230 (C.tbd.N), 1750 and 1630 (C═O); NMR (Silanor-DMSO, δ from TMS) 7.4-8.0 (d, C 6 H 5 --), 4.2-4.6 (m, --NH--CH--C═O), 1.4-1.9 (m, CH--CH 2 --), 0.8-1.1 (d, (CH 3 ) 2 CH--). Anal. Calcd for C 14 H.sub. 17 N 3 O 2 : C, 64.85; H, 6.61; N, 16.20. Found C, 64.62; H, 6.73; N, 15.93.
EXAMPLE 14. N-Cbz-glycyl-L-leucylcyanamide (12)
N-Cbz-glycyl-L-leucine (4.84 g, 0.015 mol) was allowed to react with DCC (3.09 g, 0.015 mol) and N-hydroxysuccinimide (1.73 g, 0.015 mol) in 50 ml of THF at ice bath temperature for 2.5 hours. The reaction mixture was filtered and the light brown filtrate (50 ml) was added to a solution of sodium cyanamide (2.88 g, 0.045 mol) in 30 ml of distilled water with stirring at ice bath temperature. The reaction was allowed to proceed at room temperature for 24 hours. The reaction mixture was concentrated in vacuo to half its original volume and filtered. The filtrate (pH 9) was acidified to pH 2.5 with 10% HCl and extrated with methylene chloride (4×50 ml). The combined methylene chloride extract was dired over anhydrous sodium sulfate, filtered, and the filtrate was evaporated in vacuo to give 4.86 g (93.5% yield) of crude 10 as a thick semi-solid residue. The residue was dissolved in methylene chloride and the solution washed with 5% citric acid. The organic layer was separated, dried over anhydrous sodium sulfate, and decolorized with activated charcoal. After removal of the charcoal by filtration, the filtrate was evaporated in vacuo to give 4.10 g (78.9% yield) of white glassy 10, mp 50°-55° C. [α] D 23 -34.0° (c 1.0, MeOH); TLC: R f =0.54 in CH 2 Cl 2 /MeOH/AcOH (90:10:5), detected by UV quenching and orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3300 (NH), 3060 (C 6 H 5 ), 2260 (C.tbd.N), 1650-1730 (C═O); NMR (Silanor C, δ from TMS) 7.35 (s, C 6 H--), 5.7-6.1 (NH), 5.1 (s, --O--CH 2 ), 4.3-4.7 (m, --NH--CH--CO), 3.8-4.0 (fused s, --NH--CH 2 --CO), 1.4-1.8 (m, --CH 2 --CH═), 0.8-1.0 (fused d, (CH 3 )CH--). Anal. Calcd for C 17 H 22 N 4 O 4 : C, 58.95; H, 6.40; N, 16.17. Found: C, 58.90; H, 6.55; N, 15.93.
EXAMPLE 15. N-Cbz-L-pyroglutamic Acid N-Hydroxysuccinimide Ester
DCC (2.27 g, 0.011 mol) was added to a solution of Cbz-L-pyroglutamic acid (2.63 g, 0.010 mol) and N-hydroxysuccinimide (1.15 g, 0.010 mol) in 50 mol of THF at 0° C., and the mixture was stirred at room temperature for 15 hours. The reaction mixture was filtered and the filtrate was evaporated to give 3.50 g (97.1% yield) of crude product as a thick liquid which flocculated on addition of petroleum ether. The precipitate was crystallized from isopropyl alcohol to give 2.15 g (crop 1) of white crystals. The filtrate was concentrated and crystallized in the same manner to give 0.71 g (crop 2) giving a total yield of 79.4%. Mp 132°-134° C. [reported mp 131°-133° C.]; TLC: R f =0.77 in EtOAc/AcOH (100:1), detected by UV quenching; IR (Nujol, cm -1 ) 3050 (C 6 H 5 ), 1820, 1785 and 1735 (C═O); NMR (Silanor C, δ from TMS) 7.3-7.6 (m, C 6 H 5 --), 5.3-5.4 (d, --O--CH 2 --), 4.9-5.1 (t, O═C--CH--N), 2.9 (s, O═C--CH 2 --CH 2 --C═O), 2.3-2.8 (m, O═C--CH 2 --CH 2 CH--).
EXAMPLE 16. N-Cbz-L-pyroglutamylcyanamide (13)
Cbz-L-pyroglutamic acid N-hydroxysuccinimide ester (1.8 g, 5.0 mmol) in 40 ml of THF was added drop-wise to a solution of sodium cyanamide (0.96 g, 0.015 mol) in 30 ml of distilled water at ice bath temperature. The reaction was allowed to proceed at this temperature for 4 hours and the reaction mixture was then extracted with ethyl acetate (2×50 ml). The aqueous layer (pH 11) was separated and acidified to pH 2 with 2N HCl. The resulting white precipitate was filtered and dried to give 0.66 g (45.9% yield) of 13 as a white powder, mp 185°-186° C. (turned slightly yellow>170° C.). [α] D 23 -31.56° (c 1.0, CH 3 CN); TLC: R f =0.5 in CH 2 Cl 2 /MeOH/AcOH (80:20:5), detected by UV quenching and gradual development of yellow color with ferricyanide spray reagent; IR (Nujol, cm -1 ), 3160 (NH), 3050 (C 6 H 5 ), 2240 (C.tbd.N), 1775 and 1725 (C═O); NMR (acetone-d 6 , δ from TMS) 7.4 (s, C 6 H 5 ), 5.3 (s, --CH 2 --O--), 4.8-5.0 (m, O═C--CH--N), 2.2-3.0 (m, O═C--CH 2 --CH 2 --CH). Anal. Calcd for C 14 H 13 N 3 O 4 : C, 58.53; H, 4.56; N, 14.63. Found: C, 58.33; H, 4.73; N, 14.63.
EXAMPLE 17. L-Pyroglutamic Acid N-Hydroxysuccinimide Ester
DCC (4.13 g, 0.020 mol) and N-hydroxysuccinimide (2.3 g, 0.020 mol) were added to a solution of L-pyroglutamic acid (2.58 g, 0.020 mol) in 50 ml of THF and 5 ml of dimethyl formamide (DMF) at ice bath temperature. The reaction was allowed to proceed at room temperature for 48 hours. The reaction mixture was then filtered to remove the bulk of the DCU and the filtrate was evaportaed in vacuo to dryness. The resulting white solid residue was dissolved in 40 ml of THF, the solution filtered, and the filtrate was evaporated in vacuo to give 5.61 g of semi-solid residue. This was crystallized from hot methylene chloride to give 2.35 g (crop 1) of white cyrstalline L-pyroglutamic acid N-hydroxysuccinimide ester. Additional product, 1.11 g (crop 2), was obtained from the filtrate giving a total yield of 76.5%. mp crop 1; 136°-137° C., crop 2; 134°-135° C.; TLC: R f =0.4 in EtOAc/AcOH (100:1), detected by brown color development with N-chloro spray reagent.
EXAMPLE 18. L-Pyroglutamyl-L-leucine Benzyl Ester
L-Pyroglutamic acid N-hydroxysuccinimide ester (4.52 g, 0.020 mol) was added to a solution of L-leucine benzyl ester (4.43 g, 0.020 mol) in 60 ml of THF at room temperature and the reaction was allowed to proceed for 15 hours. The reaction mixture was evaporated in vacuo to give a pale yellow liquid. This liquid was dissolved in methylene chloride (50 ml) and washed with 10% citric acid (50 ml) followed by 5% sodium bicarbonate (50 ml). The methylene chloride layer was dried over anhydrous sodium sulfate and evaporated in vacuo to give 6.37 g (95.8% yield) of crude product as a pale yellow, thick, liquid. Crystallization from hot methylene chloride and petroleum ether gave 5.42 g (81.53% yield) of white crystalline compound, mp 127°-128° C. TLC: R f =0.58 in EtOAc/AcOH (100:1), detected by UV quenching; NMR (Silanor C, δ from TMS) 7.34 (s, C 6 H 5 ), 5.4 (s, --O--CH 2 --C 6 H 5 --), 4.5-4.9 (m, --NH--CH--C═O), 3.9-4.3 (m, --NH--CH--C═O), 2.0-2.7 (m, cycl. --NH--CH 2 --CH 2 --CH), 1.4-1.8 (m, --CH 2 --CH), 0.7-1.1 (fused d, --CH(CH 3 ) 3 ). Anal. Calcd for C 18 H 24 N 2 O 4 : C, 65.04; H, 7.28; N, 8.43. Found: C, 65.23; H, 7.51; N, 8.36.
EXAMPLE 19. L-Pyroglutamyl-L-leucine
L-Pyroglutamyl-L-leucine benzyl ester (6.65 g, 0.020 mol) was hydrogenated with 9% palladium on charcoal in 100 ml of methanol for 1 hour. The hydrogenation mixture was filtered through Celite and the filtrate was evaporated in vacuo to give 4.78 g of product as a white solid. This was crystallized from methanol and diethyl ether to give 4.63 g (95.6% yield) of white crystals, mp 152°-154° C. [reported mp 151°-152° C.]; [α] D 23 ° C. -19.35° (c 1.0, MeOH); TLC: R f =0.57 in CHCl 3 /MeOH/AcOH (80:20:5), detected by brown color development with N-chloro spray reagent; NMR (methanol-d 4 , δ from TMS) 4.3-4.6 (m, --NH--CH--C═O), 4.1-4.3 (q, --NH--CH--C═O), 1.9-2.6 (m, cycl. O═C--CH 2 --CH 2 --CH), 1.5-1.8 (m, --CH 2 --CH), 0.7-1.1 (m, --CH(CH 3 ) 3 ). Anal. Calcd for C 11 H 18 N 3 O 4 : C, 54.53; H, 7.49; N, 11.56. Found: C, 54.55; H, 7.39; N, 11.58.
EXAMPLE 20. L-Pyroglutamyl-L-leucylcyanamide (14)
L-Pyroglutamyl-L-leucine (1.21 g, 5.0 mmol) was stirred with DCC (1.03 g, 5.0 mmol) and N-hydroxysuccinimide (0.58 g, 5.0 mmol) in 150 ml of THF, initially at ice bath temperature, then at room temperature overnight. The reaction mixture was filtered and the solvent was removed in vacuo to dryness. The residue was redissolved in THF and filtered. The filtrate (70 ml) was added drop-wise to a solution of sodium cyanamide (0.64 g, 0.010 mol) in 70 ml of distilled water at ice bath temperature. The reaction was allowed to proceed at this temperature for 4 hours. The reaction mixture was concentrated in vacuo to half its original volume at 25° C. and filtered. The filtrate (pH 7.5) was neutralized to pH 7 with 10% HCl and applied to an AG 1×2 anion exchange resin column (15×2 cm, 100-200 mesh, acetate form) packed with distilled water. The column was washed with water (380 ml) until no more cyanamide was detected by spotting on TLC plates (purple color with ferricyanide spray reagent), then eluted with a linear pH gradient consisting of equal volume of 0.15N HCl in the reservoir and water in the mixing flask (1000 ml:1000 ml). A total of 45×20 ml fractions were collected. The fractions containing the desired product (orange color when spotted on TLC plates and sprayed with ferricyanide reagent) were pooled and extracted with EtOAc/THF (5:1)(2×30 ml) and EtOAc (4×30 ml). The organic extract was dried over anhydrous sodium sulfate and evaporated in vacuo to dryness. The resulting solids were collected to give 1.29 g (96.9% yield) of crude product as white powder. A portion of the product (140 mg) was dissolved in methanol and applied on 4 preparative TLC plates (Preadsorbent, Analtech, 1000 u thickness) then eluted with CHCl 3 /MeOH/AcOH (80:20:5). The bands which corresponded to the desired product were removed, extracted with ETOAc/absolute EtOH (2:1), and the extract was then filtered. The filtrate was evaporated in vacuo to dryness, the residue triturated with diethyl ether, and the product collected and dried in vacuo to give 79 mg (54.7% total yield) of off-white powder, mp dec.>175° C. (gradually turns yellow, then to a dark brown residue at 205° C.). [α] D 23 -29.93° (c 1.0, MeOH); TLC: R f =0.36 in CHCl 3 /MeOH/AcOH (80:20:5) detected by UV quenching (weak), orange color with ferricyanide spray reagent, and brown color with N-Cl spray reagent; IR (Nujol, cm -1 ) 3300 (NH), 2170 (C.tbd.N), 1670-1690 (C═O); NMR (methanol-d 4 , δ from TMS) 4.1-4.6 (m, --NH--CH--C═O), 2.1-2.6 (m, cycl. --CH 2 --CH 2 --), 1.4-1.8 (m, --CH 2 --CH), 0.8-1.1 (m, --CH(CH 3 ) 2 ).
EXAMPLE 21. L-Pyroglutamyl-L-phenylalanine Methyl Ester
N-Methylmorpholine (2.02 g, 0.020 mol) and isobutyl chloroformate (2.73 g, 0.020 mol) were added to a solution of L-pyroglutamic acid (2.58 g, 0.020 mol) in 100 ml of THF/DMF (6:1) at -15° C. After a 2 minute coupling period, a mixture of L-phenylalanine methyl ester hydrochloride (4.31 g, 0.020 mol) (suspension) and N-methyl morpholine (2.02 g, 0.020 mol) in 50 ml of DMF was added to the reaction mixture. The reaction was allowed to proceed at this temperature for 30 minutes and then at room temperature for 1 additional hour. The reaction mixture was then filtered to remove fines and the filtrate was evaporated in vacuo to incipient dryness. The resulting yellow liquid was dissolved in 100 ml of ethyl acetate, and the ethyl acetate solution was washed with 5% citric acid saturated with sodium chloride (50 ml) and 5% sodium bicarbonate saturated with NaCl (50 ml). The separated organic layer was dried over anhydrous sodium sulfate and evaporated in vacuo to yield quantitative amounts of a pale yellow liquid which was used directly for the following step. TLC: R f =0.22 in EtOAc/AcOH (100:1), detected by UV quenching; IR (neat, cm -1 ) 3300 (NH), 3020-3060 (C 6 H 5 ), 2860-2960 (alkyl), 1650-1750 (C═O); NMR (Silanor C, δ from TMS) 7.25 (fused s, C 6 H 5 --), 5.5-5.7 and 6.6-6.8 (broad, NH's), 4.6-5.1 (q, --NH--CH--C═O), 3.0-3.2 (q, --CH 2 --C 6 H 5 ), 1.6-2.5 (m, cycl. O═C--CH 2 --CH 2 ).
EXAMPLE 22. L-Pyroglutamyl-L-phenylalanine
L-Pyroglutamyl-L-phenylalanine methyl ester (1.27 g, 4.4 mmol) in 50 ml of methanol was stirred with 10% NaOH (1.93 ml, 0.193 g of NaOH, 4.8 mmol) at room temperature for 1 hour. The reaction mixture was evaporated in vacuo to dryness, the residue then dissolved in distilled water and the mixture extracted with ethyl acetate (100 ml). The aqueous layer (pH 10.5) was separated, acidified to pH 2 with 10% HCl, then saturated with sodium chloride and extracted with ethyl acetate (6×50 ml). The pooled ethyl acetate extract was dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated in vacuo to give a white foamy solid residue. This was triturated with anhydrous diethyl ether, collected, and dried in vacuo to give 1.04 g (86.04% yield) of white powder which was used directly for the following step. Mp 128°-130° C.; [α] D 23 +13.51 (c 1.0, MeOH); TLC: R f =0.66 in CHCl 3 /MeOH/AcOH (80:20:5), detected by UV quenching and brown color with N-Cl spray reagent; NMR (methanol-d 4 , δ from TMS) 7.22 (s, C 6 H 5 --), 4.6-4.8 (m, --NH--CH--C═O), 4.0-4.2 (q, --NH--CH--C═O), 2.8-3.2 (m, --CH 2 --C 6 H 5 ), 1.7-2.5 (m, cycl. O═C--CH 2 --CH 2 --CH--).
EXAMPLE 23. L-Pyroglutamyl-L-phenylalanylcyanamide (15)
L-Pyroglutamyl-L-phenylalanine (4.10 g, 0.0148 mol) was allowed to react with DCC (3.37 g, 0.0163 mol) and N-hydroxysuccinimide (1.88 g, 0.0163 mol) in 60 ml of THF at ice bath temperature for 3 hours, and then at room temperature overnight. The reaction mixture was filtered and the filtrate was added drop-wise to a solution of sodium cyanamide (1.90 g, 0.0297 mol) in 60 ml of distilled water at ice bath temperature. The reaction was allowed to proceed at this temperature for 6 hours. The reaction mixture (pH 8) was then neutralized to pH 7 with 10% HCl, saturated with sodium chloride, and extracted with ethyl acetate (2×50 ml). The aqueous portion (pH 6.2) was acidified to pH 1.5 with 10% HCl and extracted with EtOAc/THF (3:1) (100 ml) and ethyl acetate (2×50 ml). The combined organic extract was dried over anhydrous sodium sulfate and evaporated in vacuo to give 4.20 g (94.5% yield) of crude product as an off-white solid residue. This was crystallized from abs. EtOH/diethyl ether to give 1.36 g (crop 1) of 15. The filtrate was concentrated and crystallized in the same manner to give 9.53 g (crop 2), giving a total yield of 42.5%. Mp 163°-165° C.; [α] D 23 +7.81° (c 1.0, MeOH); TLC: R f =0.29 in CHCl 3 /MeOH/AcOH (80:20:5), detected by UV quenching and orange color with ferricyanide spray reagent; IR (Nujol, cm -1 ) 3350 (NH), 3020 (C 6 H 5 ), 2160 (C.tbd.N), 1650-1690 (C═O); NMR (methanol-d 4 , δ from TMS) 7.22 (s, --C 6 H 5 ), 4.5-4.7 (q, --NH--CH--C═O), 4.0-4.2 (m, --NH--CH--C═O), 2.8-3.2 (m, --CH 2 --C 6 H 5 ), 1.7-2.6 (m, cycl. O═C--CH 2 --CH 2 --). Anal. Calcd for C 15 H 16 N 4 O 3 : C, 59.99; H, 5.37; N, 18.66. Found: C, 59.61; H, 5.61; N, 18.40.
II. Evaluation of Acylated Cyanamides In Vivo
Compounds 1-11 were evaluated in rats for their ability to elevate and maintain blood acetaldehyde (AcH) levels following ethanol administration employing the methodology outlined in Table I.
TABLE I______________________________________A. Initial Screen Protocol1. Drug Dose: 1.0 mmol/kg (ip)2. Animals: Male rats of Sprague-Dawley descent (BioLab, Inc., St. Paul, MN), weighing 185-225 g were used. Four animals were used for each drug administration protocol.3. Timing: Animals were fasted beginning at 7:00 or 8:00 AM. One group of rats were admi- nistered the prodrug at 5:00 PM (zero time) and ethanol (2 g/kg, ip) at 8:00 AM (15 hours), and the animals were sacrificed at 9:00 AM (16 hours). A second set of rats received the prodrug at 6:30 AM (zero time) and ethanol at 8:30 AM (2 hours) and the animals were sacrificed at 9:30 AM (3 hours). Cyanamide treated animals (1.0 mmol/kg) served as positive control. Blood AcH levels were determined as described hereinbelow.B. Time Course Protocol1. Drug Dose: 0.5 mmol/kg (ip); 1.0 mmol/kg (po)2. Animals: Male rats of Sprague-Dawley descent (BioLab, Inc., St. Paul, MN), weighing 176-200 g were used. Two animals were used for each drug administration protocol.3. Timing: Overnight fasted animals were administered the prodrug at zero time, ethanol (2 /kg, ip) at 1, 4, 11, 23, 35, 47 and 71 hours and sacrificed 1 hour subsequent to each ethanol administration. Cyanamide treated animals (1.0 mmol/kg) served as positive control.______________________________________
Blood AcH levels were measured 1 hour after ethanol (2 g/kg, ip) in treated and control animals essentially as described by Shirota et al., in J. Med Chem., 23, 669 (1980). The animal was stunned by a quick blow to the head and blood was immediately withdrawn by open chest cardiac puncture. Aliquots (0.2 ml) were placed in 20 ml serum vials containing 1.0 ml of 5 mM sodium azide (to minimize the artifactual generation of AcH from ethanol), and the vials immediately capped with a rubber septum, frozen on Dry Ice, and kept frozen at -20° C. until assayed. AcH was determined in duplicate by the head-space gas chromatographic procedure previously described by Nagasawa et al., in Life Sci., 20, 187 (1977), and quantitated using a standard curve based on standards with known concentrations of AcH. The results of this study are summarized in FIGS. 1-4.
Cyanamide, a known potent AlDH inhibitor and positive control, elevated blood AcH 150-fold over drug-free controls at 3 hours, and more than 25-fold over controls at 16 hours post-drug administration. Sodium acetylcyanamide (1), the salt of the major urinary metabolite of cyanamide, was, as expected, much weaker than cyanamide in the elevation of ethanol-derived blood AcH; however, the compound still significantly elevated blood AcH at 3 hours (25-fold over controls). Benzoylcyanamide (2) displayed similar activity to 1 giving rise to slightly more elevation of blood AcH (10-fold over controls) at 16 hours than 1.
n-Butyrylcyanamide (3), with a four-carbon aliphatic acyl group, was found to be a short-acting AlDH inhibitor and was even more potent than cyanamide itself. The compound elevated blood AcH 170-fold over controls at 3 hours; however, AcH blood levels were rapidly reduced to approximately 20-fold over control levels at 16 hours. Pivaloylcyanamide (4) and 1-adamantoylcyanamide (5), which were designed to retard the rate of hydrolysis of the acylcyanamide linkage by attaching sterically bulky substituents on the carbonyl group, were found to be very potent, but short acting.
Palmitoylcyanamide (6) and stearoylcyanamide (7), two aliphatic fatty acylcyanamides, were almost as potent as cyanamide at 3 hours, and significantly higher blood AcH still prevailed at 16 hours, viz, 100-fold, and more than 50-fold over controls, respectively.
Pretreatment of rats with N-carbobenzoxycyanamide (8) followed by ethanol elevated to blood AcH levels 120-fold over controls at 3 hours, indicating that the carbobenzoxy group must have been cleaved effectively by an enzymatic process. N-Cbz-glycylcyanamide (9) also elevated blood AcH more than 80-fold over controls at 3 hours; however blood AcH was reduced to almost control levels at 16 hours. N-Cbz-glycyl-L-leucyl-cyanamide (12) was more potent than (9) at 3 hours, but like the latter, did not maintain significantly elevated blood AcH level at 16 hours.
Hippurylcyanamide (10) was less potent than N-benzoyl-L-leucylcyanamide (11), probably because 10 is a poorer substrate for leucine aminopeptidase than is 11. These compounds not only elevated blood AcH levels at 3 hours, but were also long-acting with significant levels of blood AcH present at 16 hours.
N-Cbz-L-pyroglutamylcyanamide (13) and L-pyroglutamyl-L-leucyl-cyanamide (14) were not nearly as potent as the other prodrugs. Unlike 14, L-pyroglutamyl-L-phenylalanylcyanamide (15) was found to be a very potent inhibitor of AlDH in vivo, giving rise to blood levels which were more than 110-fold higher than control levels at 3 hours.
Based on the above results, compounds 6, 7, 10 and 11 were selected for further studies in vivo. Their duration of effectiveness in elevating blood AcH was evaluated over a 72-hour time course according to the protocol described hereinabove.
As shown in FIG. 5, blood AcH elevation by cyanamide reached a maximum within 2 hours, then the levels fell rapidly almost to control values at 36 hours. When palmitoylcyanamide (6) and stearoylcyanamide (7) were preadministered before ethanol, blood AcH levels reached their maxima at around 5 hours, then gradually fell, but the blood AcH elicited by 6 was significantly elevated even at 48 hours. Hippurylcyanamide (10) failed to maintain elevated blood AcH past 12 hours. In contrast, N-benzoyl-L-leucylcyanamide (11) initially elevated the blood AcH level less than cyanamide at 2 hours, but this compound continued to maintain elevated blood AcH even at 72 hours.
When 6 and 11 were administered by the oral route, both compounds gave similar blood AcH elevation curves, i.e., maximum AcH levels were seen at 2 hours, the AcH levels rapidly decreased to a trough at 12 hours, then once again increased at 24 hours (FIG. 6). Blood AcH then gradually fell back to control levels at around 36 hours.
Thus, a wide variety of acylated cyanamide analogs have been demonstrated to be effective to substantially raise mammalian blood AcH levels in the presence of ethanol. A number of the analogs of the present invention produced higher initial AcH levels and/or maintained the elevated AcH levels for longer periods of time than those produced by cyanamide itself. However, even relatively less-potent or short-acting compounds may be clinically useful as alcohol deterrent agents if they are found to be more specifically-acting than cyanamide itself, and/or are formulated appropriately.
The invention has been described with reference to various specific and preferred embodiments and techniques. However, it should be understood that many variations and modifications may be made while remaining within the spirit and scope of the invention. | Acylated cyanamide compounds useful for ethanol deterrence of the formula RCONHCN, wherein R is a lipophilic acyl group or is derived from an (N-substituted)-alpha-aminoacyl group. | 8 |
RELATED APPLICATIONS
[0001] This patent application claims the benefit of U.S. Provisional Patent Application No. 62/329,937, filed Apr. 29, 2016, which is incorporated by reference herein in its entirety.
TECHNICAL FIELD
[0002] The present disclosure relates generally to sensing systems, and more particularly to capacitance-sensing systems configurable to measure self capacitance or convert self capacitance to digital values representative of the capacitance.
BACKGROUND
[0003] Capacitance sensing systems can sense electrical signals generated on electrodes that reflect changes in capacitance. Such changes in capacitance can indicate a touch event (i.e., the proximity of an object to particular electrodes). Capacitive sense elements may be used to replace mechanical buttons, knobs and other similar mechanical user interface controls. The use of a capacitive sense element allows for the elimination of complicated mechanical switches and buttons, providing reliable operation under harsh conditions. In addition, capacitive sense elements are widely used in modern customer applications, providing new user interface options in existing products. Capacitive sense elements can range from a single button to a large number arranged in the form of a capacitive sense array for a touch-sensing surface.
[0004] Arrays of capacitive sense elements work by measuring the capacitance of a capacitive sense element, and looking for a delta (change) in capacitance indicating a touch or presence of a conductive object. When a conductive object (e.g., a finger, hand, or other object) comes into contact with or close proximity to a capacitive sense element, the capacitance changes and the conductive object is detected. The capacitance changes of the capacitive touch sense elements can be measured by an electrical circuit. The electrical circuit converts the measured capacitances of the capacitive sense elements into digital values.
[0005] There are two typical types of capacitance: 1) mutual capacitance where the capacitance-sensing circuit has access to both electrodes of the capacitor; 2) self capacitance where the capacitance-sensing circuit has only access to one electrode of the capacitor where the second electrode is tied to a DC voltage level or is parasitically coupled to Earth Ground. A touch panel has a distributed load of capacitance of both types (1) and (2) and some touch solutions sense both capacitances either uniquely or in hybrid form with its various sense modes.
DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 illustrates a capacitance measurement system, according to one embodiment.
[0007] FIG. 2 illustrates a ratiometric capacitance to code converter, according to one embodiment.
[0008] FIG. 3 illustrates voltage waveforms for a ratiometric capacitance to code converter, according to one embodiment.
[0009] FIG. 4 illustrates accumulated voltage waveforms for varied proportions of sensor, modulation, and integration capacitances, according to one embodiment.
[0010] FIG. 5 illustrates a ratiometric capacitance to code converter with different clock sources, according to one embodiment
DETAILED DESCRIPTION
[0011] FIG. 1 illustrates a capacitance sensing system 100 that may incorporate the proposed ratiometric capacitance to code converter of the present application. System 100 may include at least one capacitance sensing electrode 101 coupled to a sensing circuit 110 . In one embodiment, sensing circuit 110 may include circuitry integrated into a single device. In another embodiment, the various components of sensing circuit 110 may be distributed amongst several discrete components. For ease of explanation, sensing circuit 110 will be described herein as a single integrated circuit device. Sensing electrodes 101 may be coupled to sensing circuit 110 through inputs 105 . Inputs 105 may be coupled to inputs of a receive channel 120 . Receive channel 120 may be configured to convert capacitance to a digital value, such as with the proposed ratiometric capacitance to code converter. Receive channel 120 may be coupled to external components 125 as such may be necessary for the conversion. External components may be coupled to sensing circuit 110 through inputs 106 . Receive channel 120 may be coupled to decision logic 130 and to MCU 140 .
[0012] Decision logic 130 may be configured to process the output of receive channel 120 to determine whether a change in digital values representative of capacitance is associated with a touch or other action. Decision logic 130 may also be configured to track baseline or background capacitance values for use in touch detection. MCU 140 may be used to configure receive channel 120 based on system or application requirements. The configuration of receive channel 120 and MCU 140 may be at startup, during runtime, or based on some interrupt of host-generated commands. MCU 140 may also be configured to execute functions similar to decision logic 130 and used to make decisions regarding the presence of an object on the capacitance sensing electrodes 101 or for baseline or background capacitance tracking. MCU 140 and decision logic 130 may be coupled to memory unit 150 for storing values associated with touch detection. Memory unit 150 may also store program files and commands that are executed by MCU 140 . MCU 140 may also be coupled to external components, as necessary, through inputs 107 . MCU 140 may also be coupled to communication interface 160 , which may be used to output status to host 180 or another external device. Communication interface 160 may also be configured to receive commands from an external device.
[0013] FIG. 2 illustrates an embodiment of a capacitance-to-code converter 200 that may be implemented as receive channel 120 of sensing circuit 110 of FIG. 1 . Capacitance-to-code converter 200 may include a first charge transfer circuit 210 including a sensor capacitor 212 (see capacitance sensing electrode 101 of FIG. 1 ). Sensor capacitor 212 may have a first plate alternately coupled to a source voltage and an integration capacitor 216 . Sensor capacitor 212 may have a second plate coupled to a ground potential. Sensor capacitor 212 alternates between the source voltage and integration capacitor 216 through deadband switches 213 and 214 . Deadband switches 213 and 214 may be clocked by clock signal Fclk. In a first phase, when switch 213 is closed, a voltage potential is produced on sensor capacitor 212 . In a second phase, when switch 214 is closed, charge accumulated on sensor capacitor 212 during the first phase is transferred to integration capacitor 216 .
[0014] Capacitor to code converter 200 includes a second charge transfer circuit 220 including a modulation capacitor 222 . Modulation capacitor 222 may have a first plate alternately coupled to an integration capacitor 226 and a source voltage. Modulation capacitor 222 may have a second plate coupled to a ground potential. Modulation capacitor 222 alternates between the source voltage and integration capacitor 226 through deadband switches 223 and 224 . Deadband switches 223 and 224 may be clocked by an output of sigma-delta modulator 230 . Switches 223 and 224 may couple modulation capacitor 222 to integration capacitor 226 and the source voltage at opposite phases as modulation capacitor 222 is coupled to integration capacitor 226 and the source voltage. That is, in a first phase, when switch 224 is closed, modulation capacitor 222 is coupled to integration capacitor 226 , transferring charge accumulated on the modulation capacitor 222 to integration capacitor 226 . In the second phase, when switch 223 is closed, modulation capacitor 222 is coupled to the source voltage, allowing charge to accumulate on modulation capacitor 222 .
[0015] Integration capacitors 216 and 226 may be coupled to inputs of comparator 232 . In one embodiment, integration capacitor 216 is coupled to an inverting input of comparator 232 . One of ordinary skill in the art would understand that integration capacitor 226 may be coupled to an inverting input instead. As the voltages on integration capacitors 216 and 226 are compared by comparator 232 , a bit stream output 238 is generated. Bit stream output 238 may be a synchronized output of comparator 232 and a control clock from control block 244 through latch 234 .
[0016] The bit stream output of comparator 232 may be digitized by decimator and control logic 240 . The bit stream output 238 may also be used to provide a clock frequency to charge transfer circuit 220 through AND gate 236 , which may have a second input coupled to Fclk.
[0017] The operation of capacitance-to-code converter 200 has a reset phase, wherein integration capacitors 216 and 226 are reset to a ground potential by switches 217 and 227 , respectively. One of ordinary skill in the art would understand that a reset to ground is merely one embodiment. In various other embodiments, reset switches 217 and 227 may be configured to reset integration capacitors to voltages that are not a zero potential. After integration capacitors 216 and 226 are reset to ground, switches 217 and 227 are opened and the charge transfer from sensor capacitor 212 and modulation capacitor 222 begins. Integration capacitors 216 and 226 have charge accumulated on them by the repeated transfer of charge from sensor capacitor 212 and modulation capacitor 222 , respectively. The duty cycle (DC) of the bit stream output of comparator 232 , based on the inputs from the integration capacitor 216 and modulation integration capacitor 226 is given by:
[0000]
DC
=
C
int
2
C
int
1
·
C
s
C
m
.
[0018] The duty cycle output depends on the capacitive relationship between the sensor capacitor 212 and the reference capacitors (modulation capacitor 222 and integration capacitors 216 and 226 , wherein Cint 1 is integration capacitor 216 and Cint 2 is integration capacitor 226 ). In one embodiment, reference capacitors may be sensors but configured as reference capacitors for measurement of other sensor capacitors. As long as the capacitance values of the reference capacitors (either discrete or on-chip capacitors, or sensor capacitors) remain relatively constant over the measurement of the sensor capacitor under test, capacitance-to-code converter 200 operates as expected. If a sensor capacitor not under test is used as the modulation capacitor 222 , the temperature coefficients of the sensor capacitor 212 under test and the modulation capacitor 222 will be similar, providing temperature insensitivity. This temperature insensitivity may be particularly useful in wake-on-touch and low-power applications.
[0019] In one embodiment, the capacitance value of each integration capacitor 216 and 226 is considerable larger than its respective sensor capacitor 212 or modulation capacitor 222 . The values of integration capacitors 216 and 226 may be 1000 times greater than the capacitance of the sensor capacitor 212 and modulation capacitor 222 .
[0020] As the number of charge transfer cycles for integration capacitors 216 and 226 define the resolution of the capacitance to code converter 200 , a digital timer counts the number of charge transfer cycles (the operation of switches 213 / 214 and 223 / 224 ) and terminates the measurement cycle when the required number of charge transfer cycles has been reached. Of note, the output of the capacitance-to-code converter 200 is not dependent on the clock frequency, Fclk, only the number of clock pulses for the desired measurement count. Also, the output of capacitance-to-code converter 200 is not dependent on supply voltage (V DD ). This architecture allows the use of spread-spectrum, random, pseudo-random, or fixed frequency clock sequencers. Fclk may be any of these clock types.
[0021] As the output of comparator 232 is processed by the decimator and control logic 240 , the digital value, RawData, representative of the capacitance on sensor capacitor 212 may be given by:
[0000] RawData= DC·N RES ,
[0000] where N RES is the number of Fclk cycles during the measurement time. In one embodiment, N RES is selected from the order of two:
[0000] N RES =2 n −1,
[0000] where n is a whole, positive integer. The average excitation current, I s1 _ avg , which defines the noise immunity to external noise is given by:
[0000] I s1 _ avg =V swing _ avg ·F clk ·C s1 ,
[0000] where V swing _ avg is the average difference between the voltage on integration capacitor 216 and the supply voltage of charge transfer circuit 210 over the measurement interval.
[0022] Decimator and logic block 240 may include a decimator 242 and a module 244 . Decimator 242 may be a digital filter configured to reduce the input sample rate received from the output of latch 234 and provide a reduced data rate as the output of decimator and logic block 240 .
[0023] FIG. 3 illustrates voltage waveforms at various nodes of the capacitance to code converter 200 . During operation of charge transfer circuit 210 , the voltage on sensor capacitor 212 increases according to waveform 312 . Note, this is an exponential increase, but one of ordinary skill in the art would understand that charge transfer circuit 210 may be configured to generate a linear response as charge is shared with integration capacitor 216 . As charge is accumulated on integration capacitor 216 and modulation capacitor 226 , the voltage on each increases as shown by wave forms 316 and 326 . Fclk provides the clock signal to the charge transfer operation as well as the comparator 232 , which generates the bitstream output waveform 332 , which is converted to the digital value used in making determinations on the state of sensor capacitor 212 .
[0024] As stated above with regard to FIG. 2 , the proportionate capacitance of sensor capacitor 212 and modulation capacitor 222 to integration capacitors 216 and 226 , respectively, determines the effective resolution and the external noise immunity of capacitance to code converter 200 . Proportionately larger integration capacitors may provide greater resolution and noise immunity. With regard to noise immunity, the greater the average value of V swing , the greater the immunity. V swing is the difference between the voltage on the integration capacitor at each charge transfer cycle and the supply voltage.
[0025] FIG. 4 illustrates example V swing values for sensor-to-integration capacitance ratios of 1:10 ( 410 ) and 1:100 ( 420 ). With a smaller integration capacitor, relative to the sensor capacitor, the voltage increase across the integration capacitor with each charge transfer cycle is greater. For example, if ten charge transfer cycles are used for the conversion measurement window, the average V swing value at each cycle is greater.
[0026] FIG. 5 illustrates another embodiment of capacitance to code converter 500 , which is similar to capacitance to code converter 200 of FIG. 2 , but wherein the clock frequency, Fmod, of the modulation capacitor charge transfer circuit 220 is greater than the clock frequency, Fsw, of the sensor capacitor charge transfer circuit 210 . In this embodiment, Fmod may be given by:
[0000] Fmod= N·F sw ,
[0000] where N is a positive integer. The duty cycle output of capacitance to code converter 500 is therefore given by:
[0000]
DC
=
C
int
2
C
int
1
·
C
s
N
·
C
m
.
[0000] Increasing the Fmod relative to Fsw allows for smaller modulation capacitors ( 212 and 222 ), which may allow them to be integrated on-chip far easier.
[0027] The embodiments described herein may be used in various designs of mutual-capacitance sensing arrays of the capacitance sensing system, or in self-capacitance sensing arrays. In one embodiment, the capacitance sensing system detects multiple sense elements that are activated in the array, and can analyze a signal pattern on the neighboring sense elements to separate noise from actual signal. The embodiments described herein are not tied to a particular capacitive sensing solution and can be used as well with other sensing solutions, including optical sensing solutions, as would be appreciated by one of ordinary skill in the art having the benefit of this disclosure.
[0028] In the above description, numerous details are set forth. It will be apparent, however, to one of ordinary skill in the art having the benefit of this disclosure, that embodiments of the present invention may be practiced without these specific details. In some instances, well-known structures and devices are shown in block diagram form, rather than in detail, in order to avoid obscuring the description.
[0029] Some portions of the detailed description are presented in terms of algorithms and symbolic representations of operations on data bits within a computer memory. These algorithmic descriptions and representations are the means used by those skilled in the data processing arts to most effectively convey the substance of their work to others skilled in the art. An algorithm is here and generally, conceived to be a self-consistent sequence of steps leading to a desired result. The steps are those requiring physical manipulations of physical quantities. Usually, though not necessarily, these quantities take the form of electrical or magnetic signals capable of being stored, transferred, combined, compared and otherwise manipulated. It has proven convenient at times, principally for reasons of common usage, to refer to these signals as bits, values, elements, symbols, characters, terms, numbers or the like.
[0030] It should be borne in mind, however, that all of these and similar terms are to be associated with the appropriate physical quantities and are merely convenient labels applied to these quantities. Unless specifically stated otherwise as apparent from the above discussion, it is appreciated that throughout the description, discussions utilizing terms such as “encrypting,” “decrypting,” “storing,” “providing,” “deriving,” “obtaining,” “receiving,” “authenticating,” “deleting,” “executing,” “requesting,” “communicating,” or the like, refer to the actions and processes of a computing system, or similar electronic computing device, that manipulates and transforms data represented as physical (e.g., electronic) quantities within the computing system's registers and memories into other data similarly represented as physical quantities within the computing system memories or registers or other such information storage, transmission or display devices.
[0031] The words “example” or “exemplary” are used herein to mean serving as an example, instance or illustration. Any aspect or design described herein as “example’ or “exemplary” is not necessarily to be construed as preferred or advantageous over other aspects or designs. Rather, use of the words “example” or “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 includes A or B” is intended to mean any of the natural inclusive permutations. That is, if X includes A; X includes B; or X includes both A and B, then “X includes A or B” is satisfied under any of the foregoing instances. In addition, the articles “a” and “an” as used in this application and the appended claims should generally be construed to mean “one or more” unless specified otherwise or clear from context to be directed to a singular form. Moreover, use of the term “an embodiment” or “one embodiment” or “an implementation” or “one implementation” throughout is not intended to mean the same embodiment or implementation unless described as such.
[0032] Embodiments described herein may also relate to an apparatus for performing the operations herein. This apparatus may be specially constructed for the required purposes, or it may comprise a general-purpose computer selectively activated or reconfigured by a computer program stored in the computer. Such a computer program may be stored in a non-transitory computer-readable storage medium, such as, but not limited to, any type of disk including floppy disks, optical disks, CD-ROMs and magnetic-optical disks, read-only memories (ROMs), random access memories (RAMs), EPROMs, EEPROMs, magnetic or optical cards, flash memory, or any type of media suitable for storing electronic instructions. The term “computer-readable storage medium” should be taken to include a single medium or multiple media (e.g., a centralized or distributed database and/or associated caches and servers) that store one or more sets of instructions. The term “computer-readable medium” shall also be taken to include any medium that is capable of storing, encoding or carrying a set of instructions for execution by the machine and that causes the machine to perform any one or more of the methodologies of the present embodiments. The term “computer-readable storage medium” shall accordingly be taken to include, but not be limited to, solid-state memories, optical media, magnetic media, any medium that is capable of storing a set of instructions for execution by the machine and that causes the machine to perform any one or more of the methodologies of the present embodiments.
[0033] The algorithms and displays presented herein are not inherently related to any particular computer or other apparatus. Various general-purpose systems may be used with programs in accordance with the teachings herein, or it may prove convenient to construct a more specialized apparatus to perform the required method steps. The required structure for a variety of these systems will appear from the description below. In addition, the present embodiments are not described with reference to any particular programming language. It will be appreciated that a variety of programming languages may be used to implement the teachings of the embodiments as described herein.
[0034] The above description sets forth numerous specific details such as examples of specific systems, components, methods and so forth, in order to provide a good understanding of several embodiments of the present invention. It will be apparent to one skilled in the art, however, that at least some embodiments of the present invention may be practiced without these specific details. In other instances, well-known components or methods are not described in detail or are presented in simple block diagram format in order to avoid unnecessarily obscuring the present invention. Thus, the specific details set forth above are merely exemplary. Particular implementations may vary from these exemplary details and still be contemplated to be within the scope of the present invention.
[0035] It is to be understood that 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 reading and understanding 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. | A circuit, system, and method for converting self capacitance to a digital value may include a pair of charge transfer circuits, each including a deadband switch network, a sensor capacitor or modulation capacitor, and an integration capacitor may be coupled to a comparator to produce a bitstream representative of the capacitance of the sensor capacitor of one of the charge transfer circuits. The bitstream may be used to indicate a capacitance value of the self capacitance through conversion by a digitizing circuit element. | 7 |
BACKGROUND OF THE INVENTION
Energy resources are finally being recognized as finite. Temporary shortages have already surfaced. On-the-farm energy consumption is small (2%-4%) compared to the total U.S. use. Nonetheless, energy conservation in all segments is important and the accumulation of savings can have a significant effect on energy use. While food production must be considered a priority use of energy resources, there is a need to operate as efficiently as possible.
The energy consumed on dairy farms for cleaning the milking system is a major component of the total energy use. New designs in parlors, CIP systems, and demands from inspectors for better sanitation in general have resulted in increased consumption of hot water, detergents and sanitizing agents.
On dairy farms that use electric water heaters, approximately 1/4 of the electrical power consumed is for heating water. Improved efficiency in cleaning milking equipment could, therefore, result in substantial savings in energy. Dairy farms are continually increasing in size and the economic benefits associated with salvaging water and cleaning supplies for reuse are becoming significant.
Various systems of the CIP type for automatic milking machines have previously been described, e.g., U.S. Pat. No. 2,558,628 issued to Redin, 2,717,576 issued to Hansen, and U.S. Pat. No. 3,728,157 issued to Griparis. In such previously described machines it has been common practice to (1) employ high temperature prerinse and cleaning solutions, and (2) discharge the cleaning solution following the cleaning cycle into the environment. That previous practice apparently assumed that high temperature prerinse and cleaning solutions and the use of a fresh cleaning solution for each cleaning cycle would eliminate harmful residual bacteria. It was recently discovered that contrary to those assumptions, the pre-rinse and reconstituted and recycled cleaning solution when maintained at a temperature of 50° F - 120° F, not only improves cleaning of the system and reduces the quantity of harmful bacteria, but also results in energy savings, reduction in environmental pollution, and a reduction in cost of cleaning agents, as well as water consumption.
SUMMARY OF THE INVENTION
In accordance with the principles of this invention, a cleaning method and apparatus is provided for automatic milking machines of the CIP type wherein a cleaning solution holding tank stores the solution at a pre-determined temperature and the solution is reconstituted before reuse.
A feature of this invention is that when the cleaning solution is stored and reconstituted before reuse, and that solution as well as the pre-rinse are maintained within 50° F and 120° F, a substantial saving in energy and improved cleaning results.
Another feature of the invention is that cleaning solutions are stored for reuse in an insulated container thereby preserving the heat energy.
BRIEF DESCRIPTION OF THE DRAWINGS
The single FIGURE of the drawing is in schematic form and illustrates a CIP system for automatic milking machines constructed in accordance with the principles of this invention.
DETAILED DESCRIPTION
Referring now to the drawing, there is illustrated in schematic form, a milking claw and holder 1, a milk weigh jar 2, a receiving jar 3, a vacuum pump 4, and a milk pump 5. During the normal milking operation, the milking claw is attached to the cow and milk flows through the milk lines 6, 7 and the connecting portion of main line 8 to the milk weigh jar 2. Following that milking operation, the milk from milk weigh jar 2 is transferred to the receiving jar 3. That milking operation may be repeated for each of several cows. It will be understood that it is common practice for an automatic milking machine to have many milking claw and holder units and many milk weigh jars similarly connected to the main line 8 so that several cows can be milked simultaneously. When the milk level in receiving jar 3 is above a pre-determined level, the milk pump 5 transfers the milk through lines 10, 11 by way of check valve 12 and filter 13 to a bulk storage tank not shown. As shown in the drawing, the milk pump 5 is connected to the receiving jar 3 by line 9.
A customary milking operation as thus far described, usually takes about 1 to 3 hours (about 75 to 300 cows). The time between successive milking operations may be about 8 to 12 hours since cows are ususally milked twice a day. If milk residue is allowed to remain in the various units and milk lines of the system between milking operations, bacteria growth could present serious health hazards. Following each major milking operation, it has become common practice to employ a CIP line 14 which is connected to the milk weigh jar 2 and milking claw and holder 1 and through that line has been transmitted in succession a hot pre-rinse liquid, a hot cleaning solution, and a cold post-rinse liquid. The pre-rinse, the cleaning solution and the post-rinse passes through all of the milking system units and milk lines to remove milk residue and thereby avoid a favorable condition for bacteria growth.
Such previous CIP systems have used water or chemically treated water for pre-rinse which is heated to about 110° F. Since most CIP lines and milk lines form a closed loop which is many feet in length and are uninsulated, that 110° F pre-rinse is frequently about 105° F when effecting the rinsing function. Similarly, it has been common practice to heat the cleaning solution to about 170° F and this solution also is about 105° F when effecting its cleaning function. The time required to complete the pre-rinse and cleaning phases of the CIP cycle is sufficiently long that the hard to clean areas are maintained at a temperature of about 105° F thereby promoting bacteria growth. It has also been common practice in such previous CIP systems to discharge into the environment the cleaning solution when the cleaning phase is completed.
In accordance with this invention, a CIP unit 15 includes a cleaning solution store (i.e., storage receptacle) 16, a sink (or container) 17, a source of cold water (CW), a source of hot water (HW), and control valves V 1 through V 5 . The cleaning solution store 16 is preferably of the insulated type to preserve the temperature of liquid stored therein and further includes a heating unit 18 to permit maintenance of the cleaning solution at the desired temperature.
The operation of the CIP unit is to perform a complete cleaning operation of the automatic milking machine parts having milk residue therein as follows:
1. Cleaning solution is placed in the store 16 and heater 18 energized, if necessary, to bring the solution to a temperature of between 50° F and 120° F;
2. valves V 3 and V 4 are opened and the flow rate of hot and cold water is suitably controlled to fill the sink 17 with pre-rinse at a temperature between 50° F and 120° F;
3. diverter valve V 1 is operated to the positon where liquid from CIP return line 11 passes to waste line 19;
4. Vacuum pump 4 is operated to create a vacuum in main milk line 8, milk weigh jar/s 2, milk claw and holder/s 1 and CIP line 14. The vacuum thus causes the pre-rinse in the sink 17 to pass through the system to the waste line 19 (the milk pump 5 automatically emptying receiving jar 3).
5. Diverter valve V 1 is operated to allow liquid from return line 11 to enter store 16 and valve 5 is operated to pass liquid from store 16 to sink 17;
6. When sink 17 contains a desired quantity of cleaning solution, the vacuum pump 4 again causes the contents of the sink to pass through the system until the desired number of passes through the loop have been made.
7. Valve V 5 is closed so that the cleaning solution is returned to the store for subsequent re-use;
8. Valve V 3 is opened to fill the sink to the desired level with cold post-rinse and diverter valve V 1 is operated to permit liquid from return line 11 to flow to waste line 19;
9. Vacuum pump 4 again causes the contents of the sink to pass through the system.
If desired, an automatic control system may be provided to cause valves V 1 through V 5 to be operated in the above noted sequence with the desired timing. As shown in the drawing, water may be introduced to the cleaning solution in the detergent storage 16 by operation of valve V 2 .
Experiments have been conducted in a milking parlor of the double-ten herringbone type in which one side employed the cleaning system according to this invention and the other side employed a conventional CIP system. About 200 cows were milked twice a day for several days on each side of the parlor. The required concentration of cleaning solution on both sides of the parlor was obtained using one pound of a standard commercial detergent. On the side employing this invention 11/2 ounces of detergent were added after each milking operation was completed. Microbial counts were made on each side at various hard-to-clean points in the system as well as in the final rinse water. There was no significant difference in microbial count in the final rinse water of the two dies of the parlor. However, hard-to-clean parts on the side employing this invention, such as the float in the receiving jar showed a marked decrease in microbial count. | A cleaning apparatus for automatic milking machines of the Clean-In-Place (CIP) type in which pre-rinse liquid and reused cleaning solutions are maintained at a temperature within 50 ° F. - 120° F. A vacuum pump and a liquid pump along with the operation of various valves enable the passage of the pre-rinse liquid and cleaning solution through the milking machine. An insulated storage receptacle with a heater maintains recovered cleaning solution at the desired temperature for reuse. | 8 |
BACKGROUND OF THE INVENTION
This application is a continuation-in-part of our copending application Ser. No. 322,423, filed Nov. 18, 1981 now U.S. Pat. No. 4,424,030 issued 1/03/84, which is a continuation of our original application, Ser. No. 019,427, filed Mar. 12, 1979 (now abandoned).
Said applications disclose various embodiments of magnetic osteogenic and orthodontic appliances, in which relative movement of magnetic devices produces varying currents in localized regions in aid of soft-tissue repair and osteogenesis. Some of the disclosed arrangements utilize magnetic devices for essentially only orthodontic purposes, while others are primarily adapted for soft-tissue repair and osteogenesis. Among the disclosed arrangements is an intra-oral positioning fixture comprising labial, buccal and lingual flanges and defining a channel adapted to span corresponding buccal and lingual areas of alveolar bone requiring osteogenesis and soft-tissue repair wherein separate sources of magnetic flux carried by the buccal and lingual flanges are adapted for coaction with each other via said areas of alveolar bone.
BRIEF STATEMENT OF THE INVENTION
It is an object of the invention to provide improved and further intra-oral positioning fixtures of the character indicated, adapted to therapeutically expose a magnetic field of desired character to a region of the periodontium, i.e., alveolar bone and and adjacent tissue requiring osteogenesis and/or soft-tissue repair.
It is one specific object to provide improved means whereby therapeutically beneficial varying magnetic fields may be produced by such a fixture, without resort to an external source of energy.
It is another specific object to provide improved means whereby such a fixture may provide a therapeutically beneficial non-varying magnetic field, with or without selective variation of the magnetic field.
Still another object is to achieve the above objects with non-invasive structure having removable, self-retaining positioning support within the mouth.
In a preferred form, the invention achieves the foregoing objects by providing a positioning fixture having buccal and lingual flanges which are adjacent corresponding buccal and lingual areas of the periodontium requiring osteogenesis and soft-tissue repair, there being separate sources of magnetic flux carried by the buccal and lingual flanges and magnetically coacting with each other via said areas.
DETAILED DESCRIPTION
The invention will be illustratively described in detail in conjunction with the accompanying drawings, in which:
FIG. 1 is a perspective view of a positioning fixture of the invention;
FIG. 2 is a sectional view taken at 2--2 in FIG. 1;
FIG. 2A is a view similar to FIG. 2, to show a modification;
FIG. 3 is a view similar to FIG. 1, to show another embodiment;
FIG. 4 is an enlarged and simplified view in perspective to show a magnetic component of the fixture of FIG. 3;
FIG. 5 is an end view of the component of FIG. 4, partly broken-away to show the central vertical section thereof;
FIG. 6 is another view in perspective to show the other side of the component of FIG. 4;
FIG. 7 is a view similar to FIGS. 1 and 3, to show a further embodiment;
FIG. 8 is a perspective view to show a magnetic component of the fixture of FIG. 7; and
FIG. 9 is a simplified plan view of a dental plate incorporating magnetic means of the invention.
In FIGS. 1 and 2, the invention is shown in application to a positioning fixture 10 of suitably compliant bio-compatible plastic or elastomeric material, generally characterized by buccal and lingual flanges 11-12 which are integrally connected by an occlusal flange 13. The flanges 11-12-13 define a channel 14 which, in the form shown, is downwardly open and conforms to and spans the course of teeth and the periodontium, including the alveolar bone, of the lower jaw or mandible; and it will be understood that similar structure, inverted to provide an upwardly open channel, may similarly conform to the course of teeth and alveolar bone of the upper jaw.
The flanges 11-12-13 of fixture 10 are the product of custom-molding to the individual tooth and jaw features of the particular patient. Thus, the inner surfaces of the buccal and lingual flanges converge in the direction of the channel opening (as seen in FIG. 2), in conformance with involved tooth profiles, to establish a naturally hugging engagement with and retention to involved teeth, while permitting selective removability, by reason of the compliant nature of the material of the flanges.
In accordance with a feature of the invention, first and second sources 15-16 of magnetic flux are carried by or embedded in the respective buccal and lingual flanges 11-12. As shown, each of the sources 15-16 is a permanent magnet, in the shape of a thin circular disc, of suitably half-inch or one-centimeter diameter and of thickness which is a small fraction of the diameter, as in the range of 10 to 25 percent of the diameter. Preferably, each of the magnets 15-16 is polarized on its axis, thus establishing the circular end faces of each magnet as opposite poles, and the placement of magnets 15-16 is in mutually facing relation across that part of the channel 14 where periodontal therapy and/or alveolar-ridge maintenance is needed.
If the opposed adjacent faces of magnets 15-16 are of opposite polarity, a strong uniform flux field is established across the region of desired tissue therapy or maintenance, with therapeutically beneficial effectiveness over approximately six or more months, when worn with daily consistency, if not continuously. The exact mechanism of cell reaction to the strong flux field is not as yet fully understood, but it is presently believed that the degree of compliant yieldability of the fixture (10) material enables magnets 15-16 to be subject to periodic cycles of small displacement with respect to each other and with respect to the region of tissue therapy, as by reason of bite action, thus establishing concomitant variations in flux field through the tissue region, with accompanying induction of therapeutically beneficial, albeit low-level, voltages and currents in affected tissues and/or cells.
If, on the other hand, the opposed adjacent faces of magnets 15-16 are of the same polarity, then repulsion action between the magnets forces mushroom-like flux concentrations at and surrounding both the involved lingual and buccal regions of the teeth and alveolar bone. The same compliant yieldability exists in the material of fixture 10, and therefore the same belief is held that small displacements of the respective magnets enables local induction of beneficial voltages and currents in affected tissues and/or cells.
The modification of FIG. 2A illustrates that the supportive fixture of the invention may in fact comprise two parts, namely, an outer channel-shaped shell 10' which is preformed with thin walls (flanges 11'-12') which mount the sources 15-16 of magnetic flux, and a lining 17 which is custom molded to the involved buccal and lingual profiles of the patient. The preformed shell 10' may be of acrylic material, being one of a series of standardized shapes and sizes to accommodate a range of patients' individual requirements, with small clearance for molded development of the lining 17. The series of shapes may include premounted pairs of magnets 15-16, at particular standardized locations along the course of jaw; alternatively, the dentist may be supplied with a suitable punch and/or adhesive means for mounting the magnets 15-16 at buccal and lingual regions he has professionally determined to be most applicable to his patient's need. In either event, the lining 17 will effectively seal inner adjacent faces of magnets 15-16 against exposure to body or other fluids, and preference is indicated for a protective coating of biocompatible material, such as an acrylic, expoxy, urethane or other suitable adhesive at least over the outer faces of magnets 15-16.
In the embodiment of FIG. 3, a positioning fixture of the invention comprises an arcuate inner or lingual flange member 20 (corresponding to flange 12 in FIG. 1) and two separate arcuate outer or buccal flange members 21-22. The two buccal members 21-22 separably meet at the front center of the course of the jaw, and their molar (distal) ends are flexibly connected to the corresponding ends of lingual member 20, via generally U-shaped wires 23--23' having end-embedment in members 20-21 and 20-22 respectively; the wire connections 23--23' will be understood to provide additional means of tooth anchorage or of orthodontic force application to a tooth, for example, to a molar. Each of the buccal members 21 (22) has a small integrally formed half-stud projection 24 (25), adapted for selectively removable retention to each other as by a small orthodontic elastic (not shown) applied around both projections 24-25.
As in the first-described embodiment, separate sources 26 (27) of magnetic flux may be embedded in or otherwise carried by members 20-21 (or 20-22) at mutually opposed locations, and the opposed adjacent surfaces of members 20-21 and 20-22 will be understood to be preferably custom-molded to the patient's individual dental buccal/lingual profiles. The technique of such molding may accord with either of the techniques described in connection with FIGS. 2 and 2A, except of course, there is nothing in FIG. 3 to correspond to the occlusal flange 13. This latter fact means more comfortable wearing of the FIG. 3 fixture, for the patient who can use his own teeth; and removal or mere stretching of the elastic retaining band at 24-25 enables simple removal of the fixture, as for cleaning purposes.
The sources 26-27 may again be permanent magnets, being shown as thin and rectangular, and the above-expressed belief as to why the arrangement is therapeutically beneficial continues to apply, it being noted that in FIG. 3, the magnets 26-27 are susceptible to more ready displacement than in FIG. 1, thus enabling at least as much varying magnetic-field action discussed above, in addition to the polarized field which is inherent in the coacting relation of the opposed magnets.
FIGS. 4, 5 and 6 are directed to a modified magnetic element which may be understood to be in substitution for the lingual-flange magnet 27 of FIG. 3. The point in FIGS. 4, 5 and 6 is that a permanently polarized magnet 27' carried by lingual flange member 20 shall be movable with respect to member 20. To this end, a rectangularly prismatic casing 30, as of bio-compatible acrylic material, is embedded in or otherwise mounted locally to the lingual flange member 20 as to expose its inner face 31 at the lingual side of flange member 20. The inner surfaces of casing 30 establish a guide for ready vertical displaceability of magnet 27', and means such as a headed stud 32 fixed to magnet 27' extends through a vertically short slot 33 in the lingual wall 31, poised for ready actuation by the tongue of the patient. Thus, with the embodiment of FIG. 3, modified to include the movable magnet 27' of FIGS. 4 to 6, greater and more frequent movement of magnets 26-27' is possible, with attendant enhancement of the voltage and current levels induced in affected tissues and/or cells.
Much of what is shown in the embodiment of FIG. 7 corresponds to what has been described for FIGS. 3 to 6, and therefore the same reference numerals are used for corresponding parts. The point of difference in FIG. 7 is that a different means is employed to permit tongue-actuated displacement of one or more sources of magnetic flux. In the form shown, a pair of laterally adjacent permanent-magnet discs 40-41 is carried by an arcuate bail 42 of archwire, as of stainless steel, having outwardly bent ends 43--43' (FIG. 8) which are pivotally referenced to local bearings (holes) at the molar ends of lingual flange member 20. Two similar magnet discs 44-45 are fixedly positioned in similar adjacency on one (22) of the buccal flange members, in coacting opposition to the movable magnet discs 40-41. Corresponding pole faces of magnets 40-41 should face in the same direction, and corresponding pole faces of magnets 44-45 should face in the same direction. And whether the polarities of magnets 40-41 should be in flux-aiding or flux-opposing relation to tne polarities of magnets 44-45 is subject to considerations discussed above for polarity relationships in the embodiment of FIGS. 1 and 2. The use of multiples of magnets in laterally adjacent array, as in the case of magnets 40-41 and 44-45 in FIG. 7, will be understood merely to extend the antero-posterior span of the described range of therapeutic action.
FIG. 9 illustrates application of the invention to a dental plate 50, which may be of the well-known Hawley variety, wherein a buccal magnet 51, protectively embedded as in an acrylic mount or casing is attached to plate 50 via wires 52-53 which span the tooth region to be treated. A coacting lingual magnet 54 is similarly encased and may be mounted for hinge action to posterior regions of plate 50, as described for the arcuate wire 42 and its magnet(s) in FIGS. 7 and 8; however, in the form shown, magnet 54 will be understood to have been received in a suitable local opening cut into and through plate 50, being suitably bonded in place.
The described embodiments of the invention will be seen to achieve the stated objects. These embodiments will be understood to be specifically applicable to various different patient requirements. For example, the embodiment of FIGS. 1 and 2 is more suitable (than those of FIGS. 3 and 7) for children as distinguished from older patients, for the reason that in children the lateral walls of teeth are less relieved or undercut, thus making for easy snap-action application and removal of the fixture. On the other hand, for the more undercut nature of teeth in older persons, the three-member articulated supports of FIGS. 3 and 7 are not only more comfortable but also more easily manipulated, for application or for removal.
In all three of the embodiments of FIGS. 1, 3 and 7, it will be understood that the custom-fit of the positioning fixture includes appropriate undulated contouring of the base profile, as by scissors-cut of the skirt 19 of buccal flange 11 in FIG. 1, to provide maximum overlap with the alveolar ridge, without chafing contact with the gums.
The embodiments of FIGS. 1, 3 and 7 will be seen to serve primarily for periodontal therapy and alveolar-ridge maintenance in edentulous patients, all such treatments being non-invasive. These embodiments also have application for bone augmentation, in the case of boneimplant surgery in the alveolar ridge. And the various embodiments are illustrative of use of the invention in an oral cavity which is also undergoing orthodontic therapy.
Various permanent-magnet materials are discussed in said copending parent application Ser. No. 322,423 and therefore their discussion need not be repeated. We merely state our present preference for SmCo as the magnet material and indicate our preference that each such magnet element be protectively coated with bio-compatible material, such as an acrylic.
While the invention has been described in detail for preferred embodiments, it will be understood that modification may be made without departing from the scope of the invention. For example, the particular lingual-magnet suspensions of FIGS. 3 to 6 and 7 will be understood to be further optionally applicable to FIG. 1, in place of the fixed lingual magnet 16.
Further, by way of example, although usage of plural magnets has been described in the context of all such magnets being permanently polarized, it is not necessary that they all be polarized to achieve a beneficial orthodontic or osteogenic or periodontic result. For orthodontic purposes, it is sufficient that one permanent magnet or other source of magnetic flux be established and that one or more elements of magnetic-flux conducting material serve for attractive coaction therewith. And for an osteogenic or periodontic result, it is again sufficient to employ a single source of magnetic flux, for magnetic-field variation as a function of relative movement between one of the elements as the source and the other (or another) of the elements as a means of parasitic coaction with the source element. Thus, reference herein to plural polarized magnet elements reacting with each other merely states a preferred relationship, and non-polarized parasitic reaction of the character indicated is included within the compass of the invention.
It is also to be understood that the expression "non-invasive" as used herein applies to the fact that magnetic fields and changing magnetic fields, as the same are exposed to tooth, bone and other body tissue, are surgically non-invasively applied. The expression "non-invasive" as used herein thus does not preclude applicability of magnetic fields of the invention to tooth, bone or other body tissue which may have been surgically implanted, as for reasons of bone grafting or other reinforcement. | The invention contemplates a unitary intra-oral positioning fixture for use in orthodontic and/or periodontal therapy and bone augmentation. The fixture provides compliant support for two coacting sources of magnetic flux, respectively positioned on the lingual and buccal sides of a region of a tooth or teeth (and adjacent alveolar bone) requiring osteogenesis and soft-tissue repair. | 0 |
BACKGROUND OF THE INVENTION
[0001] The present invention provides for an improved electrical conduit outlet body. Electrical wiring is usually provided in bundles which may be a bundle of single conductors where each conductor is covered with its own dielectric barrier. An additional insulating layer such as polytetrafluoroethylene (PTFE) shrink tubing may be added over the bundles.
[0002] Conduits provide the means by which wires or bundles of wires are secured to the facility where the electrical wiring is to be installed. Typically the conduits are provided in various sizes and can be straight or have bends depending upon the type of installation. The electrical conduit thus serves to hold and to protect the wiring run through it.
[0003] The electrical conduits can be made of metal such as galvanized steel pipe, or made from plastic pipe. Electrical conduits are generally divided into four classes: thin-wall metal conduit, rigid threaded conduit, plastic conduit and flexible metal conduit. These conduits can come in different lengths and can be employed in any installation as long as they are employed in compliance with local, state and/or national codes.
[0004] The electrical conduits will typically terminate with a piece that must provide for drainage of water. For example, the 2008 National Electrical Code states in Article 225.22 that raceways on exteriors of buildings or other structures shall be arranged to drain and shall be rain tight in wet locations. Further in Article 230.53, this Code states that raceways enclosing service-entrance conductors shall be suitable for use in wet locations and arranged to drain. Raceways embedded in masonry shall be arranged to drain as well. Article 501.15(f) also addresses requirements that raceway systems have appropriate water removal means. Water can accumulate through condensation in the electrical conduit due to the factors of temperature change during the course of day and heating and cooling of the electrical wires inside the electrical conduit. This water must be removed in some fashion or it can cause problems such as shorting of the electrical wires or rusting and corrosion of the electrical conduit itself. Typically the electrical conduit termination will have an opening in the conduit which is generally threaded and to which a trap or drain is attached. This will allow for egress of moisture and prevent the problems associated with water accumulating in the electrical conduit.
[0005] While these are necessary solutions to the build up of water, they also add cost and time to the job of installing electrical wires and add further complexity to the wiring job. The present inventor has discovered a solution to the problem of water build-up that does not require the use of additional connections, traps and drains.
SUMMARY OF THE INVENTION
[0006] The present invention provides for an improved electrical conduit outlet body comprising a tubular member having at least two apertures, the improvement comprising at least one hole being present in the tubular member.
[0007] The tubular member must have a diameter sufficient to allow the passage of electrical wires there through. This “fill” is also dictated by the National Electrical code as to the percentage of circular area you can fill with wiring and still maintain enough air circulation for cooling of the wires (typically about 40%).The tubular member consists of an interior wall surface and an exterior wall surface. The thickness of the tubular member will vary according to local and national building codes but is typically in the range of about 3/16 inch to about ⅜ inch.
[0008] The tubular member may be made of any material that is suitable for electrical conduits and approved. Typically this is based on national or local building codes and the electrical conduits are made of metal or plastic. Preferred electrical conduit materials are selected from those approved by NEC and AHJ ((National Electrical Code (“NEC”) and Authority Having Jurisdiction (“AHJ”)) as well as those from nationally recognized listing agencies such as Underwriters Laboratories. Electrical conduits are commercially available from Cooper/Crouse-Hinds, Appleton and Killark.
[0009] At least two apertures are installed in the tubular member to allow the tubular member to be attached to different varieties of electrical conduits. These apertures are sized to be roughly the same diameter as the tubular member and comprise a flange which may be threaded or not. At least two apertures are typical and three, four or five may be on the ends of the tubular member or intersecting the tubular member at some point between the two ends. In the instance of two apertures, the tubular member will be closed at one end, generally opposite from where the aperture is present, forming a front wall that is situated above one aperture.
[0010] The at least one hole present in the tubular member may be any opening that is sized to allow for the egress of moisture and penetrates both the inner wall and outer wall of the tubular member. The at least one hole may be present at any of four locations depending upon the configuration of the tubular member and the number of apertures present in the tubular member These holes may be present on the top portion of the tubular member or on the bottom portion of the tubular member. The at least one hole may also be present in the closed end of the tubular member, as well as the side walls of the tubular member.
[0011] Alternatively, if the tubular member is cast, a knockout may be present on each surface and the end user can knockout whichever side is needed for drainage.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is an open top view schematic of an electrical conduit outlet body according to the present invention.
[0013] FIG. 2 is a side view schematic of an electrical conduit outlet body according to the present invention.
[0014] FIG. 3 is a top view schematic of an electrical conduit outlet body showing an alternative punch out for the holes depicted in FIGS. 1 and 2 .
DETAILED DESCRIPTION OF THE INVENTION
[0015] Turning to the figures, FIG. 1 is a top view schematic of the electrical conduit of the present invention. Tubular member 10 which can be made from a metal such as galvanized steel or plastic is shown with the cover removed. First side wall 11 and second side wall 12 define the outer walls of the tubular member and first inner wall 11 A and second inner wall 12 A define the inside dimensions of the tubular member. The diameter of the tubular member 10 must be sufficient to allow the appropriate wiring to pass through the tubular member 10 . This diameter is defined by local and national building codes and can range from about ½ inch to about 6 inches. The thickness of the wall between 11 and 11 A and 12 and 12 A can be in the range of about 3/16 inch to about ⅜ inch with 0.200″ typical.
[0016] For purposes of the present invention the tubular member can be any conventional shape such as circular, square, rectangular, triangular, oval and can be either straight or containing bends along its length.
[0017] The open end aperture 15 of the tubular member hosts a flange which is threaded so that the electrical conduit can connect with other components of the electrical wiring scheme. Likewise at the opposite end of the tubular member there is an aperture 13 hosting a threaded flange which is situated below the outer walls 11 and 12 . The positions of the holes that can be made in the tubular member are indicated by 14 A, 14 B, 14 C and 14 D. The number of holes that can be employed can be as few as one but can range upwards to any number that provides the appropriate moisture removal and taking into account the placement and positioning of the electrical conduit. As indicated in FIG. 1 , a hole may be placed in either of the two side walls 11 and 12 of the tubular member 10 or the hole can be placed at the front end of the tubular member as noted at position 14 D. Alternatively or with one or more of the other holes, a hole 14 B can be made in the bottom portion of the tubular member.
[0018] FIG. 2 depicts the electrical conduit from its side. This is a typical configuration for the electrical conduit which allows for the electrical wires to make a 90 degree angle to a further electrical railway. The tubular member 20 has a removal cover piece 25 which is situated above the top wall 21 of the tubular member 10 . The bottom wall 22 of tubular member 10 defines the diameter of the tubular member. As noted for FIG. 1 , the thickness of the walls can be in the range of about 3/16 inch to about ⅜ inch with 0.200″ typical. The inside diameter of the tubular member 20 must be sufficient to allow the appropriate electrical wiring to pass through the tubular member 20 . This diameter is defined by local and national building codes and can range from about ½ inch to about 6 inches.
[0019] The aperture 26 hosts a threaded flange which will allow this electrical conduit to be connected to other devices in the electrical wiring scheme. The front wall 23 of the tubular member 20 is situated above a second aperture 27 which hosts a threaded flange as well.
[0020] The one or more holes that can be employed in this electrical conduit are depicted by the designations 24 A, 24 B and 24 C. 24 A is actually a representation of two holes which can be present in either of the side walls of the tubular member 20 . Hole 24 B is positioned in the bottom of the tubular member 20 relative to the cover 25 . Hole 24 C is positioned in the front wall 23 of the tubular member. As indicated in the discussion of FIG. 1 , the at least one hole may be two or more holes depending upon the moisture removal needs of the installer of the electrical wiring and electrical conduit.
[0021] The holes can be fashioned in any suitable manner. They may be drilled through the walls of the tubular member or made by punching a hole in the tubular member. The holes may also be made after the electrical conduit has been made or may be created when the electrical conduit is originally formed.
[0022] The hole may be any size to allow moisture to leave the tubular member while not damaging the structural integrity of the electrical conduit. Typically up to 3/16 of an inch is preferred.
[0023] FIG. 3 shows a top view of a electrical conduit outlet body 30 according to the present invention. Outer side walls are shown as 31 and 32 being generally parallel to each other and being of a thickness of about 3/16 inch to about ⅜ inch to the inner walls 31 A and 32 A respectively. Outer end wall 34 and inner end wall 34 A are of the same thickness. The holes are not fully formed and are shown as punch outs 33 A and 33 B and are roughly trapezoidal shaped. The end user can utilize a punch or other instrument to punch through the punch out. This will create a hole in the electrical conduit body specifically for the electrical wiring installation utilizing the electrical conduit outlet body.
[0024] While this invention has been described with respect to particular embodiments thereof, it is apparent that numerous other forms and modifications of the invention will be obvious to those skilled in the art. The appended claims in this invention generally should be construed to cover all such obvious forms and modifications which are within the true spirit and scope of the invention. | An improved electrical conduit outlet body having a tubular member which contains at least two apertures and at least one hole. The hole will allow for the removal of water from the electrical conduit and will reduce the cost and labor in providing wiring by eliminating external traps and drains. | 7 |
FIELD OF THE INVENTION
The present invention relates to thin film batteries, and in particular, improved cathode materials and deposition techniques for certain layers of a thin film battery structure.
BACKGROUND OF THE INVENTION
All solid state Thin Film Batteries (TFB) are known to exhibit several advantages over conventional battery technology such as superior form factors, cycle life, power capability and safety. However, there is a need for cost effective and high-volume manufacturing (HVM) compatible fabrication technologies to enable broad market applicability of TFBs.
Most of the past and current state-of-the-art approaches, as they pertain to TFB and TFB fabrication technologies, have been conservative, wherein the efforts have been limited to scaling the basic technologies of the original Oak Ridge National Laboratory inventions that started in the early 1990s. More recently, some efforts to improve the properties and deposition rates for the cathode and electrolyte material layers have been seen. First is the application of a pulsed DC sputtering (i.e. pDC) technique to the cathode (LiCoO 2 specifically; e.g. U.S. Patent Pub. 2006/0134522), with some improvement in deposition rate. In addition, substrate biasing has been applied to both cathode (U.S. Patent Pub. 2006/0134522 and U.S. Pat. No. 6,921,464, the second one with RF on the target) and electrolyte (U.S. Pat. No. 6,506,289) deposition steps, leading to some improved properties. However, much improvement is still needed.
FIGS. 1A to 1F illustrate a traditional process flow for fabricating a TFB on a substrate. In the figures, a top view is shown on the left, and a corresponding cross-section A-A is shown on the right. There are also other variations, e.g., an “inverted” structure, wherein the anode side is grown first, which are not illustrated here.
As shown in FIGS. 1A and 1B , processing begins by forming the cathode current collector (CCC) 102 and anode current collector (ACC) 104 on a substrate 100 . This can be done by (pulsed) DC sputtering of metal targets (˜300 nm) to form the layers (e.g. main group metals such as Cu, Ag, Pd, Pt and Au, metal alloys, metalloids or carbon black), followed by masking and patterning for each of the CCC and ACC structures. It should be noted that if a metallic substrate is used, then the first layer may be a “patterned dielectric” deposited after a blanket CCC 102 (the CCC may be needed to block Li in the cathode from reacting with the substrate).
Next, in FIGS. 1C and 1D , the cathode 106 and electrolyte layers 108 are formed, respectively. RF sputtering has been the traditional method for depositing the cathode layer 106 (e.g. LiCoO 2 ) and electrolyte layer 108 (e.g. Li 3 PO 4 in N 2 ). However, pulsed DC has been used for LiCoO 2 deposition. The cathode 106 layer can be about 3 μm thick, and the electrolyte 108 layer can be about 1-2 μm thick.
Finally, in FIGS. 1E and 1F , the Li layer 110 and protective coating (PC) layer 112 are formed, respectively. The Li layer 110 can be formed using an evaporation process. The Li layer 110 can be about 3 μm thick (or other thickness depending on the thickness of the cathode layer) and the PC layer 112 can be in the range of 3 to 5 μm. The PC layer 112 can be a multilayer of parylene, metal or dielectric as disclosed by Oak Ridge National Laboratory. Note that, between formation of the Li layer and the PC layer, the part must be kept in an inert environment, such as argon gas.
There may be an additional “barrier” layer deposition step, prior to the CCC 102 , if the CCC does not function as the barrier and if the substrate and patterning/architecture call for such a barrier layer. Also, the protective coating need not be a vacuum deposition step.
In typical processes, annealing of the cathode layer 106 will be required if the TFB performance specification calls for “plateau of operating voltage” and high power capability. A summary of the TFB properties can be found in N. J. Dudney, Materials Science and Engineering B 116, (2005)245-249.
While some improvements have been made to the original ORNL approaches, there are many problems with the prior art fabrication processes for TFBs that prevent them from being compatible with cost effective and high-volume manufacturing (HVM), and thereby preclude broad market applicability of TFBs. For example, issues with the state-of-the-art thin film cathode and cathode deposition processes include: (1) a low deposition rate leading to low throughput and inefficient scaling (of economy) for cost reduction, (2) a need for a high temperature anneal for the crystalline phase, which adds to process complexity, low throughput and limitations on the choice of substrate materials, and (3) a higher electrical and ionic resistivity, which limits the thickness of the cathode and high power (in battery operation) application, as well as the applicable sputtering methodology and sputtering power (which determines deposition rate).
With respect to the electrolyte, RF sputtering does not provide a high deposition rate with good conformality for pinhole free deposition. The low deposition rate RF sputtering process affects the throughput while the low conformality affects yield. The electrolyte is the key layer that allows the TFB to function as an energy storage device. More particularly, electrolyte layers with very high electrical resistivity (>1×10 14 ohm-cm), have been deposited using RF sputtering with rates up to ˜2 Å/sec. Recently, when electrolyte layers were deposited using a PECVD process, the deposition rates appear to be higher, and provide reasonable properties in the resulting films. However, the long term reliability (cycle life) appears less than that observed in TFBs produced with RF sputtered layers. This discrepancy can be attributed to reactions between the charge carriers (lithium) and the impurity inclusions that likely result, during the PECVD processing, from incomplete oxidation of the organic ligands of the volatile precursors. As such, improvement in this layer will lead to significant outcomes for the overall technology.
Accordingly, a need remains in the art for fabrication processes and technologies for TFBs that are compatible with cost effective and high-volume manufacturing (HVM), and thereby enable broad market applicability of TFBs.
SUMMARY OF THE INVENTION
The present invention relates to methods and apparatuses that overcome key problems of current state-of-the-art thin film battery (TFB) technologies that preclude broad market applications. According to aspects of the invention, a key detriment addressed is the high cost of manufacturing, which can be attributed to both TFB technology and TFB manufacturing technologies. According to aspects of the invention, application of such techniques, methods and materials leads to much improved physical properties of TFBs (e.g. for improved performance with higher ionic and electronic conductivity), simplification of the TFB fabrication process (e.g. elimination or reduction of anneal step), and increase in throughput for HVM compatibility. All of these benefits will lead to reduced cost per function (or energy density) for truly broad application.
In one embodiment, the invention provides techniques and methods for new cathode materials and deposition methods for improved battery performance. A method of fabricating a layer of a thin film battery comprises providing a sputtering target and depositing the layer on a substrate using a physical vapor deposition process enhanced by a combination of plasma processes. The plasma processes are designed to transfer energy to a combination of: (a) the ions which bombard the target, (b) the ions in the bulk plasma between the target and the substrate, and (c) the ions hitting the deposition surface. Control of these ion energies and densities affects the deposition rate and morphology of deposited layers. The deposition process may include: (1) generation of a plasma between the target and the substrate; (2) sputtering the target; (3) supplying microwave energy to the plasma, including electron cyclotron resonance (ECR); and (4) applying radio frequency power, in continuous wave (CW) or burst mode, at a first frequency to the substrate. The sputtering step may include applying radio frequency power, of a second frequency, to the target. The first and second frequencies may either be sufficiently different to avoid interference effects or may be the same and locked in phase. Furthermore, when the target is sufficiently conductive, the sputtering step may include applying (pulsed) direct current to the target. High power pulsed magnetron (HPPM) may also be utilized as a sputtering power supply.
In another embodiment, the invention provides new deposition sources to facilitate the TFB fabrication process—increasing the throughput and yield. A sputtering target for a thin film battery cathode layer is manufactured to have an average composition of LiM a N b Z c , wherein 0.20>{b/(a+b)}>0 and the ratio of a to c is approximately equal to the stoichiometric ratio of a desired crystalline structure of the cathode layer, N is an alkaline earth element, M is selected from the group consisting of Co, Mn, Al, Ni and V, and Z is selected from the group consisting of (PO 4 ), O, F and N. The metals represented by M and the substitutional elements represented by N are not restricted to single species. For example, M may include both Co and Mn. In preferred embodiments, 0.12>{b/(a+b)}>0.05. Furthermore, the target may also comprise other substitutional elements taken from the transition metals in the periodic table. A desirable property of a deposited TFB cathode layer is good crystallinity and relatively high conductivity, whereby post deposition annealing is not required and the layer may be made relatively thick for increased capacity, but without compromising the power (current) density.
For electrolytes, the addition of energy to the growing film will allow enhanced conformality by allowing additional energy to promote surface diffusion of deposited species. Thus, pinhole free layers can be achieved with lesser thickness. This will help with throughput and battery properties, for example power density or capacity, by reducing the internal impedance.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other aspects and features of the present invention will become apparent to those ordinarily skilled in the art upon review of the following description of specific embodiments of the invention in conjunction with the accompanying figures, wherein:
FIGS. 1A to 1F illustrate steps of a conventional process for forming TFBs;
FIG. 2 is a schematic block diagram of an example combinatorial plasma chamber according to aspects of the invention; and
FIG. 3 is a schematic block diagram of an example combinatorial plasma chamber with a rotatable cylindrical target according to aspects of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will now be described in detail with reference to the drawings, which are provided as illustrative examples of the invention so as to enable those skilled in the art to practice the invention. Notably, the figures and examples below are not meant to limit the scope of the present invention to a single embodiment, but other embodiments are possible by way of interchange of some or all of the described or illustrated elements. Moreover, where certain elements of the present invention can be partially or fully implemented using known components, only those portions of such known components that are necessary for an understanding of the present invention will be described, and detailed descriptions of other portions of such known components will be omitted so as not to obscure the invention. In the present specification, an embodiment showing a singular component should not be considered limiting; rather, the invention is intended to encompass other embodiments including a plurality of the same component, and vice-versa, unless explicitly stated otherwise herein. Moreover, applicants do not intend for any term in the specification or claims to be ascribed an uncommon or special meaning unless explicitly set forth as such. Further, the present invention encompasses present and future known equivalents to the known components referred to herein by way of illustration.
In general, the present invention overcomes several of the key problems of current state-of-the-art thin film battery (TFB) technologies that preclude them from being compatible with cost-effective and high-volume manufacturing. In one embodiment, the invention provides concepts for new cathode materials and new deposition methods for improved battery performance. In another embodiment, the invention provides new deposition sources to reduce various requirements of the TFB fabrication process, and thereby increase the throughput and yield.
According to a first embodiment described herein, the present inventors leverage past studies in bulk (not thin film form) cathode materials with LiMn 2 O 4 and LiCoO 2 , wherein the Mn and Co were fractionally substituted for improved electrical and electrochemical material properties. See, for example for LiMn 2 O 4 , F. Zhang and S. Whittingham, Electrochemical and Solid-State Letters, 3 (2000) 309-311, and for LiCoO 2 , H. J. Kim et al., J. Power Sources, 159 (2006) 233-236.
More particularly, in a first embodiment, the present inventors' concept for the new cathode materials includes modifying the original material so that both the electrical and ionic conductivities are increased. This is achieved by adjusting the composition of the sputter target materials. For example, in the cathode material LiCoO 2 , the present inventors recognize that replacing some of the Co with Mg can lead to a significant increase in electrical conductivity. In addition, the lattice parameters, as well as the interstitial channels, can be expected to increase in size. The present inventors further recognize that this increase in lattice constant and channels can lead to an increase in ionic conductivity as well.
Accordingly, the target material for the cathode layer (e.g. cathode layer 106 in FIG. 1C ), according to this embodiment of the invention can be represented by:
LiM a N b Z c
Where: M is one or more elements chosen from Co, Mn, Al, Ni and V;
N is one or more substitutional elements chosen from the alkaline earth elements (e.g. Mg, Ca, Sr, Ba, and Ra); Z is one or more elements/molecules chosen from (PO 4 ), O, F, N, etc.; and a, b, c specify the relative atomic fractions of the target material.
Note that the composition of the deposited film may not be identical to that of the target material, but will be very close. The desired stoichiometry of the deposited film will be reflected primarily in the values of a and c. Some examples follow. If the desired cathode layer composition and morphology belongs to the group of LiCoO 2 and analogous materials, then the ratio of a to c will be roughly 1 to 2. If the desired cathode layer composition and morphology belongs to the group of spinel materials such as LiMn 2 O 4 , then the ratio of a to c will be roughly 2 to 4. If the desired cathode layer composition and morphology belongs to the group of LiFePO 4 and analogous materials, then the ratio of a to c will be roughly 1 to 1. Furthermore, the deposited films are not restricted to stoichiometric materials—substoichiometric/non-stoichiometric compositions may be used. Regarding the relative amount of substitutional element N, the ratio of b to a should be less than 1 to 4, in other words 0.2>{b/(a+b)}>0. Although, in preferred embodiments 0.12>{b/(a+b)}>0.05.
The substitution elements, N, preferably contribute (electrons) to the conduction bands while increasing the size of the diffusion channels. Whereas Mg and Ni have been used in past studies for bulk materials, the present inventors recognize that analogous (or perhaps better) results can be obtained with other metals of the alkaline earth column and d-orbital rows of the Periodic Table. The ultimate choice will be determined by many factors, including pertinent properties of the resulting TFBs and cost.
There are several potential benefits of using new cathode materials according to the invention. First, the increase in electrical conductivity will allow application of non-RF sputtering techniques that are capable of higher deposition rates, and further allow higher power delivery to the target as compared to undoped targets. As an example, a pulsed DC (pDC) sputtering technique can be used which exhibits higher deposition rates than the rates available with RF techniques. With a new deposition source (explained in more detail below), a significantly higher deposition rate, beyond those available using just pDC, is anticipated. Moreover, the increase in electrical and ionic conductivities of the bulk sputtering target material can lead to higher conductivities in the deposited materials. Such improved properties can allow a thicker cathode layer (versus the non-substituted cathodes) for higher charge, energy and power densities, as the effect from overall impedance increase is minimized (as compared to the non-substituted TFB). The traditional loss of energy/power density due to thickness can be seen from previous studies, wherein the thicker cathode layer leads to lower energy density at higher power application.
In order to take advantage of pDC sputtering the target needs to have a resistivity of less than 1E5 Ohm-centimeters. Utilizing a sputter target such as LiCo 1-x Mg x O 2 the deposited cathode layer has a resistivity of less than 1E1 Ohm-centimeters. This now reduces the overall impedance of the TFB, which allows greater current capability or greater cathode thickness with comparable current capability to undoped cathodes. With the anticipated increase in ionic conductivity, the effect will be accentuated further. For example, cathode layers may be at least 3 to 5 microns thick.
Another embodiment of the invention that addresses both the deposition rate and properties of the deposited film will now be described. According to one aspect of this embodiment, higher deposition rates and improved film properties are achieved by using combinatorial plasma sources. According to another aspect, the present inventors apply new deposition methods and sources, as well as methods and sources from existing Si—IC applications (e.g. U.S. Pat. No. 5,886,866 to G. Hausmann).
An example combinatorial plasma system according to an embodiment of the invention is shown schematically in FIG. 2 . The system includes a chamber 200 housing a substrate holder 202 for holding a substrate and a sputter target 204 . Pumping system 206 is connected to chamber 200 for controlling a pressure therein, and process gases 208 represents sources of gases supplied to chamber 200 used in the deposition process. According to aspects of the invention, combinatorial plasma is achieved by coupling appropriate plasma power sources 210 and 212 to both the substrate 202 and target 204 . An additional power source 214 may also be applied to the target, substrate or for transferring energy directly to the plasma, depending on the type of plasma deposition technique. Furthermore, a microwave generator 216 may provide microwave energy to a plasma within the chamber through the antenna 218 . Microwave energy may be provided to the plasma in many other ways, as is known to those skilled in the art.
Depending on the type of plasma deposition technique used, substrate power source 210 can be a DC source, a pulsed DC (pDC) source, a RF source, etc. Target power source 212 can be DC, pDC, RF, etc., and any combination thereof. Additional power source 214 can be pDC, RF, microwave, a remote plasma source, etc.
Although the above provides the range of possible power sources, it is preferred that the plasma sources be provided in the following combinations of power source to target plus power source to substrate. For cathode layer deposition: (1) pDC at the target plus RF substrate bias; (2) pDC at the target plus microwave plasma, without any substrate bias and where the microwave plasma affects both the target and the growing film; (3) pDC at the target plus microwave plasma plus RF substrate bias. Although pDC sputtering of the target is preferred when the target is sufficiently conductive, RF sputtering may also be used. For electrolyte layer deposition: (1) RF at the target plus microwave plasma enhancement; (2) RF at the target plus HF/RF substrate bias; and (3) RF at the target plus microwave plasma plus HF/RF substrate bias. The nomenclature HF is used to indicate the potential need for power sources of two different frequencies, where the frequencies are sufficiently different to avoid any interference. Although, the frequencies of the RF at the target and at the substrate may be the same providing they are locked in phase. Furthermore, the substrate itself can be biased to modulate the plasma-substrate interactions. An RF bias is preferred, although a DC bias or a pDC bias is an option.
Process conditions for deposition of cathode and electrolyte layers of the TFB according to the present invention are provided in Table I below.
TABLE I
Potential ranges of deposition process conditions are provided for both the cathode and
electrolyte layers of the TFB, according to the present invention. The power levels for pDC and
RF can be based on the target surface area, for microwave the power levels are based on the
“antenna area”, and for RF/HF bias the power levels are based on substrate surface area.
Target
Target
Plasma
Substrate
Target
Process
Chamber
pDC Power
RF Power
Microwave
RF/HF Bias
Materials
Gases
Pressure
Level
Level
Power Level
Power Level
Cathode:
Ar/O 2
1-100 mTorr
Up to 25 W/cm 2
N/A
Up to 10 W/cm 2
Up to 5 W/cm 2
LiCoO 2
RF
LiCo x Mg y O 2
Electrolyte:
N 2
1-100 mTorr
N/A
Up to 5 W/cm 2
Up to 10 W/cm 2
Up to 5 W/cm 2
Li 3 PO 4
HF
or RF
According to aspects of the invention, the combined plasma sources are expected to increase the modulation capability of the target bias and plasma density to increase the yield from the target (and thus the deposition rate), and at the same time, allow redirecting of the plasma energy to affect the depositing film. The purpose of redirecting the plasma energy to the growing film is to affect the crystallinity and surface morphology. Additionally, the redirected energy can enhance the internal microstructure and stress to contribute to improved TFB performance and stack stability.
The improved crystallinity in cathode layers deposited using the above-described combinatorial plasma deposition source will allow elimination or reduction of the need to anneal the cathode layer after deposition, which will lead to increased throughput, lower cost, and reduced complexity. If additional excitation is needed, the deposition chambers can be fitted with heating capability, either thermal or electromagnetic (EM) radiation. Additionally or alternatively, post-deposition thermal or EM radiation treatment can be performed, including microwave post and in-situ anneal. For the EM radiation treatment, a specific wavelength would be selected for layer-specific rapid thermal anneal, in situ. The point is to eliminate the time-consuming ex situ “furnace anneal” to minimize the impact on throughput and complexity.
One of the benefits of the deposition methods of the present invention, improved surface morphology, will allow improved conformal and pinhole free coverage during the key subsequent electrolyte deposition step. In fact, the suitability of the resulting surface morphology for electrolyte deposition would be a yield enhancing requirement for all processes, including the high deposition rate processes. In actual tests performed by the present inventors, a 600 nm Al-layer was formed by conventional evaporation processing, and a 600 nm Al-layer was formed by plasma activated evaporation. A microscopic comparison of the layers was performed. The Al-layer formed by conventional processing exhibited a columnar structure and a rough surface. On the other hand, the impact of additional plasma during Al film deposition according to the invention was readily apparent—the Al-layer is a denser, pinhole-free film with smooth surface morphology.
The combinatorial plasma sources, as discussed above, can also be used to enhance the deposition rate, the film density and the surface morphology of the electrolyte layer in a TFB. The higher deposition rate will increase the process throughput, while the enhanced density and surface morphology improve the TFB yield.
Further to the planar sputter target 204 shown in FIG. 2 , the sputter deposition may use single rotatable cylindrical targets 304 and dual rotatable cylindrical targets. See FIG. 3 . The configuration of rotatable cylindrical targets is well known to those skilled in the art. Supply of microwave energy to the plasma may include ECR. RF power may by supplied in CW or burst mode. Furthermore, HPPM may be utilized as a sputtering power supply.
Although the present invention has been particularly described with reference to the preferred embodiments thereof, it should be readily apparent to those of ordinary skill in the art that changes and modifications in the form and details may be made without departing from the spirit and scope of the invention. It is intended that the appended claims encompass such changes and modifications. | A method of fabricating a layer of a thin film battery comprises providing a sputtering target and depositing the layer on a substrate using a physical vapor deposition process enhanced by a combination of plasma processes. The deposition process may include: (1) generation of a plasma between the target and the substrate; (2) sputtering the target; (3) supplying microwave energy to the plasma; and (4) applying radio frequency power to the substrate. A sputtering target for a thin film battery cathode layer has an average composition of LiM a N b Z c , wherein 0.20>{b/(a+b)}>0 and the ratio of a to c is approximately equal to the stoichiometric ratio of a desired crystalline structure of the cathode layer, N is an alkaline earth element, M is selected from the group consisting of Co, Mn, Al, Ni and V, and Z is selected from the group consisting of (PO 4 ), O, F and N. | 7 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is based on and claims domestic priority benefits under 35 USC §119(e) from U.S. Provisional Application Ser. No. 60/907,774 filed on Apr. 17, 2007, the entire content of which is expressly incorporated hereinto by reference.
FIELD OF THE INVENTION
[0002] The present invention relates generally to elastic composite yarns having an elastic core filament and a fibrous sheath covering the core filament. In especially preferred forms, the present invention is embodied in ring spun yarns having an elastic core which may be woven into fabrics exhibiting excellent recovery characteristics.
BACKGROUND AND SUMMARY OF THE INVENTION
A. Definitions
[0003] As used herein and in the accompanying claims, the terms below are intended to have the following definitions:
[0004] “Filament” means a fibrous strand of extreme or indefinite length.
[0005] “Fiber” means a fibrous strand of definite or short length, such as a staple fiber.
[0006] “Yarn” means a collection of numerous filaments or fibers which may or may not be textured, spun, twisted or laid together.
[0007] “Sliver” means a continuous fibrous strand of loosely assembled staple fibers without twist.
[0008] “Roving” means a strand of staple fibers in an intermediate state between sliver and yarn. According to the present invention, the purpose of a roving is to provide a package from which a continuous stream of staple fibers is fed into the twist zone for each ring spinning spindle.
[0009] “Spinning” means the formation of a yarn by a combination of drafting and twisting or prepared strands of staple fibers, such as rovings.
[0010] “Core spinning” means introducing a filamentary strand into a stream of staple fibers so that the staple fibers of the resulting core spun yarn more or less cover the filamentary strand.
[0011] “Woven fabric” means a fabric composed of two sets of yarns, warp and filling, and formed by interlacing (weaving) two or more warp yarns and filling yarns in a particular weave pattern (e.g., plain weave, twill weave and satin weave). Thus, during weaving the warp and fill yarns will be interlaced so as to cross each other at right angles to produce the woven fabric having the desired weave pattern.
[0012] “Draft ratio” is the ratio between the length of a stock filamentary strand from a package thereof which fed into a spinning machine to the length of the filamentary strand delivered from the spinning machine. A draft ratio of greater than 1.0 is thus a measure of the reduction in bulk and weight of the stock filamentary strand.
[0013] “Package length” is the length of a tensioned filament or yarn forming a package of the same.
[0014] “Elastic recovery” means that a filament or fabric is capable of recovery to its original length after deformation from elongation or tension stress.
[0015] “Percent elastic recovery” is a percentage ratio of the length of a filament or fabric following release of elongation or tension stress to the length of the filament or fabric prior to being subject to elongation or tension stress. A high percent elastic recovery therefore means that the filament or fabric is capable of returning substantially to its original pre-stressed length. Conversely, a low percent elastic recovery means that the filament or fabric is incapable of returning substantially to its original pre-stressed length. The percent elastic recovery of fabrics is tested according to ASTM D3107 (the entire content of which is expressly incorporated hereinto by reference).
[0016] An “elastic filament” means a filament that is capable of stretching at least about 2 times its package length and having at least about 90% elastic recovery up to 100% elastic recovery. Thus, the greater that a yarn of fabric which includes an elastic filament is stretched, the greater the retraction forces of such yarns and fabrics.
[0017] An “inelastic filament” means a filament that is not capable of being stretched beyond its maximum tensioned length without some permanent deformation. Inelastic filaments are therefore capable of being stretched only about 1.1 times their tensioned (package) length. However, due to texturing (crimping), an inelastic filament may exhibit substantial retraction force and thereby exhibit substantial percent elastic recovery.
II. BACKGROUND OF THE INVENTION
[0018] Composite elastic yarns are in and of themselves well known as evidenced, for example, by U.S. Pat. Nos. 4,470,250; 4,998,403; 5,560,192; 6,460,322 and 7,134,265. 1 In general, conventional composite elastic yarns comprise one or more elastic filaments as a core covered by a relatively inelastic fibrous or filamentary sheath. Such elastic composite yarns find a variety of useful applications, including as component filaments for making stretchable textile fabrics (see, e.g., U.S. Pat. No. 5,478,514). Composite yarns with relatively high strength inelastic filaments as a core surrounded by a sheath of other filamentary material are also known, for example, from U.S. Pat. No. 5,735,110. 1 The entire contents of each of these cited U.S. patents as well as each U.S. patent cited hereinafter are expressly incorporated into this document by reference as if each one was set forth in its entirety herein.
[0019] Woven fabrics made of such yarns, in particular ring spun yarns with an elastic core can be used to make woven stretch fabrics. Typically these fabrics have an elongation of 15 to 40% usually in the weft direction only, but sometimes also in the warp directions. A typical problem with these fabrics is that the recovery characteristics can be poor, usually on the order of as low as 90% (ASTM D3107).
[0020] Fabrics made with yarns having “inelastic filaments” with retraction power due to artificial crimp (textured or self textured as in elasterell-p, PTT/PET bi-component fibers) generally have low elongation in the range of 10 to 20%. In general, these fabrics have excellent recovery characteristics when tested using ASTM D3107.
III. SUMMARY OF THE INVENTION
[0021] It would therefore be highly desirable if the excellent recovery properties of inelastic filaments could be combined with the excellent elongation or stretch properties of elastic filaments in the same ring spun core yarn. If such a ring spun core yarn were possible, then several problems would be solved. For example, fabrics made from such ring spun core yarns would exhibit both good stretch and excellent recovery according to ASTM D3107, could be heat-set with better control of stretch properties, and could be made into garments and subsequently resin treated with much better recovery remaining after the treatment. It is towards fulfilling such a need that the present invention is directed.
[0022] Broadly, the present invention is embodied in ring-spun yarns which satisfy the need in this art noted above. In accordance with one preferred embodiment of the present invention, a composite yarn is provided which includes a filamentary core comprised of an elastic performance filament and an inelastic control filament and a fibrous sheath surrounding the filamentary core, preferably substantially along the entire length thereof. The fibrous sheath is preferably ring-spun from a roving of staple fibers and thereby forms an incoherent mass of entangled spun stable fibers as a sheath surrounding the elastic and inelastic filaments.
[0023] According to some preferred embodiments of the invention, an elastic composite yarn is provided wherein at least one elastic performance filament comprises a spandex and/or a lastol filament, and wherein at least one inelastic control filament comprises a filament formed of a polymer of copolymer of a polyamide, a polyester, a polyolefin and mixtures thereof. Preferably, the fibrous sheath comprises synthetic and/or natural staple fibers. In especially preferred embodiments, the fibrous sheath comprises staple cotton fibers.
[0024] The elastic composite fibers of the present invention find particular utility as a component part of a textile fabric. Thus, according to some embodiments of the present invention, the composite elastic filaments will be woven into a textile fabric, preferably a denim fabric.
[0025] The composite elastic yarn may be made by providing a filamentary core comprised of at least one elastic performance filament and at least one inelastic control filament, wherein the at least one elastic performance filament has a draft ratio which is at least two times, preferably at least tree time, the draft ratio of the at least one inelastic control filament; and thereafter spinning a fibrous sheath around the filamentary core. The filamentary core may be supplied to the spinning section as a preformed unit, for example by joining the elastic and inelastic fibers in advance and providing such a filamentary core stock on a package to be supplied to the spinning section. Alternatively, the filamentary core may be formed immediately in advance of the spinning section by unwinding the elastic performance filament and the inelastic control filament from respective separate supply packages, and bringing filaments together prior to spinning of the fibrous sheath thereabout. The elastic performance filament and the inelastic control filament may thus be acted upon by respective draw ratio controllers so as to achieve the desired draw ration differential therebetween as briefly noted above.
[0026] These and other aspects and advantages will become more apparent after careful consideration is given to the following detailed description of the preferred exemplary embodiments thereof.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
[0027] Reference will hereinafter be made to the accompanying drawings, wherein like reference numerals throughout the various FIGURES denote like structural elements, and wherein;
[0028] FIG. 1 is a schematic representation of a yarn package of a composite yarn in accordance with the present invention;
[0029] FIG. 2 is a greatly enlarged schematic view of a section of the composite yarn shown in FIG. 1 in a relaxed (non-tensioned) state;
[0030] FIG. 3 is a greatly enlarged schematic view of a section of the composite yarn similar to FIG. 2 but shown in a tensioned state; and
[0031] FIG. 4 is a schematic representation of a process and apparatus for making the composite yarn in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0032] As depicted in FIGS. 1-31 the present invention is most preferably embodied in a composite yarn 10 which may be wound around a bobbin BC so as to form a yarn package YP thereof. The yarn package YP may therefore be employed in downstream processing to form a textile fabric, preferably a woven fabric, according to techniques well known to those in this art.
[0033] The composite yarn 10 according to the present invention will necessarily include a filamentary core 10 - 1 comprised of at least an elastic performance filament 12 and an inelastic control filament 14 . The filamentary core 10 - 1 is surrounded, preferably along the entirety of its length by a fibrous sheath 10 - 2 comprised of a mass of spun staple fibers 16 .
[0034] Although not shown in FIGS. 2-3 , the filamentary core 10 - 1 may comprise additional filaments deemed desirable for the particular end use application contemplated for the composite filament 10 . Furthermore, filaments 12 and 14 are depicted in FIGS. 2-3 as monofilaments for ease of illustration only. Thus, the elastic performance filament 12 and/or the inelastic control filament 14 may be comprised of multiple filaments. In one especially preferred embodiment of the present invention, the elastic performance filament is a single filament while the inelastic control filament is a multifilament. More specifically, the preferred elastic performance filament may advantageously be formed of multiple elastic monofilaments which are coalesced with one another so as to in essence form a single filament. On the other hand, the inelastic control filament is formed of multiple monofilaments and/or multiple filaments of spun staple fibers.
[0035] As depicted schematically in accompanying FIG. 2 , when the composite yarn 10 is in a non-tensioned state, the inelastic control filament 14 is twisted relatively loosely around the elastic performance filament 12 . Such relative loose twisting of the inelastic control filament 14 about the elastic performance filament 12 thus allows the elastic filament 12 to be extensible under tension until a point is reached whereby the inelastic control filament 14 reaches its extension limit (i.e., a point whereby the relative looseness of the inelastic filament has been removed along with any extensibility permitted by filament texturing (crimping) that may be present such that any further tensioning would result in permanent deformation or breakage). Such a tensioned state is depicted schematically in accompanying FIG. 3 .
[0036] It will be understood that, since the fibrous sheath 10 - 2 is comprised of an incoherent mass of entangled, randomly oriented spun staple fibers, it will permit the extension of the elastic performance filament 12 to occur up to the limit of the inelastic control filament 14 without physical separation. Furthermore, the fibrous sheath itself serves to limit the extensibility of the elastic performance filament 12 , albeit to a much lesser extent as compared to the inelastic control filament 14 . Thus, throughout repeated tensioning and relaxation cycles, the fibrous sheath 10 - 2 will continue to visibly hide the filamentary core 10 - 1 .
[0037] Virtually any commercially available elastomeric filament may be employed satisfactorily as the elastic performance filament 12 in accordance with the present invention. Preferred are elastic filaments made from spandex or lastol polymers. As is well known, spandex is a synthetic filament formed of a long chain synthetic elastomer comprised of at least 85% by weight of a segmented polyurethane. The polyurethane segments of spandex are typically interspersed with relatively soft segments of polyethers, polyesters, polycarbonates or the like. Lastol is an elastic polyolefin having a cross-linked polymer network structure, as disclosed more fully in U.S. Pat. Nos. 6,500,540 and 6,709,742. Other suitable elastomeric polyolefins may also be employed in the practice of the present invention, including homogeneously branched linear or substantially linear ethylene/α-olefin interpolymers, e.g. as disclosed in U.S. Pat. Nos. 5,272,236, 5,278,272, 5,322,728, 5,380,810, 5,472,775, 5,645,542, 6,140,442, and 6,225,243.
[0038] A particularly preferred spandex filament is commercially available from Invista (formerly DuPont Textiles & Interiors) under the trade name LYCRA® having deniers of about 40 or about 70. A preferred lastol filament is commercially available from Dow Fiber Solutions under the tradename XLA™ having deniers of about 70, 105, or 140.
[0039] The inelastic control filament may be virtually any inelastic filament known to those in the art. Suitable inelastic control filaments include filaments formed of virtually any fiber-forming polymers such as polyamides (e.g., nylon 6, nylon 6,6, nylon 6,12 and the like), polyesters, polyolefins (e.g., polypropylene, polyethylene) and the like, as well as mixtures and copolymers of the same. Presently preferred for use as the inelastic control filament are polyester filaments, such as those commercially available from Unifi, Inc. in 1/70/34 stretch textured polyester or 1/70/34 in set textured polyester.
[0040] The relative denier of the elastic performance filament 12 and the inelastic control filament 14 may be substantially the same or substantially different. In this regard, the denier of the elastic performance filament 12 may vary widely from about 10 to about 140, preferably between about 40 to about 70. After the proper draft ratio is applied the denier of the elastic filament inside a tensioned yarn would be about 5 to 70, preferably between 10 and 25. The denier of the inelastic control filament 14 may vary widely from about 40 to about 150, preferably between about 70 to about 140. In one particularly preferred embodiment of the invention, the denier of the elastic performance filament 12 and the inelastic control filament 14 is each about 70.
[0041] As noted briefly above, the fibrous sheath 10 - 2 is formed from a relatively dense mass of randomly oriented entangled spun synthetic staple fibers (e.g., polyamides, polyesters and the like) or spun natural staple fibers (e.g., cotton). In especially preferred embodiments, the fibrous sheath 10 - 2 is formed of spun cotton fibers. The staple fiber length is not critical. Typical staple fiber lengths of substantially less than one inch to several inches may thus be used.
[0042] The composite yarn 10 may be made by virtually any staple fiber spinning process known to those in this art, including core spinning, ring spinning and the like. Most preferably, however, the composite yarn 10 is made by a ring spinning system 20 depicted schematically in accompanying FIG. 4 . As shown, the preferred ring spinning system 20 includes a ring-spinning section 22 . The elastic performance filament 12 and the inelastic control filament 14 forming the filamentary core 10 - 1 are removed from a creel-mounted supply package 12 a , 14 a , respectively, and brought together at a merger ring 24 prior to being fed to the ring-spinning section 22 . A roving 26 of the staple fibers to be spun into the fibrous sheath 10 - 2 is similarly removed from a creel mounted supply package 26 a and directed to the ring-spinning section 22 .
[0043] The size of the roving is not critical to the successful practice of the present invention. Thus, rovings having an equivalent cotton hank yarn count of between about 0.35 to about 1.00, preferably between about 0.50 to about 0.60 may be satisfactorily utilized. In one preferred embodiment of the invention, a roving of cotton staple fibers is employed having a cotton hank yarn count of 0.50 and is suitably spun with the elastic and inelastic core filaments to achieve a resulting equivalent cotton yarn count of 14/1. Filamentary cores totaling about 90 denier can be suitably spun with a fibrous sheath to equivalent cotton yarn counts ranging from 20/1 to 8/1, while filamentary cores totally 170 denier can be suitably spun with a fibrous sheath to yarn counts ranging from 12/1 to 6/1.
[0044] Individual independently controllable draft ratio controllers 28 , 30 and 32 are provided for each of the filaments 12 and 14 , and the roving 26 . According to the present invention the draft ratio controllers 30 and 32 are set so as to feed the inelastic control filament 14 and the roving 26 of staple fibers to the ring-spinning section 22 at a draft ratio of about 1.0 (+/−about 0.10, and usually +/−about 0.05). The draft ratio controller 28 on the other hand is set so as to supply the elastic performance filament 12 to the ring-spinning section 22 at a draft ratio of at least about 2.0, and preferably at least about 3.0. Thus, when joined with the inelastic control filament 14 , the elastic performance filament 12 will be at a draft ratio which is at least two times, preferably at least three times, the draft ratio of the inelastic control filament 14 . The elastic performance filament 12 will thereby be under tension to an extent that it is extended (stretched) about 200%, and preferably about 300% as compared to its state on the package 12 a . On the other hand, as compared to its state on the package 14 a , the inelastic control filament 14 will be essentially unextended (unstretched).
[0045] The ring-spinning section 22 thus forms the fibrous sheath 10 - 2 around the filamentary core 10 - 1 using ring-spinning techniques which are per se known in the art. Such ring-spinning techniques also serve to relatively twist the inelastic control filament 14 about the elastic performance filament. Thus, the ring-spinning of the fibrous sheath 10 - 2 from the roving 26 of staple fibers and the draft ratio differential as between the elastic performance filament 12 on the one hand and the inelastic control filament on the other hand serve to achieve an elastic composite yarn 10 as has been described previously. The composite yarn may thus be directed to a traveler ring 34 and wound about the bobbin BC to form the yarn package YP.
[0046] The composite yarn 10 according to the present invention may be used as a warp and/or filling yarn to form woven fabrics having excellent elastic recovery characteristics. Specifically, according to the present invention, woven fabrics in which the composite yarn 10 is woven as a warp and/or filling yarn in a plain weave, twill weave and/or satin weave pattern, will exhibit a stretch of at least about 15% or greater, more at least about 18% or greater, most preferably at least about 20% or greater Such fabrics in accordance with the present invention will also preferably exhibit a percent elastic recovery according to ASTM D3107 of at least about 95.0%, more preferably at least about 96.0% up to and including 100%.
[0047] The present invention will be further understood as careful consideration is given to the following non-limiting Examples thereof.
EXAMPLES
Example 1
[0048] A composite core yarn was made of 70 denier spandex filament commercially obtained from RadicciSpandex Corporation drafted at 3.1 and a 70 denier stretch textured polyester filament (Jan. 70, 1968) commercially obtained from Unifi, Inc. drafted at 1.0. The composite yarn was spun on a Marzoli ring spinning machine equipped with an extra hanger and tension controllers for the composite core yarn. A hank roving size of 0.50 was used and drafted sufficiently to yield a total yarn count of 14/1. The resulting composite yarn was woven on an X-3 weaving machine to create a vintage selvage denim with stretch. The reed density of 14.25 (57 ends in reed) was used instead of the normal 16.5. The resulting fabric was desized, mercerized, and heat set to a width of 30 inches on a Monforts tenter range. The resulting denim fabric stretch was 18% and the elastic recovery was 96.9% according to ASTM D3107.
[0049] A comparison fabric was made using a 14/1 regular core spun yarn containing only 40 denier spandex. The elastic recovery was only 95.5% when tested according to ASTM D3107.
Example 2
[0050] A denim fabric was woven using yarns of Example 1 as weft on a Sulzer rapier wide loom. This denim was made with one pick of the 14/1 multi-core yarn followed by one pick of 14/1 normal core spun with 40 denier spandex. This denim was made with 16.0 reed density (64 ends in reed). The fabric was desized and mercerized but not heat set. The resulting fabric had 29% stretch and a recovery of 96.0% based on ASTM D3107.
[0051] A comparison fabric was made using all picks of 14/1 normal core spun with 40 denier spandex. The comparison fabric had 25% stretch but only 95.3% recovery when tested according to ASTM 3107.
Example 3
[0052] A 3/1 twill bi-directional stretch denim made with warp and weft comprised of multi-core yarns made with the apparatus described in Example 1. The core consisted of a 1/70/34 textured polyester continuous filament strand drafted at 1.00 to 1.02, and a 40 denier spandex elastomeric (RadicciSpandex Corporation) drafted at 3.1. The wrapping or sheath of the core spun yarn consisted of cotton fibers sufficient to provide a total weight of 7.5/1 Ne in warp and 14/1 Ne in weft. The warp yarn was woven at low density and the fill yarn was woven at 48 weft yarns per inch. After mercerization, heat setting, and finishing the final yarn density was 64×52 giving a fabric weight of 11.25 oz. per square yard. The stretch after heat setting was 11% in warp direction with 97% average recovery. The stretch in the weft direction was 22% with a recovery of 96%.
Example 4
[0053] A 3/1 twill bi-directional stretch denim was made with warp and weft comprised of multi-core yarns made with the apparatus described in Example 1. The core consisted of a 1/70/34 textured polyester continuous filament strand drafted at 1.00 to 1.02, a 75 denier lastol elastomeric (Dow Chemical, XLA™) drafted at 3.8. The wrapping or sheath of the core spun yarn consisted of cotton fibers sufficient to provide a total weight of 7.5/1 Ne in warp and 11.25/1 Ne in weft. The warp yarn was woven at low density and the fill yarn was woven at 42 weft yarns per inch. After mercerization, heat setting, and finishing the final yarn density was 68×47 giving a fabric weight of 11.50 oz. per square yard. The stretch after finishing was 112.5% in warp direction with 97% average recovery. The stretch in the weft direction was 19% with a recovery of 96%.
Example 5
[0054] A 3/1 twill weft stretch denim was made with an all cotton warp having an average yarn number of 9.13 Ne at a density of 57 ends per inch in the loom reed. The weft was comprised of a multi-core yarn made with the apparatus described in Example 1. The core consisted of a 1/70/34 textured polyester continuous filament strand drafted at 1.00 to 1.02, and a 40 denier spandex elastomeric (RadicciSpandex Corporation) drafted at 3.1. The wrapping or sheath of the core spun yarn consisted of cotton fibers sufficient to make a total weight of 14/1 Ne. This yarn was woven at the rate of 45 weft yarns per inch. After mercerization, heat setting, and finishing the final yarn density was 75×48.5 giving a fabric weight of 9.75 oz. per square yard. The stretch after heat setting was 17% with 96.8 average recovery. The overall blend level for the fabric is 93% cotton/6% polyester/1% spandex.
Example 6
[0055] A 3/1 twill weft stretch denim was made with an all cotton warp having an average yarn number of 9.13 Ne at a density of 57 ends per inch in the loom reed. The weft was comprised of a multi-core yarn made with the apparatus described in Example 1. The core consisted of a 1/70/34 textured polyester continuous filament strand drafted at 1.00 to 1.02, and a 40 denier spandex elastomeric (RadicciSpandex Corporation) drafted at 3.1. The wrapping or sheath of the core spun yarn consisted of cotton fibers sufficient to make a total weight of 14/1 Ne. This yarn was woven at the rate of 50 weft yarns per inch. After mercerization and finishing the final yarn density was 77×55.5 giving a fabric weight of 10.5 oz. per square yard. The stretch was 26% with 96% average recovery. The overall blend level for the fabric was 92% cotton/7% polyester/1% spandex.
Example 7
[0056] A 3/1 twill weft stretch denim was made with an all cotton warp having an average yarn number of 9.13 Ne at a density of 57 ends per inch in the loom reed. The weft was comprised of a multi-core yarn made with the apparatus described in Example 1. The core consisted of a 1/70/34 textured polyester continuous filament strand drafted at 1.00 to 1.02, and a 75 denier lastol elastomeric (Dow Chemical, XLA™) drafted at 4.0. The wrapping or sheath of the core spun yarn consisted of cotton fibers sufficient to make a total weight of 11.25/1 Ne. This yarn was woven at the rate of 46 weft yarns per inch. After mercerization and finishing the final yarn density was approximately 75×51 giving a fabric weight of 11.5 oz. per square yard. The stretch was 17% with 96% average recovery. The overall blend level for the fabric is 93% cotton/6% polyester/1% lastol.
[0057] While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | Composite yarns have a filamentary core provided with at least one elastic performance filament and at least one inelastic control filament. A fibrous sheath, preferably formed from spun staple fibers, surrounds the filamentary core, preferably substantially along the entire length thereof. The at least one elastic performance filament most preferably includes a spandex and/or a lastol filament. The at least one inelastic control filament is most preferably formed of a textured polymer or copolymer of a polyamide, a polyester, a polyolefin and mixtures thereof. Preferably, the fibrous sheath is formed of synthetic and/or natural staple fibers, most preferably staple cotton fibers. The elastic composite fibers find particular utility as a component part of a woven textile fabric, especially as a stretch denim fabric, which exhibits advantageous elastic recovery of at least about 95.0% (ASTM D3107). | 3 |
BACKGROUND OF THE INVENTION
The invention relates to new compositions of alpha-olefin homo- or copolymer as well as to the preparation method thereof. The invention further relates to the use of the alpha-olefin homo- or copolymer composition i.a. in end applications, wherein any taste and/or odor of the polymers are undesired.
BACKGROUND ART
It is well known that a polymer composition obtained from a polymerisation reaction comprises a mixture of polymer molecules with varying chain lengths having different molecular weights (Mw). It is also known that the molecular weight distribution (MWD) of a composition may be tailored to be broad or narrow and the profile may have e.g. one or more maximas.
The MWD curve has typically a low molecular weight (LMW) “tail” comprising very short chain molecules and a high molecular weight (HMW) “tail” comprising very long chain molecules at both end of the curve. The LMW tail of the polymer composition comprises i.a. oligomers. The oligomers are known to be volatile.
The oligomers thus belong to a generally known group of compounds, namely volatiles, which contribute to the undesired taste and/or odour of the final polymer product. The other volatile compounds include e.g. solvents and/or catalyst components which may be used during the polymerisation step, as well as compounds that are optionally incorporated to the polymer composition during or after the polymerisation step, such as some conventional post-reactor additives incorporated to the polymer powder obtained from the polymerisation reactor. Volatiles may also include any degradation products of the polymer or said added compounds.
Such volatiles contribute also to the so called “fogging” problem, i.e. these compounds tend to separate, e.g. evaporate, from the polymer material and cause fogging on the surrounding surfaces e.g. on car windows. Thus in certain end applications the presence of the very LMW tail, particularly of the oligomers, in the polymer composition may not be desirable.
In prior art e.g. WO 03000752 discloses polypropylene composition for expanded granules based on semi-crystalline polypropylene comprising less than 0.025 part by weight of volatile compounds per 100 parts by weight of the polymer. Volatiles are stated to comprise mainly the following components: 1. volatile hydrocarbons, i.e. oligomers of propylene polymer formed during the polymerisation reaction, 2. polymer additive(s) and/or 3. degradation products thereof. As the polymer additives, sterically hindered phenol or organic phosphate are mentioned.
In recent years e.g. polypropylene products have been produced commercially with the so called 4 th generation high yield Zieglar Natta catalysts. These conventional catalysts comprise typically TiCl 4 and internal donors (e.g. ester of carboxylic acids) which are supported on a separately formed MgCl 2 based carrier. Such catalyst are widely described in the literature and e.g. in EP395083 of Montell North America, EP86472 of Montedison Spa, EP491566 of Borealis and EP856390 of Chisso Corp. Polymers, produced with these catalysts have typically a high oligomer content.
JP-A-11-323071 discloses a polypropylene composition comprising 3500 ppm oligomers or less. EP 0 799 839 A2 discloses the use of visbreaking to reduce the oligomer content of a polymer composition. EP, 1 273 595 A2 and EP 1 403 292 A2 disclose catalysts for olefin polymerisation. No information regarding oligomer content or MWD of the produced polymers is disclosed.
There is a continuous need for polymer materials which fulfil the increasing environmental and customer requirements in many end application areas of polymer materials, such as packaging, including food and medical packaging (e.g. mono- and multilayered coatings and films or moulded articles), fiber, pipe and automobile industry, without limiting to these.
SUMMARY OF THE INVENTION
The object of the present invention is to provide further alpha-olefin homo- or copolymer compositions for extending the end application window of polymers. Particularly, further alpha-olefin polymers are provided which are highly suitable for end applications, wherein at least one of the properties of taste, odour and fogging are undesired.
THE PRESENT INVENTION
The invention is directed to a new alpha-olefin homo- or copolymer composition which comprises a markedly reduced fraction of alpha-olefin oligomers over the prior art alpha-olefin compositions.
Accordingly, an alpha-olefin homo- or copolymer composition comprising at least one (i) alpha-olefin homo- or copolymer component is provided, whereby
(a) the alpha-olefin homo- or copolymer composition comprises C6-C15-oligomers of alpha-olefin in an amount which satisfies the following equitation (1):
“oligomer content”≦ e [3.5+(0.504·ln(MFR 2 ))] (1)
wherein
“oligomer content” is the amount, in ppm, of alpha-olefin C6-C15-oligomer and
“MFR 2 ” is the MFR 2 value of the alpha-olefin homo- or copolymer composition as determined from the alpha-olefin composition, and
(b) MFR 2 of said composition is at least 0.001 g/10 min.
“Alpha-olefin homo- or copolymer composition” of the invention is referred herein as “polymer composition” and includes herein homopolymers of alpha-olefins and copolymers of alpha-olefins together with one or more comonomers, such as another alpha-olefin(s). Alfa-olefins are understood herein to include ethylene and higher alpha-olefins, e.g. C3-C12-alpha-olefins, such as C3-C10-alpha-olefins. The higher alpha-olefins may be linear, branched, aliphatic cyclic or aromatic cyclic alpha-olefins.
In equitation (1) “e” and “ln” have their generally known meanings, i.e. “e”≈2,718 and “ln” means the natural logarithm.
The invention includes any polymer composition, wherein the value of alpha-olefin C6-C15-oligomer measured from said composition equals or is less than “oligomer content”-value obtained from equitation (1) when using the MFR 2 value measured from said polymer composition.
As to the definitions and measurements of C6-C15-oligomer content and MFR 2 : The alpha-olefin C6-C15-oligomer means the alpha-olefin oligomer fraction with oligomers containing 6 to 15 carbon atoms. The C6-C15-oligomer content is preferably measured using the determination method described later below under “Definitions and Determination methods”. The parameter ppm refers to parts per million by weight. The MFR 2 refers to the melt flow rate of the polymer composition determined in a manner known in the art. Accordingly, the MFR 2 value of propylene (PP) composition is preferably determined according to ISO 1133 at 230° C., using 2.16 kg load and MFR 2 of ethylene (PE) composition using e.g. 1133 (190° C., 2.16 kg load).
Oligomers as described herein are thus products originating from the polymerisation of monomers of the alpha-olefin homo- or copolymer of the invention.
Typically, said oligomers originate from the low Mw tail of the polymer composition produced during the polymerisation process.
The present low amount of C6-C15-oligomers is beneficial e.g. for many demanding end applications of polymers. Moreover, the low level of C6-C15-oligomers indicates also markedly reduced levels of the total oligomers, e.g. of up to C39 or higher oligomers, present in the polymer composition.
The decreased C6-C15-oligomer fraction as defined above and determinable e.g. as defined herein below can reduce or prevent the above mentioned taste, odour problems and fogging of volatiles at levels that are very feasible in many end applications. Thus any further treatments of polymer composition for removing the volatiles can be completely avoided or in such treatment steps, if needed, markedly milder conditions and/or shorter treatment times over the prior art treatments can be used. The risk of deteriorating and/or changing the originally produced composition due to such removal treatments can therefore be minimised.
According to one preferable embodiment, the polymer composition of the invention is so called reactor-made polymer composition. It is very advantageous that a reactor-made polymer composition can satisfy the equitation (1) as is the case in this embodiment.
“Reactor-made polymer composition” means herein the reaction product which is obtained from a polymerisation reaction of the alpha-olefin monomers, optionally together with one or more comonomers. Accordingly, “reactor-made polymer composition” refers to the polymerisation product as obtained from a polymerisation step, i.e. it has not been subjected to any post reactor treatments, e.g. chemical treatments, such as visbreaking with organic peroxides, which are conventionally used to modify further the MFR of the polymer product, or treatments which would modify the oligomer content or MFR of the composition. Reactor-made polymer composition is sometimes referred also as reactor powder. Naturally, the reactor-made composition of the invention can further be subjected to such treatments, if desired.
The oligomer content as referred to in the present application, in particular for the reactor-made products, is the oligomer content as obtained after polymerisation and before employing usual process steps for reducing the oligomer content, such as degassing, although the present invention does not exclude the use of such treatments, including degassing, for further reducing the oligomer content.
The reactor-made polymer compositions as envisaged by the present invention comprise polymer compositions being the product of a singe stage polymerisation process as well as multi stage polymerisation processes, including polymerisation sequences comprising different types of polymerisation reactors and/or conditions, as explained in further detail below under the heading “Polymerisation process”. The embodiments described there in connection with the polymerisation process apply also to the reactor-made polymer compositions as disclosed herein.
In this preferable embodiment, both determinations of said polymer composition, i.e. the determination of the MFR 2 value of the polymer composition used in the equitation (1) to calculate the upper limit of the C6-C15-oligomer content and the determination of the actual oligomer content of the composition, are analysed from the reactor-made polymer composition (reactor powder) as such before any optional subsequent post-reactor treatment thereof.
The below given embodiment describing propylene polymer compositions preferably defines a propylene homopolymer composition, but the embodiment disclosed likewise also is applicable for other propylene polymers, including in particular propylene copolymers with ethylene.
In a preferable embodiment, the polymer composition is a propylene homo- or copolymer which is referred herein as PP composition. Accordingly, the propylene homo- or copolymer composition comprises at least one (i) propylene homo- or copolymer component, whereby
(a) the propylene homo- or copolymer composition comprises C6-C15-oligomers of propylene in an amount which satisfies the following equitation (1′):
“oligomer content”≦ e [3.5+(0.504·ln(MFR 2 ))] (1′)
wherein
“oligomer content” is the amount, in ppm, of propylene C6-C15-oligomer and “MFR 2 ” is the MFR 2 value of the propylene homo- or copolymer composition as determined from the PP composition, and (b) MFR 2 of said composition is at least 0.001 g/10 min.
Recently, the trend has been towards polymer materials with higher melt flow rate (MFR). Higher MFR means better processability of the polymer material i.a. due to good flowability. Thus faster through put of the process lines for producing end application articles from the polymer, and thus cost savings, can be achieved. It is well known in the art that the higher the MFR the higher the content of the LMW component of the polymer. Accordingly, also the oligomer content in polymer composition increases with increasing MFR. Therefore polymers with high MFR, but still low oligomer content are becoming increasingly important. Embodiments of the polymer composition of the invention, wherein the MFR 2 of the composition is high, are thus very feasible material for such end applications.
The oligomer content of the composition of the invention is decreased both in case of a polymer compositions with high melt flow rate and with low melt flow rate over the prior art compositions with corresponding MFR 2 .
In the following some preferable subranges of the oligomer content of the composition are given. It is evident that all the below embodiments (subranges) may equally be satisfactory and depend i.a. on the demands of the end application.
Thus in one embodiment (a) the polymer composition corresponds to the following equitation (1a):
“oligomer content”≦ e [3.3+(0.504·ln(MFR 2 ))] (1a),
wherein “oligomer content” and MFR 2 are as defined above.
In another embodiment (b) the polymer composition corresponds to the following equitation (1b):
“oligomer content”≦ e [2.8+(0.504·ln(MFR 2 ))] (1b),
wherein “oligomer content” and MFR 2 are as defined above.
In some embodiments even lower oligomer contents are desired for a polymer composition with a certain MFR 2 . In these embodiments (c) the oligomer content may even correspond the equitation (1c)
“oligomer content”≦ e [2.7+(0.504·ln(MFR 2 ))] (1c),
wherein “oligomer content” and MFR 2 are as defined above.
Also the MFR 2 value of the polymer composition may vary depending on the desired end use application of the composition. Again it is evident that all the below embodiments (subranges) may equally be satisfactory and the choice depends i.a. on the end application which determines the MFR range usable in that application. The polymer composition may be selected from any of the below embodiments alone or in any combinations thereof:
embodiment (i) MFR 2 of not more than 1000 g/10 min, or embodiment (ii) MFR 2 of not more than 100 g/10 min, or embodiment (iii) MFR 2 of not more than 10 g/10 min, embodiment (iv) MFR 2 of 1 g/10 min or lower.
The MFR 2 of the polymer composition is preferably at least 0.01 g/10 min, more preferably at least 0.1 g/10 min.
In further embodiment (v) the polymer composition with a MFR 2 of between 50 and 500 g/10 min can be advantageous for the desired end application of the composition.
The polymer composition of the invention is preferably a homo- or copolymer of ethylene or propylene.
The invention is further directed to an alpha-olefin composition which is selected from one or more of (P1) to (P7):
(P1) composition having a MFR 2 of not more than 1000 g/10 min and an oligomer content of less than 100 ppm, preferably less than 900 ppm, (P2) composition having a MFR 2 of not more than 500 g/10 min and an oligomer content of less than 760 ppm, preferably less than 630 ppm, (P3) composition having a MFR 2 of not more than 100 g/10 min and an oligomer content of less than 340 ppm, preferably less than 280 ppm, (P4) composition having a MFR 2 of not more than 50 g/10 min and an oligomer content of less than 240 ppm, preferably less than 200 ppm, (P5) composition having a MFR 2 of not more than 10 g/10 min and an oligomer content of less than 110 ppm, preferably less than 90 ppm, (P6) composition having a MFR 2 of not more than 1 g/10 min and an oligomer content of less than 35 ppm, preferably less than 30 ppm, and (P7) composition having a MFR 2 of not more than 0.1 g/10 min and an oligomer content of less than 10 ppm, preferably less than 8 ppm.
For the reasons already given above each of the combination are equally preferable. Moreover, any of these limits can be used to form further embodiments of subranges with lower and upper limits. These further embodiments include without limiting e.g. a polymer composition having MFR 2 and oligomer content which is between the limits given for (P2) and (P4), i.e. MFR 2 between the range of 50 g/10 min to 500 g/10 min and the C6-C15-oligomer content between the range of 240 ppm to 760 ppm.
The compositions (P1) to (P7) covered by the present invention are thus independent from the composition satisfying the equitation (1) and any subgroups given above. However, as one preferable embodiment of the composition of (P1) to (P7), the composition of (P1) to (P7) also fulfil the equitation (1) and optionally may be combined with any of the above subgroup embodiments defined for the composition of equitation (1). Furthermore, the composition of (P1) to (P2) is suitably a PE or PP composition, preferably a PP composition.
As still further embodiments the present invention provides polymeric products being characterized in that they satisfy the low oligomer content requirement as defined in the present application, in particular of any one of equations (1), (1a), (1b) and (1c), while at the same time providing a MFR 2 value of 15 or higher, preferably 20 or higher, more preferably 25 or higher and in embodiments even 45 or higher (always g/10 min and determined in accordance with the description and definition provided herein). A suitable upper limit for the MFR 2 value for this embodiment of the present invention is about 1000, and preferably about 500, and in embodiments 250 or even 150 (always g/10 min).
Preferred examples of the above MFR 2 embodiment of the present invention are polymeric products as defined and described herein wherein the oligomer content is below 1100 ppm, preferably below 760 ppm, and in embodiments below 560 ppm, below 340 ppm, below 240 ppm, below 110 ppm, below 35 ppm and even below 10 ppm.
Further preferred ranges for combinations of MFR 2 values and oligomer content can be derived from the following table:
Oligomer content ppmw as
MFR 2
indicated or lower
<0.1
10
8
5
5
7
4
<1
35
30
16
15
21
13
<15
130
106
64
58
82
53
<20
150
123
74
67
95
61
<25
168
137
83
75
106
68
<45
226
185
112
101
143
92
<100
340
280
168
152
214
137
<150
414
339
205
186
262
168
<250
535
438
266
241
339
218
<500
760
630
377
341
481
308
<1000
1100
900
535
484
682
437
In the table the first column defines a polymer composition in accordance with the present invention wherein the composition furthermore preferably satisfies the requirement of equation (1) as provided in this application. The second column likewise defines a composition furthermore satisfying equation (1a), the third column furthermore preferably satisfies equation (1b), the fourth column furthermore preferably satisfies equation (1c), the fifth column furthermore preferably satisfies equation (1d), and the sixth column furthermore preferably satisfies equation (1e) (formulae (1d) and (1e) are defined further below).
In the above embodiments and subgroups of the present invention MFR 2 and oligomer content are preferably the properties, as already outlined above, of the reactor-made polymer composition, i.e. the properties obtained after polymerisation without any post processing, with the only exception being standard extrusion processes for producing pellets and the like. These pellets accordingly then display the same properties as the reactor-made polymer composition.
It is evident that, within the embodiments of the present invention described above and in particular within the limits defined by equitation (1), (1′) (1a) to (1e), or (P1) to (P7), the other properties of the polymer composition can also be varied or tailored considerably depending i.a. on the end use application. The other properties of the polymer composition include the properties of the polymer structure, such as molecular weight distribution (MWD and/or PI), xylene solubles (XS), chain (stereo)structure and comonomer content, stereo regularity and comonomer distribution, the processing properties including herein the physical properties (such as rheological and thermal properties) and morphological properties (such as crystal and lamella structure as well as crystallinity), as well as the properties the final product produced from the polymer composition (e.g. stiffness, impact, creep etc.). As an example only, a propylene homopolymer may have xylene solubles (XS) varying between 1 and 5 wt-% and the XS value of a propylene random copolymer may vary between 1 to 50 wt-%, preferably 1-30 wt-%, such as 1 to 15 wt-%.
In a further preferred embodiment the polymer composition in accordance with the present invention not only displays the feasible balance of oligomer content and MFR 2 values but also shows a remarkable narrow molecular weight distribution. The narrow molecular weight distribution can be expressed in various alternative ways, e.g. in terms of rheological behaviour expressed as SHI (0/50) .
Accordingly the polymer compositions of the present invention have a narrow molecular weight distribution, typically a SHI (0/50) value of 10 or less, more preferably 8 or less and even more preferably 6 or less.
In this “narrow molecular weight distribution embodiment” the polymer composition may preferably have a MWD value of 6 or less, more preferably 5 or less, and even more preferably of from 3 to 5 or from 3.5 to 5. Furthermore in this embodiment the polymer compositions of the present invention described here further preferably display a PI value of 5 or less, more preferably 4 or less.
Alternatively, the combination of advantageous oligomer content and narrow molecular weight distribution of the polymer composition, preferably of the propylene polymer composition, can also be expressed with the following equation (1n):
Oligomer content≦ e (3.83+0.398·ln(MFR2)+0.0669·MWD) (1n)
More preferably the polymer compositions are compositions corresponding to the following equation (1n′):
Oligomer content≦ e 3.25+0.3981·ln(MFR2)+0.0669·MWD) (1n′)
In these equations “MFR 2 ” and “MWD” are determined as defined herein below and MFR 2 is 0.5 g/10 min or more and MWD is 3 or more while the “Oligomer content”, in ppm, refers to the oligomer content as defined herein.
The polymer composition corresponding to formula (1n) or (1n′) have a SHI (0/50) value of 10 or less, more preferably 8 or less and even more preferably 6 or less.
In this “narrow molecular weight distribution embodiment” the polymer composition may preferably have a MWD value of 6 or less, more preferably 5 or less, and even more preferably of from 3 to 5 or from 3.5 to 5. Furthermore in this embodiment the polymer compositions of the present invention described here further preferably display a PI value of 5 or less, more preferably 4 or less.
These further improved and surprising embodiments of the present invention in particular enable the use of polymer compositions in accordance with the present invention in fields where narrow molecular weight distributions are required, such as fiber applications since mechanical properties can be improved.
Furthermore in one embodiment the polymer composition comprises at least (i) a homopolymer component, preferably propylene (PP) homopolymer. In the case of “the narrow molecular weight distribution embodiments” described above the polymer composition preferably is a propylene homopolymer.
In another embodiment the polymer composition comprises at least (i) a copolymer component, preferably PP copolymer, more preferably PP random copolymer.
In a further embodiment the polymer composition comprises at least (i) a homopolymer or copolymer and at least (ii) a homopolymer or copolymer, in any combination. It is understood that such components (i) and (ii) are different. As well known the weight ratios thereof (split) may vary. The amount of component (i) may be 30 to 80, e.g. 40 to 70, preferably 45 to 60, wt-% and the amount of component (ii) may be 20 to 70, e.g. 30 to 60, preferably 40 to 55, wt-%, calculated from the total composition, particularly in case of PP compositions.
Alternatively, the polymer composition may consist of any of the above embodiments of components (i) or of (i) and (ii).
The alpha-olefin copolymer can be unimodal or multimodal with respect to comonomer distribution as known in the art.
The copolymer, e.g. in case of PP copolymer is preferably a PP random copolymer and may comprise in a well known manner a mixture of a homopolymer and copolymer components or a mixture of two copolymer components with differing comonomer contents.
Comonomers can be selected e.g. from a list including one or more of ethylene and C3- or higher alpha-olefins, such as C4-C12-, e.g C4-C10-alpha-olefins. In case of PP composition the comonomer is preferably at least ethylene. The C3- or higher alpha-olefin comonomer(s) can be linear, branched, aliphatic cyclic or aromatic cyclic alpha-olefins. They may be used e.g. in usual amounts, e.g. from up to 20 wt %.
In case of unimodal polymer compositions with respect to the weight average molecular weight distribution the composition may comprise one component (i) or at least two components (i) and (ii). In case of at least two components (i) and (ii) both have essentially the same weight average molecular weight distribution so that the overall molecular weight profile of the polymer composition has a single peak. In the above described “narrow molecular weight distribution embodiments” the polymer composition is preferably unimodal, more preferably a unimodal homopolymer of propylene, and comprises components (i) and (ii).
Furthermore, the polymer composition may be unimodal or multimodal with respect to the molecular weight distribution. In case of multimodal polymer composition the composition comprises at least a lower molecular weight (LMW) component and a higher molecular weight (HMW) component.
As is readily apparent from the above description, the term polymer composition or homo- or copolymer composition as employed herein refers to a polymeric product comprising at least one but in embodiments also more then one polymeric product. In accordance with the present invention it is required that at least one of the polymeric products fulfils the requirements as outlined and explained herein, but preferably the overall polymer composition fulfils these requirements, i.e. the composition comprising more then one polymeric product. Such compositions may be prepared in any suitable manner, including mechanical or melt blending as well as suitable polymerisation processes for the preparation of reactor-blends. Such reactor blends as defined herein are preferred embodiments of the present invention. In this respect reference is made to the detailed description under the heading “Polymerisation process”.
It is naturally understood that the properties of the polymer composition of the invention can be further modified. E.g. the preferable reactor-made polymer composition of the invention may be further modified, e.g. after the polymerisation step, in one or more subsequent post reactor treatment steps. It is evident that such modifications may result in another polymer composition of the invention or to other polymer products.
Such modifications include the well known post reactor chemical modification of the MFR of the polymer (visbreaking) using e.g. peroxides e.g. for increasing the MFR.
The polymer composition may also comprise e.g. additives or other polymer components which may result in a polymer composition with modified properties, as known in the art.
As mentioned the C6-C15-oligomer content of the polymer composition may contribute to the total amount of volatiles producing compounds. Additionally, it may also comprise other compounds or decomposition products which are often referred under volatiles producing compounds, e.g. volatiles originating from the overall oligomers or from any-added additives, as described above or in the prior art, e.g. in WO 03000752. The amount of these “other compounds” is not limited in this invention, and they may increase or contribute to the total amount of volatiles present in the polymer composition. If needed, this total volatile content may further be reduced or removed in a subsequent removal step in a known manner, depending e.g. on the desired end application.
The present invention achieves the improvement with respect to the oligomer content as identified and discussed above without requiring costly and/or laborious post polymerization processes, as often needed and relied upon in the prior art. Accordingly the present invention is able to provide the polymer products disclosed herein in the form of pellets or any other desired shape such as rods, powder, spheres and the like, immediately after the polymerization process, requiring only standard measures such as extruding under standard conditions, but no other post treatments, such as visbreaking and the like.
Such pellets and the like are in particular suitable for applications in fields having increased demands on organoleptic properties, the present invention provides pellets of polymer compositions directly obtained from polymerization and subsequent pelletisation without any further post processing. The improved properties of the polymer compositions of the present invention, i.e. in particular the low oligomer content, and in embodiments specific MFR 2 values as explained herein and relatively narrow molecular weight distribution values, are accordingly directly passed on to the pellets and are present therein, so that these pellets may suitably be used in high quality end applications, such as applications requiring a low volatile and low oligomer content, for example in order to suppress or exclude detrimental effects such as fogging and/or migration.
These advantages are furthermore not sacrificed by subjecting the polymer composition in accordance with the present invention to a subsequent pelletizing process, such as a process using an extruder or any other conventional device for palletizing. The pelletizing process involves melting and mixing steps of the reactor made polymer powder, optionally together with conventional additives, in an extruder and thereafter forming the extrudate in the form of pellets as known in the art.
The polymer composition can be used alone or in the form of a blend with other polymer components.
The invention covers also heterophasic polymers of an alpha-olefin (also called block copolymers), preferably of propylene, whereby the PP composition of the invention forms the polypropylene matrix component, wherein an elastomeric propylene copolymer component, so called rubber component, is dispersed. Comonomers can be selected from the options given above.
The polymer composition as defined in the present invention can be used in a wide variety of end applications, e.g. applications wherein the odor, taste and/or fogging should be avoided or minimized, e.g. in automobile, packaging (including food and medical), fiber, pipe or wire and cable (W&C) industry without limiting to these.
The invention provides also a further step of pelletising the polymer composition to polymer pellets. The pellets can be formed in a subsequent pelletising step e.g. by extrusion as known in the art and may comprise additives in the known manner as indicated above. In addition to the polymer of the invention, the pellets may also comprise further polymer components.
Moreover, the PP composition, optionally in the form of pellets, can be processed in a known manner to articles, including molded and extruded articles, layered structures, fibers, pipes, just few to mention.
The layered structures of the PP composition can be monolayer or multilayer structures including films, coatings, packaging materials, cables etc.
Polymerisation Process for the Preparation of the Polymer Composition of the Invention
In principal any polymerisation method including slurry and gas phase polymerisation can be used for producing the polymer composition. Slurry polymerisation is preferably a bulk polymerisation. “Bulk” means a polymerisation in a reaction medium comprising at least 60 wt-% monomer.
The invention also provides a process for producing a polymer composition comprising at least (i) an alpha-olefin homo- or copolymer component as defined above or in claims below, wherein alpha-olefin monomers, optionally together with one or more comonomers, are polymerised in the presence of a polymerisation catalyst. In case the polymer composition consists of component (i) the process is a single stage process.
The invention further provides a process for producing a polymer composition comprising at least two different alpha-olefin homo- or copolymer components (i) and (ii) as defined above or in claims below, wherein each component is produced by polymerising alpha-olefin monomers, optionally together with one or more comonomers, in the presence of a polymerisation catalyst in a multistage polymerisation process using one or more polymerisation reactors, which may be the same or different, e.g. at least loop-loop, gas-gas or any combination of loop and gas. Each stage may be effected in parallel or sequentially using same or different polymerisation method. In case of a sequential stages each components, e.g. (i). and (ii), may be produced in any order by carrying out the polymerisation in each step, except the first step, in the presence of the polymer component formed, and preferably the catalyst used, in the preceding step. Alternatively, the same or different catalyst can be added in the subsequent step(s).
Preferably, at least the component (i) is produced in a slurry process, preferably bulk process. Such slurry or bulk process may be carried e.g. in a slurry reactor or, preferably, a loop reactor. The optional component (ii) is preferably produced by gas phase polymerization in a gas phase reactor.
Multistage processes include also bulk/gas phase reactors known as multizone gas phase reactors for producing e.g. multimodal polymer compositions.
A multimodal, e.g. at least bimodal, polymer composition as defined above, which comprises at least two different components (i) and (ii) with different molecular weight distribution and/or with different comonomer contents, may be produced by blending each or part of the components in-situ during the polymerisation process thereof (in-situ process) or, alternatively, by blending mechanically two or more separately produced components in a manner known in the art.
It is also possible to produce a multimodal PP composition in one reactor by selecting e.g. one or more of the following: (1) changing polymerisation conditions, (2) using at least two different catalysts and (3) using at least two different comonomer feeds.
In one embodiment the process for producing any of the above polymer composition (referred below also as “process for producing the polymer composition”) comprising (i) an alpha-olefin homopolymer or copolymer component and, optionally, (ii) an alpha-olefin homopolymer or copolymer component includes the steps of:
(a) polymerising in a slurry reactor zone, preferably a loop reactor, alpha-olefin monomers, optionally together with one of more comonomers, in the presence of a polymerisation catalyst to produce polymer component (i),
and, optionally, transferring the reaction product of step (a) to a subsequent gas phase reactor zone,
(b) polymerising in a gas phase reactor zone alpha-olefin monomers, optionally together with one or more comonomers, in the presence of the reaction product of step (a) to produce polymer component (ii) for obtaining the polymer composition,
and recovering the obtained composition.
A preferred multistage process is a “loop-gas phase”-process, such as developed by Borealis A/S, Denmark (known as BORSTAR® technology) described e.g. in patent literature, such as in EP 0887 379 or in WO92/12182.
If the polymer composition has at least a multimodal molecular weight distribution, then in case of PP, the HMW fraction is preferably component (i) produced in step (a) and the LMW fraction is component (ii) which is produced in a subsequent step (b) in the presence of component (i) as obtained from the first reactor.
In the case of a unimodal polymer compositions with respect to the weight average molecular weight distribution a composition comprising at least two-components (i) and (ii) both having essentially the same weight average molecular weight distribution so that the overall molecular weight profile of the polymer composition has a single peak, the composition preferably is prepared using a two stage process as described above (“process for producing the polymer composition”), preferably using the above described BORSTAR® technology.
Optionally, a prepolymerisation step in a manner known in the field may precede the polymerisation step (a).
If desired, a further elastomeric comonomer component, so-called rubber component, may be incorporated into the obtained polymer, preferably PP, composition to form a heterophasic copolymer of the composition mentioned above. The rubber component, preferably elastomeric PP copolymer of PP with at least ethylene comonomer, may preferably be produced after the gas phase polymerization step (b) in a subsequent second or further gas phase polymerization zones using e.g. one or more gas phase reactors.
The process of the invention is preferably a continuous process.
Preferably, the “process for producing the polymer composition” as defined above is a PP polymerization process, wherein conditions for the slurry reactor of step (a) may be as follows:
the temperature is within the range of 40° C. to 110° C., preferably between 60° C. and 100° C., 70-90° C., the pressure is within the range of 20 bar to 80 bar, preferably between 30 bar to 60 bar, hydrogen can be added for controlling the molar mass in a manner known per se;
the reaction mixture from the slurry (bulk) reactor is transferred to the gas phase reactor, i.e. to step (b) and conditions in step (b) are preferably as follows:
the temperature is within the range of 50° C. to 130° C., preferably between 60° C. and 100° C., the pressure is within the range of 5 bar to 50 bar, preferably between 15 bar to 35 bar, hydrogen can be added for controlling the molar mass in a manner known per se.
The process of the invention or any embodiments thereof above or below enable highly feasible means for producing and further tailoring the polymer composition of the invention as defined in any of the above described embodiments, preferably as defined by equation (1), (1a) to (1e), or by (P1) to (P7) to adjust e.g. the properties of the polymer desired for the end application. E.g. the properties of the polymer composition can be adjusted or controlled in a known manner e.g. with one or more of the following process parameters: hydrogen feed, comonomer feed, alpha-olefin feed in the gas phase reactor, preferably propylene and comonomer feeds, catalyst, the type and amount of an external donor (if used), split between components, e.g. components (i) and (ii).
The MFR values used in the above equitation (1), (1′) and (1a) to (1c), or later below in (1d) or (1e), as well as (P1) to (P7) are preferably determined from the reactor-made polymer composition. As well known, the adjustment of said MFR value to a desired level may be effected during the polymerisation process by adjusting and controlling the process conditions, e.g. by regulating the molecular weight of the polymerisation product using a molecular weight regulator, e.g. hydrogen.
In one preferable embodiment a PP composition produced and the polymerisation is effected at elevated temperature, such as at least 70° C., more preferably at least 80° C. for further decreasing the oligomer content.
Furthermore, the crystallinity of the PP composition can be modified further during or after the polymerisation step with nucleating agents in a manner known in the art.
As mentioned above the reactor-made polymer product may also subjected to a post-reactor modifications for further tailoring the properties of the obtained polymer product, which include e.g. a chemical post-treatment, i.e. visbreaking, with organic peroxides to adjust further the MFR of the reactor-made polymer product. Also additives or further polymers may be added to modify the product and/or processing properties of the polymer. The additives include the conventional fillers, colorants and stabilizers.
The obtained polymer composition may also be e.g. extruded in a known manner to obtain pellets. The composition, optionally in the form of pellets, may then be further processed to the desired articles used in the end applications.
Thus the polymer composition of the invention is preferably the reactor-made composition which can be tailored or modified within the limits of the invention during or after the polymerisation step.
Alternatively, as already indicated above, it is also to be understood that the composition of the invention with advantageously low oligomer content may be used as a starting material for producing further polymer compositions which may not satisfy the equitation (1) or one of the definitions (P1) to (P7).
The principles of the preferable polymerisation methods described above can be applied for any alpha-olefin composition of the invention, preferably e.g. for PP or PE composition.
Catalyst System
In principle the polymer composition of the invention can be produced using any polymerisation catalyst which provides an alpha-olefin polymer that fulfils the balance between oligomers and MFR, e.g. as given by the equitation (1) or one of the definitions (P1) to (P7). Such catalyst may include known Ziegler Natta type of catalysts, metallocenes including the single site catalysts and non-metallocenes. The meaning of this type of catalysts is known in the field. The catalyst may be based on one or more transition metal catalysts or late transition metal catalysts or any combinations thereof.
Examples of the feasible catalyst are illustrated by preferable preparation embodiments of a PP composition. It is, however, evident that the invention is not limited to these embodiments of PP, but principles described below e.g. for the catalyst preparation apply generally also to embodiments of other alpha-olefin compositions, such as to PE compositions.
Preferably, the polymerisation catalyst system for polymerisation of the PP composition is of a Ziegler Natta type and comprises:
1. a catalytically active component, e.g. as described above, preferably a Ti- and Mg-containing component which comprises an internal electron donor which can be any known in the art, e.g. as described below for the one preferable embodiment of the catalyst system, 2. a cocatalyst which is preferably an Al-compound, such as trethyl alumininum (TEA), and 3. an external electron donor. Examples of such donor are e.g. organosilicon compounds, such as silanes, e.g. cyclohexyl methyl dimethoxy silane or dicyclopentyl dimethoxy silane, depending on the properties desired for the final PP composition.
The molar ratio Al/external donor in the catalyst system may vary and is typically 3 to 200, such as 5 to 100, mol/mol. The Al typically originates from the cocatalyst. Also the molar ratio of Al/Ti in the catalyst system may vary and is typically between 50 to 500. E.g. 100 to 300 mol/mol ratio may be used.
Noticing the requirements of the other end properties desired for the PP composition, also e.g. the choice of the donor and the amount thereof may be used for further tailoring the oligomer content within the limits of the invention defined with the MFR.
In general one very advantageous way for obtaining the polymer composition is to use a polymerisation catalyst produced with the emulsion solidification technology disclosed below. Said catalyst is preferably of a Ziegler Natta type and comprises a compound of a transition metal of Group 3 to 10 of the Periodic Table (IUPAC, 1989), or of an actinide or lanthanide, and may be prepared according to the following “catalyst preparation method” comprising:
(a) forming a liquid/liquid emulsion system, which contains a homogeneous solution of at least one catalyst component, said solution being dispersed in a solvent immiscible therewith and forming the dispersed phase of the liquid/liquid emulsion system, (b) solidifying said dispersed droplets to form solid catalyst particles having a predetermined size range, (c) removing the solvent from the reaction mixture in order to obtain said solid catalyst particles.
The above general solidification principles using emulsion preparation techniques described above equally apply for any alpha-olefins, preferably for PP and PE, and also for other catalyst types than ZN, such as metallocenes.
In one preferable embodiment the PP composition is advantageously obtainable by catalyst prepared according to the emulsion/solidification technology disclosed e.g. in WO 03/000754, WO 03/000757 or WO2004029112 of Borealis, the contents of which are incorporated herein by reference.
A feasible class of catalysts to be employed in accordance with the present invention is the Ziegler-Natta catalyst described in WO 2004/029112 mentioned above. These Ziegler-Natta catalysts are subjected already during catalyst synthesis to a treatment with an alkylating agent, in particular an Al compound as illustrated in this international publication. Using such a Ziegler-Natta catalyst enables the preparation of polymer compositions in accordance with the present invention, including in particular the polymer compositions in accordance with the preferred embodiments disclosed herein, in the form of reactor-made polymer compositions not requiring any further post processing such as visbreaking. Accordingly the polymer compositions of the present invention are obtainable with the specific class of Ziegler-Natta catalysts disclosed in WO 2004/029112, incorporated herein by reference.
The PE composition may also be obtainable by any of the process described above using in one embodiment a catalyst of Ziegler Natta type which is preparable by the emulsion/solidification method adapted to PE catalyst, e.g. as disclosed in WO03106510 of Borealis, e.g. according to the principles given in the claims thereof. The contents of this document is also incorporated herein by reference.
The emulsion formation is based on the miscibility of the continuous phase and the disperse phase. The continuous phase may be substantially inert (chemically) or it may contain dissolved therein one or more of the reactants of the catalyst component. The solidification step may be effected e.g. by subjecting the emulsion system to a temperature change.
Examples of the solvents used in the continuous phase include hydrocarbons, such as aliphatic or aromatic hydrocarbons, and fluorinated hydrocarbons, such as fluorinated aliphatic or alicyclic hydrocarbons, e.g aliphatic perfluorinated hydrocarbons. For the preparation of a PP composition, examples of preferable solvents are aromatic hydrocarbons, e.g. toluene, can be used as the solvent for continuous phase. For the preparation of PE composition, preferable solvents are the above mentioned fluorinated hydrocarbons.
According to one preferable embodiment, the polymer composition is obtainable by a single stage or multistage polymerisation process as defined above using the polymerisation catalyst prepared by any process method defined above. The process may equally be a single- or multistage process of the invention as described above, depending on the properties of the produced polymer composition.
If the polymer composition is produced by a multistage process, then the polymerisation is preferably effected in the presence of a catalyst obtainable by the “catalyst preparation method” as defined above or in more detailed for PP below.
The invention also provides a polymer composition as defined above which is obtainable by any process for preparing the polymer composition as defined above, wherein a polymerisation catalyst is used which is a ZN-catalyst prepared by the “catalyst preparation method” as defined above or below.
The catalyst obtainable by the “catalyst preparation method” as defined above enables very advantageous means to produce the polymer composition of the invention, preferably the reactor-made polymer composition of the invention.
The following embodiments of a PP composition satisfying equitations (1d) or (1e) are provided only for illustrating, how the oligomer content of the polymer composition may be further optimised with the process parameters within the limits of the invention defined above or in claims:
“oligomer content”≦ e [6.7+(0.504·ln(MFR 2 ))−(0.0457·T)] (1d), or
“oligomer content”≦ e [7.3+(0.504·ln(MFR 2 ))−(0.459·D)−(0.00317·Al/Do)−(0.0453·T)] (1e),
wherein in (1d) and (1e) “oligomer content” and MFR 2 are as defined above in equitation (1),
T is the polymerization temperature, e.g. at least 70° C., preferably at least 80° C., the upper limit suitably being ≦100° C., preferably ≦90° C.,
Al/Do is the molar ratio between aluminium alkyl and the used external donor, and
D is a number between 1 and 2, and may be e.g. 1, when the external electron donor is dicyclopentyl dimethoxy silane or has a similar effect on the oligomer content to that, and 2 when the donor is cyclohexyl methyl dimethoxy silane or has a similar effect on the oligomer content to that.
In the embodiments 1(d) and 1(e), the PP composition is preferably obtainable by a single- or multistage process as defined above using the catalyst prepared by the “catalyst preparation method” described above.
In the process of the invention or any embodiments thereof, the external donor used in the catalyst system is preferably dicyclopentyl dimethoxy silane or cyclohexyl methyl dimethoxy silane.
Embodiment (1d) shows that the increase in the temperature can decrease the oligomer content further. Embodiment (1e) shows that by using cyclohexyl methyl dimethoxy silane as the donor and/or by increasing the ratio Al/Do, the oligomer content can be further lowered or optimised, if needed, depending on the other properties desired for the end product.
In one preferable embodiment, the composition is a PP composition “catalyst preparation method” a solution of a complex of Group 2 metal and an electron donor is prepared by reacting a compound of said metal with said electron donor or a precursor thereof in an organic liquid reaction medium; reacting said complex, in solution, with a compound of a transition metal to produce an emulsion, the dispersed phase of which contains more than 50 mol % of the Group 2 metal in said complex: maintaining the particles of said dispersed phase within the average size of 5 to 200 micro meter by agitation preferably in the presence of an emulsion stabilizer and solidifying said particles. The complex of the Group 2 metal is preferably a magnesium complex.
The emulsion stabiliser is typically a surfactant, of which the preferred class is that based on acrylic polymers.
For said catalyst particles, the compound of a transition metal is preferably a compound of a Group 4 metal. The Group 4 metal is preferably titanium, and its compound to be reacted with the complex of a Gp 2 is preferably a halide.
In the “catalyst preparation method” also a turbulence minimizing agent (TMA) or mixtures thereof may be used, which are preferably polymers having linear aliphatic carbon backbone chains, which might be branched with short side chains only in order to serve for uniform flow conditions when stirring.
As electron donor compound to be reacted with the Group 2 metal compound is preferably a mono- or diester of an aromatic carboxylic acid or diacid, the latter being able to form a chelate-like structured complex. Said aromatic carboxylic acid ester or diester can be formed in situ by reaction of an aromatic carboxylic acid chloride or diacid dichloride with a C 2 -C 16 alkanol and/or diol, and is preferable dioctyl phthalate, e.g. dioctyl (2-ethyl-hexyl)phthalate. The reaction for the preparation of the Group 2 metal complex is generally carried out at a temperature of 20° to 80° C. and in case that the Group 2 metal is magnesium, the preparation of the magnesium complex is carried out at a temperature of 50° to 70° C.
The magnesium dialkoxide may be the reaction product of a magnesium dihalide such as magnesium dichloride or a dialkyl magnesium of the formula R 2 Mg wherein each one of the two Rs is a similar or different C 1 -C 20 alkyl, preferably a similar or different C 4 -C 10 alkyl, Typical magnesium alkyls are ethylbutyl magnesium, dibutyl magnesium, dipropyl magnesium, propylbutyl magnesium, dipentyl magnesium, butylpentylmagnesium, butyloctyl magnesium and dioctyl magnesium. Most preferably, one R of the formula R 2 Mg is a butyl group and the other R is an octyl group, i.e. the dialkyl magnesium compound is butyl octyl magnesium.
Dialkyl magnesium, alkyl magnesium alkoxide or magnesium dihalide can react with a polyhydric alcohol R′(OH) m or a mixture thereof with a monohydric alcohol R′OH.
Preferable monohydric alcohols are those of formula R′OH in which R′ is a C 2 -C 16 alkyl group, most preferably a C 4 -C 12 alkyl group, particularly 2-ethyl-1-hexanol.
Preferably, essentially all of the aromatic carboxylic acid ester is a reaction product of a carboxylic acid halide, preferably a dicarboxylic acid dihalide, more preferably an unsaturated α,β-dicarboxylic acid halide, most preferably phthalic acid dichloride, with the monohydric alcohol.
If desired an aluminium alkyl compound, optionally containing halogen may be added to the dispersion before recovering the solidified particles. This embodiment is described e.g. in the above referred WO2004029112, see e.g. claim 1 . These catalysts, as well as those described in WO 2004/111098 enable the production of narrow molecular weight distribution polymer compositions of the present invention. Reference in this respect can be made to the disclosure in WO 2004/111098 and in WO 2004/029122, both incorporated herein by reference with respect to the catalyst synthesis using an alkylating agent during catalyst synthesis, which disclose suitable alkylating agents, preferably aluminium compounds comprising at least one alky substituent. It has been found that these catalysts, disclosed in the prior art in association with high temperature activity and ability to polymerise propylene and ethylene polymers having decreased xylene solubles contents and lower isotacticity, are feasible for narrowing the molecular weight distribution compared with polymeric products obtained with conventional Ziegler-Natta catalysts.
The finally obtained catalyst component is desirably in the form of particles having an average size range of 5 to 200 μm, preferably 10 to 100, more preferably 20 to 50 μm. Especially the catalyst particles obtainable by “the catalyst preparation method” are typically non-porous, i.e. their surface area is very small compared to prior art Ziegler-Natta catalysts supported on an external carrier. The surface area of the catalyst used in the present invention may be smaller than 20 m 2 /g, preferably less than 10 m 2 /g, and more preferably less than 5 m 2 /g, and may even be not measurable by normal measurement apparatus. This applies also to the porosity. The active components of the catalysts are evenly distributed thorough the whole catalyst particles.
The catalytically active component obtainable by the “catalyst preparation method” as defined above may be incorporated with a cocatalyst (2) and external donor (3) as mentioned above.
E.g. the PP composition of the invention may comprise said C6-C15-oligomers in a n amount which is less than 30 wt-%, preferably less than 50 wt-% and even less than 60 wt-% compared to conventional polypropylene compositions with the same MFR 2 , e.g. conventional polypropylene compositions described in EP395083 of Montell or EP86472 of Montedison referred before.
The present invention has been described above in relation to the beneficial features of low oligomer content, preferably in combination with the high MFR 2 value defined above, the narrow MWD distribution and/or the feature of the polymer composition of the present invention being a reactor-made polymer composition, optionally in the form of pellets or the like, i.e. obtained directly from the polymerisation reaction without any further post processing steps. As outlined above the present invention contemplates for polymer compositions comprising more than one polymer component to prepare same in the form of reactor blends as explained above. Suitable processes and catalysts for preparing the improved polymer compositions of the present invention are identified above.
However, the present invention provides one further surprising and particular preferred embodiment which will be described in detail in the following. All definitions provided above in connection with the present invention as well as all preferred embodiments mentioned above are also valid for this further embodiment if not further specified in the following.
Surprisingly it has been determined by the present inventors that the use of a specific class of Ziegler-Natta catalysts enables the preparation of polymer compositions as defined herein, preferably propylene homo- or copolymer, more preferably propylene homopolymers, which not only show the improvement with respect to oligomer content, i.e. low oligomer content, but which also display, compared with polymer compositions obtained with other Ziegler-Natta catalysts, a narrower MWD distribution. As illustrated in examples 1A to 10A this effect amounts to a narrowing of the molecular weight distribution of about 10% or more, an achievement which has to be considered as vast improvement in particular for fields of application where rather narrow MWD are preferred.
As is readily apparent from the above the polymer compositions of this embodiment of the present invention satisfy the low oligomer requirements of the present invention as given above, in particular the polymer compositions of this embodiment satisfy the equations as presented above in connection with the general description of the low oligomer content, namely equation (1), more preferably equation (1a), (1b) or (1c).
Accordingly the present invention provides a polymer composition as defined herein, wherein the polymer composition not only displays a lower oligomer content, as described in detail above, but also shows a narrower molecular weight distribution, compared with polymer composition which have been prepared using a Ziegler-Natta catalyst which has not been subjected to a treatment with an alkylating agent during catalyst synthesis, all other conditions being identical. As identified above the molecular weight distribution narrowing effect provided by the present invention amounts to at least 5%, preferably at least 7% and in embodiments up to about 10% or more, expressed either as SHI (0/50) , PI or Mw/Mn (MWD), all as defined herein.
Accordingly this aspect of the present invention can be described as a narrow molecular weight distribution polymer composition, wherein the present invention enables a narrowing of the molecular weight distribution of a given polymer composition, compared with corresponding polymer composition that has a higher oligomer content than the polymer composition of the invention, e.g. compared with polymer compositions, prepared under identical conditions, but not using the catalysts for polymerisation which are described herein as suitable catalysts.
In this respect the present invention in embodiments enables a lowering of the SHI (0/50) value (as measure for the molecular weight distribution) by 10%, more preferably by 20%, even more preferably by 30% and most preferably by 40%, compared with corresponding polymer composition that has a higher oligomer content than the polymer composition of the invention, e.g. compared with polymer compositions being prepared under identical conditions but, as outlined above, not using any of the catalysts illustrated herein.
In a further feasible embodiment the present invention in embodiments enables a lowering of the MWD value (as measure for the molecular weight distribution) by 10%, more preferably by 20%, even more preferably by 30% and most preferably by 40%, compared with corresponding polymer composition that has a higher oligomer content than the polymer composition of the invention, e.g. compared with polymer compositions being prepared under identical conditions but, as outlined above, not using any of the catalysts illustrated herein.
These narrow molecular weight distribution polymer compositions more preferably are compositions according to equations (1n) and (1n′) defined above, and in preferred embodiments also these polymer compositions are compositions in accordance with any of equations (1a) to (1c).
Also in this embodiment of the present invention it is further preferred when the polymer composition displays a combination of the parameters MFR 2 and narrow molecular weight distribution as outlined above in connection with the low oligomer content embodiment. These correlations are also valid for this embodiment of the present invention.
With respect to further details of this embodiment of the present invention, such as comonomer content, modality, polymerisation processes and the like reference can be made to the other parts of the specification of the present application. All information disclosed herein likewise also applies for the preferred embodiment described here.
The present invention also provides a process for producing low oligomer content and narrow molecular weight distribution polymer compositions as illustrated above. This process corresponds basically to the general process description as provided above with the exception however that the catalyst employed for polymerisation has to be a Ziegler-Natta catalyst which has been subjected during catalyst synthesis to a treatment with an alkylating agent. Reference in this connection can again be made to the two international publications mentioned above, WO 2004/111098 and in WO 2004/029122, both incorporated herein by reference with respect to the catalyst synthesis using an alkylating agent during catalyst synthesis.
As already mentioned above, all features of the description of the present application described above are also applicable to the narrow molecular weight distribution embodiment disclosed here, if not specified further herein.
DEFINITIONS AND DETERMINATION METHODS
The definitions for terms and the determination methods for the characterising properties and/or parameters are given below. These definitions and determination method descriptions apply generally both for the description part above and for the examples below, unless otherwise stated:
The oligomer content of the polymer composition means the oligomer fraction having 6 to 15 carbon atoms and can be determined using the following method:
The determination is preferably made from the reactor-made polymer product, i.e. reactor powder as obtained form the polymerisation step. The oligomer content (C6-C15) in the polymer powder was measured in the following way: 1 hour after the polymer had been taken out of the reactor about 100 gram polymer powder was put in a glass bottle and sealed. The bottle was placed in the freezer (at −18° C.), and was analysed the following day. The oligomer content was analysed with static head space gas chromatography, GC, from Hewlett Packard. 2 gram powder was placed in a 20 ml glass ampoule. After 1 hour at 120° C. a sample was automatically taken to the GC. A non polar column, silicon rubber coating, SE-30 was used. Substances containing 6, 9, 12 and 15 carbon atoms were regarded as oligomers, because oligomers more carbon atoms, 18 and more, are scarcely detected, due to low volatility. Temperature profile in the GC was: 5 minutes at 40° C., temperature increase with 10° C./min up to 250° C. and finally 4 minutes at 250° C. The GC is Hewlett Packard 5890 and the Head space is Hewlett Packard 19395.
It is to be understood that in principle any other determination method could be used which would give the corresponding results as the above determination method (within the limits of measurement accuracy as evident for a skilled person).
Mw means weight average molecular weight determined in a known manner using size exclusion chromatograpy (SEC). Unless otherwise defined, the term “molecular weight” as used herein means the weight average molecular weight Mw. MWD means Mw/Mn, wherein Mw is the weight average molecular molecular weight and Mn is the number average molecular weight. The MWD can be determined e.g. by using a size exclusion chromatography (SEC) in a manner known in the art. Weight-% is abbreviated as w % or wt-%. ppm is parts per million by weight. By the term “random copolymer” is meant herein that the comonomer in said copolymer is distributed randomly, i.e. by statistical insertion of the comonomer units, within the copolymer chain. Said term “random” copolymer is generally known and used in the art. Propylene random copolymer typically contains up to 12 wt %, preferably up to 8 wt % one or more comonomer as defined above. The xylene solubles (XS)-fraction contains amorphous polymer chains was analyzed by the known method:
2.0 g of polymer was dissolved in 250 ml p-xylene at 135° C. under agitation. After 30±2 minutes the solution was allowed to cool for 15 minutes at ambient temperature and then allowed to settle for 30 minutes at 25±0.5° C. The solution was filtered with filter paper into two 100 ml flasks.
The solution from the first 100 ml vessel was evaporated in nitrogen flow and the residue dried under vacuum at 90° C. until constant weight is reached.
XS%=(100×m 1 ×v 0 )/(m 0 ×v 1 ), wherein m 0 =initial polymer amount (g) m 1 =weight of residue (g) v 0 =initial volume (ml) V 1 =volume of analyzed sample (ml)
MFR 2 : MFR 2 values are determined in a usual manner known to the skilled person in the art, wherein load and temperature are selected depending from the type of polymer, in the examples the following methods were employed: PP composition was determined according to ISO 1133 (230° C., 2.16 kg load), and for the determination of a PE composition, reference is made to ISO 1133 (190° C., 2.16 kg load). Multimodality, including bimodality, with respect to the comonomer distribution means that the composition contains at least two polymer components having different comonomer content (wt %). Comonomer content (wt %) can be determined in a known manner based on Fourier transform infrared spectroscopy (FTIR) determination calibrated with C 13 -NMR. Multimodality, including bimodality, with respect to the weight average molecular weight distribution means that the molecular weight profile of e.g. the polymer composition does not comprise a single peak but instead comprises two or more distinct maxima, a maximum and one or more shoulders centered about different average molecular weights, or in some cases a distinctly broadened curve. E.g. the components (i) and (ii) of the composition may comprise different molecular weights. Melting temperature, crystallization temperature and degree of crystallinity are measured with a Mettler TA820 differential scanning colorimetry device (DSC) on 3±0.5 mg samples. Crystallization and melting temperatures are obtained during 10° C./min cooling and heating scans between 30° C. and 225° C. Melting and crystallization temperatures were taken as the peaks of endotherms and exotherms. The degree of crystallinity is calculated by comparison with the heat or fusion of a perfectly crystalline polypropylene, i.e. 209 J/g. Flexural modulus is measured according to ISO 178 (room temperature, if not otherwise mentioned), by using injection molded test specimens as described in EN ISO 1873-2 (80×10×4 mm). Charpy notched impact is measured according to ISO 179 (room temperature, 23° C. if not otherwise mentioned) using injection molded test specimen as described in EN ISO 1873-2 (80×10×4 mm). Tensile strength, including tensile stress at yield and strain at yield, is measured according to ISO 572-2 (cross head speed 50 m m/min). Tensile modulus is measured according to ISO 572-2 (cross head speed 1 mm/min).
Rheology: Dynamic rheological measurements were carried out with Rheometrics RDA-II QC on compression molded samples under nitrogen atmosphere at 200° C. using 25 mm-diameter plate and plate geometry. The oscillatory shear experiments were done within the linear viscoelastic range of strain at frequencies from 0.01 to 500 rad/s. (ISO6721-1)
The values of storage modulus (G′), loss modulus (G″), complex modulus (G*) and complex viscosity (η*) were obtained as a function of frequency (ω).
The Zero shear viscosity (η 0 ) was calculated using complex fluidity defined as the reciprocal of complex viscosity. Its real and imaginary part are thus defined by
f′ (ω)=η′(ω)/[η′(ω) 2 +η″(ω) 2 ] and
f″ (ω)=η″(ω)/[η′(ω) 2 +η″(ω) 2 ]
From the following equations
η′= G ″/ω and η″= G′/ω
f ′(ω)= G ″(ω)·ω/[ G ′(ω) 2 +G ″(ω) 2 ]
f ″(ω)= G ′(ω)·ω/[ G ′(ω) 2 +G ″(ω) 2 ]
The polydispercity index, PI, is calculated from cross-over point of G′(ω) and G″(ω).
There is a linear correlation between f′ and f″ with zero ordinate value of 1/η 0 . (Heino et al. 1 )
For polypropylene this is valid at low frequencies and five first points (5 points/decade) are used in calculation of η 0 .
Elasticity indexes (G′) and shear thinning indexes (SHI), which are correlating with MWD and are independent of MW, were calculated according to Heino 1, 2 ) (below). SHI is calculated by dividing the Zero Shear Viscosity by a complex viscosity value, obtained at a certain constant shear stress value, G*. The abbreviation, SHI(0/50), is the ratio between the zero shear viscosity and the viscosity at the shear stress of 50 000 Pa. 1) Rheological characterization of polyethylene fractions. Heino, E. L.; Lehtinen, A; Tanner, J.; Seppälä, J. Neste Oy, Porvoo, Finland. Theor. Appl. Rheol., Proc. Int. Congr. Rheol., 11 th (1992), 1 360-362 2) The influence of molecular structure on some rheological properties of polyethylene. Heino, Eeva-Leena. Borealis Polymers Oy, Porvoo, Finland. Annual Transactions of the Nordic Rheology Society, 1995.
DETAILED DESCRIPTION OF THE INVENTION
EXAMPLES
The starting materials are commercially available or can be produced analogously to the methods described in the literature.
Example 1
All raw materials were essentially free from water and air and all material additions to the reactor and the different steps were done under inert conditions in nitrogen atmosphere. The water content in propylene was less than 5 ppm.
The catalyst was a highly active and stereo specific Ziegler Natta catalyst (ZN catalyst) prepared according to patent WO03/000754, example 7, and had Ti content 3.37 w-%.
The polymerisation was done in a 5 liter reactor, which was heated, vacuumed and purged with nitrogen before taken into use. 553 μl TEA (triethyl aluminium, from Witco), 81 μl donor (cyclohexyl methyl dimethoxy silane, from Wacker, dried with molecular sieves) and 20 ml pentane (dried with molecular sieves and purged with nitrogen) were mixed and allowed to react for 5 minutes. Half of the mixture was added to the reactor after which the reactor was charged with 70 mmol hydrogen and 1400 g propylene. The other half of the mixture was mixed with 23.0 mg ZN catalyst in a metal cylinder and pushed into the reactor with 20 bar nitrogen. The contact time was about 20 minutes. The Al/Ti molar ratio was 250 and the Al/Do molar ratio was 10. The temperature was increased from room temperature to 70° C. during 16 minutes. The reaction was stopped, after 60 minutes at 70° C., by flashing out unreacted monomer. Finally the polymer powder was taken out from the reactor and analysed and tested. About 100 gram of the powder was put into a glass bottle and stored in the freezer for volatiles analyses the following day. The details and results are seen in table 1.
Comparative Example 1
This example was done in accordance with example 1, with the exception that a supported porous catalyst was used. The catalyst used was a typical porous 4 th generation, transesterified Zieglar Natta catalyst. This type of catalyst is described in general in EP 491 566 and was prepared as follows: TiCl 4 was fed to reactor and cooled to −20° C. MgCl 2 carrier obtained by spray-crystallising MgCl 2 (C 2 H 5 OH) n melt was suspended in aliphatic hydrocarbon solvent (bp, 90-110° C.) and cooled before adding to the cold TiCl 4 . Controlled heating to 130° C. was performed. During heating di-2-ethylhexyl phthalate (DOP) eas added and transesterification (DOP to DEP, diethylphthalate) effected by keeping the mixture for 30 min at 130° C. The solid was separated by filtration and the procedure repeated 3 times, each repeat adding TiCl 4 to the filtered solids from the previous titanation. The catalyst was then washed 4 times with aliphatic hydrocarbon solvent and dried in vacuum to free flowing powder. The surface area and porosity of a catalyst produced was typically 250-300 m 2 /g and 0.4-0.5 g/cm 3 , respectively. The catalyst contained 1.9 w-% titanium.
The details and results are seen in table 1.
Comparative Example 2
This example was done in accordance with example 1, with the exception that a catalyst which can be described as a typical porous 4 th generation Ziegler Natta catalyst, containing TiCl4, MgCl 2 as carrier and a carboxylic ester as internal donor was used. For the preparation of the catalyst the description and examples of EP 395083 of Montell are referred. The Ti content in the catalyst was 2.4 w-%. The details and results are seen in table 1.
Example 2
This example was done in accordance with example 1, with the exception that the hydrogen amount was 800 mmol. The details and results are seen in table 1.
Comparative Example 3
This example was done in accordance with example 2, with the exception that the catalyst described in comparative example 1 was used and that 650 mmol hydrogen was used. The details and results are seen in table 1.
Comparative Example 4
This example was done in accordance with example 2, with the exception that the catalyst described in comparative example 2 was used and the hydrogen amount was 450 mmol was used. The details and results are seen in table 1.
Example 3
This example was done in accordance with example 1, with the exception that as the donor dicyclopentyl dimethoxy silane with Al/Do ratio 50 was used and that the hydrogen amount was 600 mmol. The details and results are seen in table 1.
Comparative example 5
This example was done in accordance with example 3, with the exception that the catalyst described in comparative example 1 was used and that 1000 mmol hydrogen was used. The details and results are seen in table 1.
Comparative Example 6
This example was done in accordance with example 3, with the exception that the catalyst described in comparative example 2 was used and that 670 mmol hydrogen was used. The details and results are seen in table 1.
Comparative Example 7
This example was done in accordance with comparative example 5, with the exception that the hydrogen amount was 150 mmol. The details and results are seen in table 1.
Comparative Example 8
This example was done in accordance with comparative example 5, with the exception that the hydrogen amount was 10 mmol.
Comparative Example 9
This example was done in accordance with example 1, with the exception that the temperature in polymerisation was 80° C., 1000 mmol hydrogen, dicyclopentyl dimethoxy silane, Al/Do ratio of 50 and comparative example 1 was used. The details and results are seen in table 1.
Comparative Example 10
This example was done in accordance with comparative example 9, with the exception that the temperature in polymerisation was 70° C. The details and results are seen in table 1.
TABLE 1
Examples: Polymerisation conditions and Results
Comp.
Comp.
Comp.
Comp.
Comp.
Comp.
Comp.
Comp.
Comp.
Comp.
Exam-
exam-
exam-
Exam-
exam-
exam-
Exam-
exam-
exam-
exam-
exam-
exam-
exam-
ple 1
ple 1
ple 2
ple 2
ple 3
ple 4
ple 3
ple 5
ple 6
ple 7
ple 8
ple 9
ple 10
Catalyst
mg
23
23.8
18.1
13.1
17.3
13
14.3
13.2
12
15.5
28
9.7
14.9
Donor
Type
2
2
2
2
2
2
1
1
1
1
1
1
1
Al/Ti
mol/mol
250
250
250
250
250
250
250
250
250
250
250
500
500
Al/Do
mol/mol
10
10
10
10
10
10
50
50
50
50
50
50
50
Hydrogen
mmol
70
70
70
800
650
450
600
1000
670
150
10
1000
1000
Temperature
° C.
70
70
70
70
70
70
70
70
70
70
70
80
70
Yield
g
593
546
457
370
497
357
463
442
435
435
513
630
608
MFR
g/10 min
4.2
3.7
6.3
113
87
82
82
92
85
4
0.14
79
73
Xylene
w-%
1.4
1.6
3
2.1
1.9
3.1
2.1
2.6
3.6
2.2
2.2
1.5
1.5
solubles
C6-C15 in
ppmw
50
81
95
240
430
480
200
606
520
160
20
340
464
polymer
Mw/1000
g/mol
336
363
320
154
171
166
162
163
160
362
—
170
173
Mn/1000
G/mol
81.4
75.8
62.4
21.7
18.4
18.5
26.1
10.2
11.7
39.6
—
23
18.9
MWD
4.1
4.8
5.1
7.1
9.3
9
6.2
16
13.7
9.1
—
7.4
9.1
SHI (0/50)
7
9.1
10.4
8.2
9.3
9.7
10.5
12.7
13.1
12
9.6
10.3
12.6
Donor 1 is dicylo pentyl dimethoxy silane
Donor 2 is cyclohexyl methyl dimethoxy silane
The examples 1-3 clearly show the decreased oligomer levels of the polymer compositions of the invention over the comparative compounds having the similar MFR, but representing conventional prior art.
Moreover, the oligomer content of the compositions of the invention is decreased also with higher MFR values (see example 3 of the invention).
The oligomer content can further be adjusted, if desired, e.g. by the choice of the temperature and donor.
The following examples illustrate one further embodiment of the present invention, namely the surprising possibility to produce low oligomer content propylene polymers and part of them having narrow molecular weight distributions, as discussed in the general part of the description above.
Example 1A
Preparation of the Soluble Mg-Complex
A magnesium complex solution was prepared by adding, with stirring, 78.0 kg of a 20% solution in toluene of butyloctylmagnesium (BOMAG A) to 27.1 kg 2-ethylhexanol in a 150 l steel reactor. During the addition the reactor contents were maintained below 35° C. After that 7.98 kg 1,2-phthaloyl dichloride was added and the reaction mixture was stirred for 60 minutes at 60° C. Solution was cooled to room temperature and stored.
Preparation of the Catalyst Component
19.5 ml titanium tetrachloride were placed in a 300 ml glass reactor equipped with a mechanical stirrer. Mixing speed was adjusted to 170 rpm. 1.0 ml of a solution in toluene of 3.0 mg polydecene and 2.0 ml Viscoplex 1-254, 32.0 g of the Mg-complex were added to the stirred reaction mixture over a 10 minute period. During the addition of the Mg-complex the reactor content was maintained below 30° C. The temperature of the reaction mixture was then slowly raised to 90° C. over a period of 30 minutes and held at that level for 30 minutes with stirring.
After settling and siphoning 100 ml of toluene containing 0.1 ml of triethylaluminium was added to the reactor. After 30 minutes mixing solids were settled and liquid was siphonated. Then the solids were washed with 60 ml heptane for 20 minutes at 90° C. and with 60 ml pentane for 10 minutes at 25° C. Finally, the catalyst was dried at 60° C. by nitrogen purge.
The catalyst contained 4.3 w-% titanium.
Polymerization of propylene with the catalyst was done in a 5 liter reactor with stirrer. 0.607 ml triethyl aluminium (TEA) (=Al/Ti molar ratio 250), 0.103 ml dicyclo pentyl dimethoxy silane (donor 1) (=Al/Do molar ratio 10) and 30 ml pentane were mixed and allowed to react for 5 minutes. Half of the mixture was added to the reactor and the other half was mixed with 19.9 mg of the catalyst. After 10 minutes the catalyst/TEA/donor 1/pentane mixture was added to the reactor. 8 mmol hydrogen and 1400 gram propylene were added into the reactor and the temperature was raised to 80° C. within 20 minutes while mixing. The reaction was stopped after 30 min at 80° C. by flashing out unreacted propylene.
MFR of the polymer was 0.55 and broadness as measured with rheology (SHI(0/50)) was 7.2. The other results are shown in following table.
Example 2A
Preparation of the Liquid Mg-Complex
A magnesium complex solution was prepared by adding, with stirring, 40.5 kg of a 20% solution in toluene of butyloctylmagnesium (BOMAG A) to 14.0 kg 2-ethylhexanol in a 90 liter steel reactor. During the addition the reactor contents were maintained below 30° C. Stirring was continued 30 minutes, at which time reaction was complete. Then 4.1 kg 1,2-phthaloyl dichloride was added and stirring of the reaction mixture at 60° C. was continued for another 30 minutes and then let to cool down and stored.
Catalyst Synthesis
Into the 90 l reactor, 32 kg TiCl 4 was added. Then 28.8 kg of aforesaid complex was added keeping the temperature in the reactor below 35°. After that 1.24 kg Viscoplex 1-254 and 6.0 kg heptane was added. The temperature was increased to 90° C. and kept 40 min to get solid particles. After stopping the mixing and letting the catalyst settle, the liquid was removed by siphonation. The product was washed with a preheated mixture of toluene (45 kg) and a di ethyl aluminium chloride (DEAC)/toluene mixture (0.235 kg; 30 wt.-% DEAC in toluene) at about 80° C. and two times with heptane (25 kg) so that the temperature at end of second heptane was about 30° C. Product was finally mixed with white oil and stored as slurry.
Titanium content in the catalyst/oil mixture was 0.92 w-% and solid content in the mixture was 20% giving Titanium content in the dry catalyst 3.8 w-%.
Polymerisation in this example was done in accordance with example 1A, but using the catalyst described in this example. Al/Ti ratio was 150 and Al/Do ratio 5. Hydrogen amount was 15 mmol. 161 mg catalyst/oil mixture was used.
MFR of the polymer was 0.85 and broadness (SHI(0/50)) was 7.6. The other results are seen in the following table.
Comparative Example 1A
The catalyst used in this example was MCM1 from Basell. This catalyst is a typical fourth generation porous high activity catalyst. Titanium content was 2.4 w-%. The polymerisation was done in accordance with example 1, except that hydrogen amount was 10 mmol. MFR of the polymer was 0.2 and broadness (SHI(0/50)) was 11.5. The other results are seen in the following table.
Comparative Example 2A
This example was done in accordance with example 1A, with the exception that the catalyst was prepared in accordance with the Finish patent No. 88047. This catalyst can be described as a normal 4 th generation, high isotacticity, high activity Ziegler-Natta catalyst for polymerisation of propylene. The catalyst is a transesterified Ziegler-Natta catalyst with Titanium content 2.1 w-% and was supported on spray crystallised MgCl 2 . The hydrogen amount was 30 mmol. The polymer had MFR 0.41 and broadness (SHI(0/50)) 9.7. The other results are seen in the following table.
Example 3A
The catalyst prepared in example 2A was used in this example. 72 mg of the oil/catalyst mixture was used. The polymerisation was done in accordance with example 1A, except that Al/Ti molar ratio was 250 and Al/Do molar ratio was 50, temperature 70° C., time 60 minutes and hydrogen amount 750 mmol. MFR of the polymer was 45 and broadness (SHI(0/50)) 8.9. Molecular weight distribution (MWD) from size exclusion chromatography (SEC) was 7.3. The other results are seen in the following table.
Example 4A
This example was done in accordance with example 3A, except that hydrogen amount during polymerisation was 1000 mmol. MFR of the polymer was 91 and broadness (SHI(0/50)) was 9.5 MWD was 7.4 The other results are seen in the following table.
Comparative Example 3A
This example was done in accordance with example 4A, except that the catalyst used was the catalyst described in Comparative example 2A. MFR of the polymer was 92 and broadness (SHI(0/50)) was 12.7. MWD was 16. The other results are seen in the following table.
Comparative Example 4A
This example was done in accordance with example 4A, except that the catalyst used was the catalyst described in Comparative example 1A and that hydrogen amount was 670 mmol. MFR of the polymer was 85 and broadness (SHI(0/50)) was 13.1. MWD was 13.7. The other results are seen in the following table.
Example 5A
The catalyst prepared in example 1A was used in this example. 14.9 mg catalyst was used. The polymerisation was done in accordance with example 1A, except that Al/Ti molar ratio was 250, cyclo hexyl methyl dimethoxy silane was used as external donor, Al/Do molar ratio was 10, temperature 70° C., time 60 minutes and hydrogen amount 550 mmol. MFR of the polymer was 45 and broadness (SHI(0/50)) 6.6. MWD was 6. The other results are seen in the following table.
Example 6A
This example was done in accordance with example 5A, except that the amount of hydrogen was 780 mmol. MFR of the polymer was 80 and broadness (SHI(0/50)) was 6.6 MWD was 4.8. The other results are seen in the following table.
Comparative Example 5A
This example was done in accordance with example 5A, except that the catalyst described in Comparative example 2A was used and that the hydrogen amount was 650 mmol. MFR of the polymer was 87 and broadness (SHI(0/50)) 9.3. MWD was 9.3. The other results are seen in the following table.
Comparative Example 6A
This example was done in accordance with example 4A, except that the catalyst used was the catalyst described in Comparative example 1A and that hydrogen amount was 450 mmol. MFR of the polymer was 82 and broadness (SHI(0/50)) was 9.7. MWD was 9.1. The other results are seen in the following table.
Example 7A
This example was done in accordance with example 1A, except that the hydrogen amount was 150 mmol. MFR of the product was 5.9 and MWD broadness was 4.1. The other results are seen in the following table.
Example 8A
The ZN catalyst used in this example was prepared according to patent WO03/000754, example 7, and had Ti content 2.84 w-%. Polymerisation was done in accordance with example 7A, except that the hydrogen amount was 300 mmol and polymerisation time 60 min. MFR of the product was 23 and MWD broadness 4.6. The other results are seen in the following table.
Example 9A
This example was done in accordance with example 5A, except that the hydrogen amount was 70 mmol. MFR of the product was 5.6, MWD broadness 4.0 and SHI(0/50) 5.4. The other results are seen in the following table.
Comparative Example 7A
This example was done in accordance with example 9A, with the exception that the catalyst described in Comparative example 2A was used. MFR was 3.6, MWD broadness 5.7 and SHI (0/50) broadness 9.8. The other results are seen in the following table.
Comparative Example 8A
This example was done in accordance with example 9A, with the exception that the catalyst described in comparative example 1A was used. MFR was 6.5, MWD broadness 4.6 and SHI (0/50) broadness 10.3. The other results are seen in the following table.
Example 10A
This example was done in accordance with example 4A, except that Al/Do molar ratio in polymerisation was 25, hydrogen amount 1000 mmol and polymerisation temperature 80° C. MFR was 62 and oligomer content 188 ppmw. The other results are seen in the following table.
Comp.
Comp.
Comp.
Comp.
Ex.
Ex
ex.
ex.
Ex
Ex
ex.
ex.
Ex
1A
2A
1A
2A
3A
4A
3A
4A
5A
Donor
type
1
1
1
1
1
1
1
1
2
Al/Do
mol/mol
10
10
10
10
50
50
50
50
10
Temp
° C.
80
80
80
80
70
70
70
70
70
Time
min
30
30
30
30
60
60
60
60
60
H2
mmol
8
15
10
30
750
1000
1000
670
550
Yield
g
196
336
496
472
641
410
442
435
551
Activity
kgPP/gcat
9.8
10.4
13
22.2
44.2
29.9
33.5
36.3
37
MFR
g/10 min
0.55
0.85
0.2
0.41
45
90.5
92
85
45
XS
w-%
1.7
1.4
0.9
1.1
1.9
2.4
2.6
3.6
2.1
FTIR isotacticity
%
95
96.2
95.3
97
100.4
100.3
102.2
99.9
96.7
Tm
° C.
165.7
165.9
165.2
166.5
162.3
161.8
162.3
161.4
160.3
Crystallinity
%
50
40
43
53
42
55
47
45
41
Tcr
° C.
120.4
119.5
116.9
116.3
118.8
118.9
120.3
118.9
118.3
Mw/1000
g/mol
189
163
163
160
185
Mn/1000
g/mol
26
21.9
10.2
11.7
30.6
Mw/Mn
7.3
7.4
16
13.7
6
SHI (0/50)
7.2
7.6
11.5
9.7
8.9
9.5
12.7
13.1
6.6
Oilgomers
ppmw
Comp
Comp.
Comp.
Comp.
Ex
ex.
ex.
Ex
Ex
Ex
ex.
ex
Ex
6A
5A
6A
7A
8A
9A
7A
8A
10A
Donor
type
2
2
2
1
1
2
2
2
1
Al/Do
mol/mol
10
10
10
10
10
10
10
10
25
Temp
° C.
70
70
70
80
80
70
70
70
80
Time
min
60
60
60
30
60
60
60
60
60
H2
mmol
780
650
450
150
300
70
70
70
1000
Yield
g
605
497
357
271
524
589
410
677
624
Activity
kgPP/gcat
39.3
28.7
27.5
26.8
27.9
33.4
20.8
30.6
39
MFR
g/10 min
80.2
87
82
5.9
23
5.6
3.6
6.53
62
XS
w-%
2.4
1.9
3.1
1.2
1.2
1.6
2
3
1.4
FTIR isotacticity
%
97.8
100.9
98.8
98.2
99.4
93.3
96.2
94.2
101.7
Tm
° C.
159.4
161.3
160.5
164.1
163.3
160.5
164.2
162.1
Crystallinity
%
47
51
47
45
53
51
42
46
Tcr
° C.
117
118.9
118.6
117.5
118
116.3
118.5
115
Mw/1000
g/mol
167
171
166
290
213
312
371
325
168
Mn/1000
g/mol
34.8
18.4
18.5
70.2
45.9
78
65.4
70.1
30.2
Mw/Mn
4.8
9.3
9
4.1
4.6
4.0
5.7
4.6
5.6
SHI (0/50)
6.6
9.3
9.7
5.4
9.8
10.3
6.3
Oilgomers
ppmw
188
Examples 1B and 2B and Comparative Example 1B
Polymers of the Invention Prepared in a Two Stage Polymerisation Process
Some of the catalysts exemplified above were furthermore used for polymerisation reaction in a pilot plant comprising a loop reactor and a gas phase reactor. The relevant process conditions and results are summarized in the following description and tables.
The examples 1B and 2B of the invention and the Comparative Example were prepared in a continuous multistage process in pilot scale comprising a loop reactor and a fluidised bed gas phase reactor as follows:
The catalyst used was a highly active, MgCl2-supported Ziegler-Natta catalyst prepared according to example 1A (for further description of the emulsion/solidification preparation method of the catalyst, reference is made to WO2004029112). The catalyst is also characterized in Table 2. Triethyl aluminium was used as a cocatalyst with Al/Ti molar ratio of 200. The catalyst was prepolymerised in a known manner in the presence of propylene and the co-catalyst in a separate prepolymerisation step. Then propylene, and hydrogen were fed together with the prepolymerised catalyst into the loop reactor which operated as a bulk reactor at conditions given in Table 2 (production of loop fraction). Then the polymer slurry stream was fed from the loop reactor into the gas phase reactor and more propylene and hydrogen were fed in the gas phase reactor (production of the gas phase reactor fraction in the presence of the loop-fraction to obtain the matrix component). The polymerisation conditions therein are given in the tables below. These examples are representative for TF applications. The catalyst used in the comparative example was a stereospecific transesterified MgCl2-supported Ziegler-Natta catalyst prepared according to U.S. Pat. No. 5,234,879.
Table for Examples 1B, 2B and Comparative Example 1B
Comparative
Catalyst type
Example 1B
Example 2B
Example 1B
Donor type
1
1
1
AI/donor ratio (mol/
49
49
mol))
Loop
Temperature ° C.
80
80
MFR (g/10 min)
13
12
XS %
3
3
GPR
Temperature ° C.
80
80
MFR2 (g/10 min)
10.0
11.0
XS (%)
1.9
2.0
Pellet MFR
11
11
12
Ethene (wt-%)
0.0
0.2
0.3
Zero viscosity Pa * s
2695
2638
2825
SHI (0/50)
5.3
5.1
6.6
PI
3.3
3.3
3.7
G′ (2KPA)
439
429
517
Tm (° C.)
163.7
160.6
158.0
Cryst (%)
55.0
52.0
50.5
Tcr (° C.)
124.8
121.5
116.6
Tensile Modulus
1710
1590
1370
(MPa)
Tens, Stress at
36.7
35.3
27.4
yield (Mpa)
Tensile strain at
8.1
8.7
6.1
yield (%)
Charpy Impact,
3.7
3.6
4.3
notched (kJ/m 2 ),
23° C.
Examples 3B to 5B
Polymers Prepared in One Stage Pilot Loop Reactor
Examples 3B and 4B of the invention: The catalyst was the same as in examples 1B and 2B above. In Example 5B of the invention the catalyst as described in example 1 was used. Examples 3B-5B were prepared in a loop reactor according to that as described for Examples 1B and 2B, except that the polymerisation temperature was 70° C.
Table of Examples 3B to 5B
Catalyst type
Example 3B
Example 4B
Example 5B
Donor type
2
2
2
AI/donor ratio (wt/wt)
30
20
20
Ethylene wt-%
MFR2 (g/10 min)
27
27
26
XS (%)
3.9
2.7
3.1
Pellet
Zero viscosity (Pas)
1208
1200
1141
SHI (0/50)
7.6
7.1
7.9
PI
3.8
3.6
3.6
G′ (2KPA)
540
511
576
Tm (° C.)
161.7
162.4
163.0
Cryst (%)
50.0
50.0
50.0
Tcr (° C.)
117.0
116.9
117.6
Tensile Modulus (MPa)
1460
1480
1510
Tens. Stress at yield (Mpa)
33
34
34
Tensile strain at yield (%)
9.3
9.0
8.8
Charpy Impact, notched
3.0
2.9
2.9
(kJ/m 2 ), 23° C.
These examples demonstrate that the present invention achieves the desired polymer properties, such as low oligomer content and/or narrow molecular weight distribution without requiring post polymerisation steps, such as regularly required in the prior art. | The invention is directed an alpha-olefin homo- or copolymer composition comprising at least one (i) alpha-olefin homo- or copolymer component, wherein the alpha-olefin homo- or copolymer composition comprises a decreased amount of C6-C15-oligomers. | 2 |
This application is a U.S. national stage filing of International Application No. PCT/ES2009/070001 with international filing date of Jan. 2, 2009.The international Application claims priority of application CL00242008 filed Jan. 4, 2008.
FIELD OF THE INVENTION
The invention object of the present patent application relates to an integrated system for detecting, locating and identifying antipersonnel and antitank mines for application in humanitarian demining through a GPR based non-invasive electromagnetic geophysical technique.
DESCRIPTION OF PRIOR ART
Conventional antipersonnel mine detection has been carried out mainly through methods that are not different from those used during Second World War, that is, a human operator uses a metal detector and performs a thorough and slow scanning on the affected area. High false alarm rate leads to slow, very dangerous and expensive detection. Adjusting the detectors to decrease false alarm rate involves that some mines are not detected.
In the national and international scope, the situation is critical since there are no modern techniques, no reliable data to allow for carrying out good decision making with respect to demining process. It is thus apparent that in the absence of these advances, uncertain investments will still be made which will not generate knowledge, which will not involve country stakeholders that must and can generate value in this scope and do not consider fundamental variables which unnecessarily involves and increases risk.
Detection of hidden or even buried explosives is carried out through a wide range of methods: vapor release, driven neutrons and subsequent detection of gamma rays emitted in their interaction, X-rays, laser beams causing no detonation explosive ignition, electrical conductivity and other interactive ones in which the explosive, for example, a mine, is provided with a signaling system that can be activated by a signal sent by a mine field cleaning complementary tool. Location is also possible by direct contact, through a long, thin shaft.
A further technique to eradicate antipersonnel mines hosted in the outermost layer of the Earth is with the help of electromagnetic waves (airborne radar) based tools. This technique involves sending a radar signal and analyzing the return signal generated from wave reflections occurring in the discontinuities of the dielectric constants in the penetrated material, such as either ground and mine, or ground and rock. The image resolution is higher if the signal wavelength is lower, however the shorter the wavelength the lower the penetration into the ground.
However, very good results have been obtained by combining GPR (Ground Penetrating Radar) with EMI (Electromagnetic Induction). The great advantage of GPR is that changes in the dielectric are detected resulting in a wide range of mine housings that can be detected. An interesting advantage of GPR is that it can obtain horizontal sections from the subsoil at different depths forming a 3D subsoil image. The main disadvantages however are: non-homogeneous subsoil which may result in a large amount of false alarms in addition to very sensitive performance to complex interactions such as metal content, radar frequency, soil mixtures and surface soil smoothness (humidity, etc.).
GPR has been established as one of the best techniques for subsoil research. However, mine detection using GPR is complex mainly due to the material present in the site, such as rocks, stones, metals, waste, etc., dominating the obtained data and hiding mine information. This material varies with the irregularity of the surface and soil conditions, which involves taking into account uncertainty in measurements. For this reason it is necessary to have a good GPR obtained signal processing to retain only mine signals.
Electrical Impedance Tomography (EIT) uses electric currents to create an image of the site conductivity distribution. These systems use a two dimensional arrangement of electrodes placed on the surface, which collect signals from conductivity distribution that can provide information regarding the presence of mines. Among its advantages, it should be mentioned that it is sensitive to metal and non-metal detection as both may create anomalies in the conductivity; in addition, it exhibits good performance on wet grounds, and equipment is relatively simple and inexpensive. The main disadvantage however, is that sensors should be in contact with the surface, which may cause the mine to be detonated. A further disadvantage is that it does not work properly in very dry areas such as deserts or rocky surfaces since conductivity is very weak. In addition, it only serves for detecting objects that are very close to the surface.
X-rays (XBS) are usually used to produce images of an object through attenuation undergone by photons passing therethrough. Since photons penetrating the ground are impossible to be captured, as it is unfeasible to place an X-ray detector under the mines, X-Ray Compton scattering principle is used by these systems, i.e. photons irradiated by the object when receiving X-rays are captured. It is thus possible to design a system having a transmitter and receiver device on the surface. The use of this technology has three major advantages: a) the obtained information is sufficient to detect all the evenly placed mines, b) non-metal mines can be detected, c) mines placed under a variety of ground conditions can be detected (including different types of vegetation). One of the main features pointed by the authors is obtaining of an image that can be easily analyzed by a human operator. However, due to the low range of energy needed by the sensor, the use of this technology is limited to surface mine detection (less than 10 cm from the surface), since an appropriate signal to noise will not be obtained by mines placed deeper. Additionally, as such equipment works with X-rays, it is necessary to have all the measurements to ensure that no operator is exposed to radiation.
Infrared and hyperspectral methods detect abnormal variations in electromagnetic radiation reflected or emitted by mine surfaces or the ground located immediately over the mine. The idea is that the areas where mines are located these energies are reflected in a manner different from the surrounding areas. Thermal sensors are enclosed within this group exploiting the phenomenon of the difference between ground and mine temperature variations as a result of nocturnal cooling and diurnal heating rates. Thermal methods have high performance only in homogeneous ground. Laser light or high power microwave radiation can be used to induce these differences. Among the advantages it should be noted that these methods are safer since no physical contact with the surface is required; equipments used are light and image acquisition is fast. The main disadvantage however is that performance is highly variable and it greatly depends on environment characteristics. Some authors have stated that these sensors need greater maturity.
Acoustic and seismic systems emit sound waves with loudspeakers to shake ground surface. The sensors used capture waves reflected from the ground and the mines. Mine detection is made possible by the difference both in bandwidth and frequency of these waves. There are special sensors that need not be in contact with the surface. Trials show that this technique is very suitable for anti-tank mine detection. Since through this technology mechanical differences between soil and mine are detected, they can supplement the information obtained by the magnetic sensors, in order to obtain a better performance. They have a low false alarm rate, however the detector may be misled by bottles or cans. The main disadvantage is that they are able to detect deeply buried mines. In addition, sampling speed is too slow: 2-15 min/m 2 . There is also research on the use of ultrasound for characterizing underground materials, however there is still the need for further researching in this area in order to objectively determine which are the operating ranges for this technique.
Vapor detector technique uses the fact that a small percentage of explosive gets out in vapor from through cracks and structures in mine housing. The idea of the explosive vapor detectors is to determine whether vapors belonging to the explosives in the area. There are two major trends in this field: biological and chemical detectors.
Explosive detection techniques seek for directly detecting the explosive, and not the mine metal housing or shape. Among them there are those based on the nuclear quadripole resonance (NQR) principle and other methods that employ the interaction of neutrons with explosive components. These methods become of high importance in detecting explosives in passenger baggage.
However, relative numbers of specific atoms can at best be measured through these methods, but the present molecular structure can not be determined through them. This for example causes water to produce such a large number of false alarms, due to its high hydrogen content. By building images from this information it is possible to analyze the signal as a whole, thus achieving false alarms from mines to be discriminated. These techniques can be used as complementary to confirm other detections.
It is noted that there are several technologies for mine detection, however, each having good performance only in one type of mine. In deciding which technology is to be used it is also necessary to make a study on the environment in which mines are (vegetation, ground homogeneity and type), as well as a study of the type of mines laid and the type of explosives used, in some cases this information can be obtained either with a careful initial inspection or from already public military reports because of the ending of the conflict that led to mine the fields.
U.S. Pat. No. 5,673,050 to Moussally George; Ziemicki Robert; Fialer Philip A; Heinzman Fred Judson, entitled “Three-dimensional underground imaging radar system”, discloses a system comprising a radar antenna including a transmitter and receiver device on a radar platform for transmitting an interrupted, frequency modulated continuous wave (FMCW) addressed to the area of interest below the surface and receiving a reflected wave (echo wave) from the area of interest underground. Such FMCW is transmitted when an airborne vehicle circumscribes the area of interest below the surface, and said reflected wave (echo wave) is being received by the radar antenna when the area of interest below the surface is circumscribed by said airborne vehicle. This system uses stepped frequency, with the air platform path being in a straight line. This type of frequency allows greater sharpness to be obtained and the airborne vehicle path allows the illuminated area to be optimized. In addition, this system includes positioning means (using GPS data), in communication with the radar antenna for locating said radar antenna relative to the area of interest below the surface.
U.S. Pat. No. 5,502,444, to Kohlberg Ira, entitled “Method and apparatus for improving the signal-to-clutter ratio of an airborne earth penetrating radar” discloses a method for detecting objects below the surface using an aircraft with radar pulse for performing detection, from distances greater than 50 meters, while using a continuous transmission radar for performing detection of distances under 50 meters.
US patent application 2006087471 to Hintz Kenneth J., entitled “Syntactic landmine detector” discloses a method for landmine identification through an indicator system referred to as syntactic parameters. It only delivers information on the existence of landmines.
However, none of these documents uses ground marking based methodology for georeferencing, which provides better accuracy and safety in determining the coordinates of the detected objects in the image, resulting in a final risk map whether it is paper or digital. Stepped frequency is employed in transmission allowing high resolution to be obtained. Furthermore, this invention allows on site remapping of the coordinates of the object detected by radar.
Then, the object of the present invention is to provide an integrated system for detecting, locating and identifying antipersonnel and antitank mines for application in humanitarian demining by using a GPR based noninvasive electromagnetic geophysical technique. This system delivers consistent solutions to mitigate the effects of antipersonnel and antitank mines and increase certainty on certification of raised fields.
SUMMARY OF THE INVENTION
The system for detecting, locating and identifying antipersonnel and antitank mines for application in humanitarian demining considers the integration of a mathematical modeling and computer simulation subsystem, considering the calculation of natural frequencies and resonance of antipersonnel mines on unbounded, inhomogeneous environment, in order to determine the optimal frequencies at which a synthetic aperture radar (SAR) is to be operated for mine detection; a radar design and building subsystem, considering design, integration, installation and operation of a synthetic aperture radar based on selected frequencies in modeling and simulation subsystem, implemented in an air platform of the helicopter type and adjustment for use on the ground; an image re-building and processing subsystem, which considers identification and classification of signals delivered by the radar and their conversion to output data through the implementation of efficient built-in algorithms and software allowing subsequent mine georeferencing; and a georeferencing and risk map subsystem considering the orientation of the data submitted by the image re-building and processing subsystem and general and specific location of each mine placed on the ground, through the use of differential geographic position system (DGPS) technology and adjustment and display dedicated software.
Therefore, there is provided a system for detecting, locating and identifying objects above the ground and below the ground comprising a previously referenced area of interest, an airborne vehicle circumscribing the area of interest which is provided with a radar including an antenna with respective transmitter and receiver device, signal processing means, data storage media and graphical interface means, wherein said radar is a ground penetration radar (GPR) of the heterodyne type, wherein the signal transmitted by the antenna generates a light beam from a strip of land and consists of a sinusoidal electromagnetic signal whose frequency is varied in predetermined and accurate steps. This signal is mixed with the received (reflected) signal, resulting in two sets of values corresponding to the phases of each frequency step or stage. These sets of values obtained over successive scannings (as the antenna moves) are stored in the storage media and then processed in processing means for obtaining a final image or map of the location of said objects above the ground and below the ground.
There is also provided a method for detecting, locating and identifying objects above the ground and below the ground comprising an area of interest, an airborne vehicle circumscribing the area of interest that is provided with a radar comprising an antenna with its respective transmitter and receiver device, signal processing means, data storage media and graphical interface means, comprising:
setting a rectangular reference framework based on a point of reference, base points and orientation points around the area of interest; transmitting a sinusoidal electromagnetic signal whose frequency is varied in predetermined and accurate stepped stages to illuminate the area of interest and reference framework; mixing the reflected signal with the signal sent to obtain sets of values corresponding to the phases of each frequency step or stage. These sets of values are obtained over successive scannings as the antenna moves; applying the inverse Fourier transform to the sets of values in order to obtain a set of range measurements for objects in the ground illuminated by the radar light beam; sequentially aligning each of the range measurements in the same sequence in which they were obtained from successive scannings for obtaining an image; processing said image through the use of a detection algorithm which accurately determines the location of each object in the scanning region, obtaining a map of location of objects above the ground and below the ground; calibrating the map in order to obtain distances and heights expressed in length (meters, inches, etc.). georeferencing the calibrated image for submitting space coordinate data in the image, according to the following sub-steps:
geometrically encoding the calibrated image to identify and assign a code to each measured point in creating the framework; building a point densification based on points obtained on the ground in order to generate a digital field model, with which the image is orthogonally rectified and all vertical distortions and exaggerations in the image are corrected; correlating the pixels in the image in the above point and imposition of ground point coordinates, controlling the location with the points generated in densification;
drawing up a risk map containing object position vectors; and remapping the object coordinates in the image obtained in the previous step for marking on the ground.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are included to provide a better understanding of the invention, are incorporated herein and are pail of this description, illustrate one embodiment of the invention, and together with the description, serve the purpose of explaining the principles of the invention.
FIG. 1 shows a general diagram of the present invention.
FIG. 2 shows a plan diagram of the present invention.
FIG. 3 shows a diagram of base point georeferencing.
FIG. 4 shows a ground area covered by the beam of light transmitted by the radar of the present invention.
FIG. 5 shows the direction of movement of the antennae and the area scanned by the radar of the present invention.
FIG. 6 shows a graph of phase components delivered by the radar for three objects located on the ground area covered by the beam of light.
FIG. 7 shows a graph of other phase component delivered by the radar for three objects located on the ground area covered by the beam of light.
FIG. 8 shows a graph of the Fourier transform of the graphs in FIGS. 6 and 7 .
FIG. 9 shows a sequence of range measurements allowing the position of objects on the ground to be determined.
FIG. 10 shows a diagram of the system for remapping the location of the object detected by radar.
FIG. 11 shows a flow chart of the mine detection method of the present invention
DETAILED DESCRIPTION OF THE INVENTION
The system ( 1 ) for detecting, locating and identifying of antipersonnel and antitank mines ( 2 ) in its application to humanitarian demining, mainly comprises an airborne vehicle ( 3 ), preferably of the helicopter type, which incorporates a radar ( 4 ), preferably a stepped frequency radar with the respective antenna and graphical interface. In this type of radar, frequency scanned is not continuous but stepped, synthesizing a high-bandwidth pulse compression technique through the use of sequential transmissions of discrete frequencies on an established band. Its advantages are allowing high resolution as well as continuous wave transmission, both features being highly significant in short-range and high-precision applications, in addition since its architecture is of the heterodyne type, it is possible to set very narrow bandwidths as well as frequency generation is easily achieved through the use of frequency synthesizers, which ensure the required frequency step accuracy. Finally, this type of radar eliminates the problem of the proportionality of the existing bandwidth in continuous frequency scanned radars. The signal transmitted by the antenna consists of a sinusoidal electromagnetic wave whose frequency is varied in predetermined and accurate staggered steps. The received signal is mixed with the signal sent, yielding two sets of values corresponding to the phases of each frequency step or stage. FIG. 6 shows in graphical form one example for the first set of values and FIG. 7 shows one example for the second set of values.
In order to obtain accuracy and resolution suitable for detecting antipersonnel mines ( 2 ), the frequency range of operation of the radar should be between 750 MHz and 3000 MHz. These frequencies allow penetrating the ground about 1 meter deep ( 200 ) and they are high enough to achieve a suitable detection of small objects. The number of frequency steps set to obtain the necessary resolution is at least 128. The upper limit should not exceed 512 steps in order not to extend too much the radar scanning time and, consequently, extend the signal acquisition time to form the image. On the other hand, and also in order to obtain an appropriate resolution to the task of detecting of small size antipersonnel mines ( 2 ), it is necessary that frequency steps have an appropriate value.
For this reason and in order to obtain a 5 cm resolution, 256-step frequency, it is required that each frequency increase is 11.72 MHz. Note that if the number of steps is halved, i.e., 128, it is required that each step is increased twice in frequency for achieving the same resolution, i.e. 23.44 MHz.
Since the objects to be detected will be at a close distance, 10 to 50 m, is not required the power of the radar ( 4 ) to be high. Indeed, excess power may be counterproductive as many rebounds can affect signal reading by receiver. It has been established that outputs ranging from 10 W to 250 mW are sufficient for the required work.
Before beginning the task of illuminating the mined area with the frequency signal, a reference framework ( 5 ) must be developed subsequently allowing the image to be georeferenced and then the detected coordinates of the mines ( 2 ) to be determined.
As shown in FIGS. 1 and 2 , a reference point ( 8 ) is set corresponding to a geodetic reference point linked to an official geodetic network ( 9 ) in the particular country, such as the SIRGAS-CHILE National geodetic network, which is to be constituted at the point from which the coordinates to be obtained will be derived and on which a GPS Base unit will be positioned for measuring of the points in the area of the mine field ( 201 ).
Such reference point ( 8 ) should be a point of the milestone type, consisting of an upright metal pole supported by a concrete base or the like, located no more than 2 km away from of the mine field ( 201 ), ideally as close as possible thereto and which will serve as a basis for differential mode GPS (DGPS) geodetic measurements. In addition, it must also be georeferenced with static differential measurement linked to a point in the geodetic network. If this point of geodetic network is no more than 50 km away from the area where the reference framework is being developed corresponding to the mined area, then the reference point ( 8 ) must be created with 4 hours of measurement in differential method in DGPS system. On the contrary, if the point in the geodetic network is over 50 km from the working area of the reference framework, then the measurement in differential method should be increased up to 6 hours with 1-second interval. These measurements will be taken by using the static measurement method with a differential GPS for 4 to 6 hours, as appropriate, allowing each vertex of the working area having coordinates with an accuracy of about ±2 cm.
In general for all static measurements, the following parameters have to be considered: Datum: WGS-84; elevation mask: 10°; Measurement range: 5″; Minimum number of satellites: 5; Instrumental height: measured on the ground; System: GPS+GLONASS.
Once measurements for the reference point ( 8 ) have been taken, a baseline ( 10 ) (network point-reference point) is processed and with this the accurate coordinates of the reference point ( 8 ) are obtained.
The next step corresponds to create the rectangular reference framework ( 5 ) comprising points adjacent and close to the area of the mine field ( 201 ), referred to as base points ( 11 ), and they are marked with metal discs, such as aluminum, about 10 cm in diameter attached to a pole of about 50 cm high.
Location of these base points ( 11 ) is at the four corners of the rectangular reference framework ( 5 ) and at the centers of the larger sides thereof. Depending on the extent of the rectangular reference framework ( 5 ) more intermediate base points could be considered.
On the other hand, orientation points ( 12 ) are also installed in each of the vertices of the rectangular reference framework ( 5 ) and further out of these vertices with respect to the base points ( 11 ), such that they are arranged crossways to the base points ( 11 ) as shown in FIG. 2 , and distant therefrom at a distance of about one meter, with the purpose of having a better orientation of the reference framework ( 5 ). These points of orientation ( 12 ) are not georeferenced, they are only for orientation and should be under radar scanning region.
Once all of said base points ( 11 ) have been located, they must be georeferenced with a GPS unit through the real time kinematik (RTK) method, whose base GPS unit ( 14 ) is installed on the reference point ( 8 ). This base GPS unit ( 14 ) must be in continuous operation, avoiding any discontinuity of operation while performing the measurement of the base points ( 11 ). With this method coordinates of each base point ( 11 ) are obtained with an accuracy of ±2 cm.
Once the reference framework ( 5 ) has been obtained, the lighting of the mine field area ( 201 ) is performed by using, for this purpose, the radar ( 4 ) implemented on the airborne vehicle ( 3 ).
The ground penetration radar (GPR) ( 4 ) consists of a discrete step electromagnetic wave generator equally spaced in frequency in the range of 750-3000 MHz. The system further comprises an antenna ( 25 ) comprising a transmitting antenna for illuminating the area to be scanned and a receiving antenna for receiving the signal reflected from the ground surface and the underground objects.
Basic methods needed to obtain a signal with relevant information to subsequently generate an image of the subsurface components using the GPR system are set out hereinbelow.
Illumination of the covered ground area ( 16 ) comprises scanning with the transmitting antenna ( 25 ), at a height ( 277 ) from 5 to 30 meters, allowing a suitable portion of the ground to be covered. Both the radar ( 4 ) and the antennae are mounted on a helicopter for being able to safely evolve on the mine field. The transmitting and receiving antennae mounted on the outside of the airborne vehicle ( 3 ) must aim at an angle ( 26 ) ranging from 35° to 55° from the vertical.
During illumination, the antenna ( 25 ) of the radar ( 4 ) scans in discrete frequency steps (minimum 64, maximum 512 steps). Each frequency scanning allows key information for determining the distance to each of detectable objects to be obtained, which are on the covered ground area ( 16 ) by the light beam. This frequency scanning must be fast (split second), such that by moving the antennae it is possible to obtain a set of distance measurements for the different objects. The locus of the distances will allow the location of each of the objects composing the scene to be pinpointed.
To obtain a pattern that is reliable and possible to be processed for object loci, both the transmitting and the receiving antenna ( 25 ) of the radar ( 4 ), mounted outside the airborne vehicle ( 3 ), must be moved at a constant speed 27 ) and at a constant height ( 277 ), along a vertical line perpendicular to the vertical and to the light beam axis. With this, a scanning of a strip on the ground ( 16 ) is obtained.
During scanning ( 28 ), all the information received by the receiving antenna and pre-processed by the receiver of the radar is stored in a computer fitted in the airborne vehicle ( 3 ). This information is the raw material for subsequently generating images of the ground surface and subsoil. In addition, it is necessary to store continuous data of speed and height of the airborne vehicle ( 3 ), obtained from a precision GPS mounted therein. These must be synchronized with the data received by the receiving antenna of the radar, so as to allow calibration of the image or map coordinates.
Data obtained from scanning ( 28 ) performed by the radar ( 4 ) on the area of the mine field ( 201 ) is extracted and submitted to the equipment intended for image processing and acquisition.
The first step consists in generating range sequences. Data obtained from the GPR radar receiving antenna and preprocessed by the GPR receiver are processed on a computer using the inverse Fourier transform. This allows obtaining a sequence of measurements of distances (range measurements) to the different objects found in the subsoil.
As initially stated, two sets of values corresponding to the phases for each frequency step are generated by mixing of the signal transmitted by the radar with the sent one. FIG. 6 shows the first set of 128 values obtained from a simulated version of the radar signal ( 4 ) for three objects located on the ground area ( 16 ) covered by the light beam at distances of 5, 12 and 18 m. FIG. 7 shows the second set of values obtained from the same simulation for the same three objects located on the ground area ( 16 ) covered by the light beam at distances of 5, 12 and 18 m. With these two signals, formed by both sets of values, and through a mathematical process based on the inverse Fourier transform, it is possible to obtain a chart of distances for the three objects, as shown in FIG. 8 . Note that in FIG. 8 distances appear in positions 27 , 65 and 97 . To obtain the distance in meters it is necessary to multiply these values by the resolution given by frequency steps used in the simulation, which is 0.1852 m.
When both the transmitting and the receiving antenna ( 25 ) move in a straight line forming a scanning, as shown in FIG. 5 , the position of objects lying on the ground through can be determined by a series of range measurements as scanning progresses. The object(s) located on the ground and within the area covered by the light beam ( 16 ) of the radar ( 4 ) begin to approach the antennae, until reaching a minimum value, and then move away therefrom until leaving the area covered by the beam ( 16 ). Successive range measurements made will indicate a displacement in object positions to the left when approaching the antennae, and then a displacement to the right when moving away.
The second step corresponds to the combination of range measurements. The set of range measurements is combined for obtaining an object image. This operation consists in sequentially aligning each of the range measurements in the same sequence they were obtained in the scanning process in the airborne vehicle ( 3 ), as shown in FIG. 9 . This figure corresponds to the image of a set of 5 objects distributed on an area of 48×48 meters, obtained from a computer-simulated scanning.
The combined set of range measurements is processed by using a detection algorithm allowing the location of each object in the scanning region to be accurately determined, as shown in FIG. 9 , where asterisks depict the location of each object. Finally the image is calibrated, that is distances and heights are expressed in meters.
The processed and calibrated image contains the representation of the objects captured by the radar, which require the application of georeferencing procedures to obtain the object coordinates contained therein comprising geometric encoding, which involves moving from the processed and calibrated image to the scope on the ground and corrections to the angle of incidence of the image, based on measurements of the points created in the reference framework. This allows a correspondence between the position of the points in the final image and its location on a given map projection, in summary: submitting spatial coordinate data in the original image, and thus representing all of the objects contained in the image.
For the location of ground data in a georeferenced and projected space, it is necessary to analyze the data obtained on the ground and project them on the ground. Based on the GPS points Excel format file generated by the software of the equipment the code of each point measured in creating the framework is determined and assigned.
Conversion scope is used, which method consists in positioning values of the image and locating it on the ground to project it based on a coordinate system. It is necessary to know the geometry of the image creation, height of the airborne vehicle ( 3 ), time delay between signal from the region closest to the radar with respect to the furthest one, and ground elevation. Resampling, corresponding to a pixel rearrangement, is used to create the even spacing between them (in the scope domain on the ground) across the complete image width.
Scope conversion on the ground may be performed either during signal processing or during image processing. It is usually applied after radiometric correction. The approach and the algorithms used are dependent on analysis purposes.
Polynomial transformation uses best fit. Radar image obtained without georeferencing or orthogonal rectification is changed to fit a map projection using various orders.
Higher order transformations require a larger number of ground control points (GPS) for being able to produce the transformation model. High order does not ensure better accuracy. Image points are generally approached to GPS ones by a higher order transformation, but errors in points away from GPS ones may be increased. Having said that, the GPS points are located on a georeferenced map.
The next step in georeferencing is building a point densification based on points obtained on the ground in order to generate a digital field model, with which the image can be orthogonally rectified and all deformations and vertical exaggeration in the image corrected.
The next step in georeferencing is the correlation between image pixels and imposition of ground point coordinates, controlling the location with the points generated through densification. Based on pixel size as well as image spatial resolution the mean square error is determined. Having the image corrected to points, cubic convolution method is used, which takes the weighted average of sixteen surrounding pixels to estimate the digital value for the final corrected image, this process provides a good record and appearance of the product.
Once the above has been performed, the risk map can be made. It is generated in a 60×60 cm paper format. This risk map contains object position vectors in DXF and SHP format (ESRI Shapefile and DXF drawing exchange format of other CAD software.)
As a leading factor in a topographic map flying height is a precision indicator whereby the tolerance determined by the scale for an image obtained with radar data will be the pixel size, this being referred to as spatial resolution of the image. In case of validation these maps should contain centimeter-level precision whereby their scale should not exceed 1:250 (1 mm on the paper equals 25 cm on the ground).
These hybrid maps contain image relating to ground roughness with 20% transparency, plus a grid defined over a maximum distance of one meter. Above the distortion itself of the AP and AT (anti-personnel and anti-tank) objects, there will be a vector generated at the center of each AP and AT mines, to obtain these elements it is necessary a magnification of the object image located in the center thereof.
The system concludes and its objective is achieved when marking on the ground the location of the object detected by the radar, that is, remapping, (see FIG. 10 ).
Remapping ( 23 ) consists in taking the obtained coordinates of the objects in the image and using a DGPS unit, marking them on the ground. For this purpose real time kinematik (RTK) measurement method is used, for which a base and mobile GPS, a radio modem system, and the previously created remapping system are used.
As shown in FIG. 10 , the base GPS ( 29 ) is installed on the reference point ( 8 ) in the mine field ( 201 ).
As it is known the reference framework ( 5 ), that allows for a high level of security for approaching the mine field ( 201 ), starts remapping the coordinates of the object detected by the radar ( 4 ). This requires scheduling a book, which is part of the mobile GPS unit ( 30 ), and which makes it possible to submit the coordinates of the detected objects to be remapped.
Once the coordinates have been submitted in the book of the mobile GPS unit ( 30 ), the following is displayed on its screen: graphical display of the submitted points; display of plane coordinates, display of direction and distance, display of distance in meters, and direction in degrees as well as the position of the mobile GPS unit ( 30 ) itself.
In graphic remapping one of the submitted coordinates is selected, and the unit graphically displays the distance thereto and its direction referred to magnetic north.
The antenna ( 31 ) of the mobile GPS ( 30 ) is installed on the system created for remapping ( 23 ). This system created for remapping ( 23 ) comprises a tripod where a metal structure containing a 4 m long polycarbonate stick moving in a radial and retractable fashion is to be installed. At one end of this stick the antenna ( 31 ) of the mobile GPS ( 30 ) is provided having a vertical elbow such that measuring of coordinates visible on the book screen will be actually where the identified mine is.
When the antenna ( 31 ) of the mobile GPS ( 30 ) is in the required coordinate, the fact that it was obtained a coincidence between the submitted coordinate and that obtained by the mobile GPS ( 30 ) is shown graphically and through a sound alarm by the mobile GPS unit ( 30 ),
In order to mark the location of the object (mine) on the ground, a paint mark ( 32 ) is used, which is released from a polycarbonate stick end under the antenna ( 31 ) of the mobile GPS ( 30 ), this being operated from a device fitted on the tripod. | The invention relates to a system and method for detecting, locating and identifying objects located above ground or below ground in an area of interest, comprising an airborne vehicle which circumscribes the area of interest and which includes a built-in radar having an antenna with a respective transmitter and receiver, signal-processing means, data-storage means and graphical interface means. According to the invention, the area of interest has been pre-referenced and the radar is a heterodyne ground penetration radar (GPR). The signal transmitted by the antenna generates a beam that illuminates a strip of earth, consisting of a sinusoidal electromagnetic signal having a frequency that is varied in precise pre-determined progressive steps. This signal is mixed with the received (reflected) signal, thereby producing two sets of values corresponding to the phases of each frequency step or stage. Said sets of values, which are obtained throughout successive sweeps (as the antenna moves), are stored in the storage means and subsequently processed in the processing means in order to obtain a final map or image of the location of the objects above ground or below ground. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a filing under 35 U.S.C. 371 of International Application No. PCT/GB2008/000430 filed Feb. 6, 2008, entitled “Process for the Preparation of Ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride,” claiming priority of Indian Patent Application No. 215/MUM/2007 filed Feb. 6, 2007, which applications are incorporated by reference herein in their entirety.
FIELD OF INVENTION
The present invention relates to an improved process for the preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride which is a key intermediate used in the preparation of anagrelide, (6,7-dichloro-1,5-dihydroimidazo[2,1-b]quinazolin-2 (3H)-one.
BACKGROUND OF THE INVENTION
Anagrelide, is a potent reducer of platelet count induced by a variety of aggregating agents and has the following structure
U.S. Pat. No. 4,146,718 discloses the process for the preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride from 1,2,3-trichlorobenzene as depicted in Scheme I via 2,3-dichloro-6-nitrobenzonitrile, which involves the use of poisonous reagents, such as cuprous cyanide. Cyanation is carried out at a temperature of 165° C. which is highly exothermic, uncontrollable and not scalable. 2,3-dichloro-6-nitrobenzonitrile has extreme toxic and skin-irritant properties. Diborane is a flammable gas, used for the reduction of 2,3-dichloro-6-nitrobenzonitrile. The reduction reaction is exothermic, uncontrollable and not feasible industrially.
U.S. Pat. No. 5,801,245 discloses process for the preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride from 2,3-dichloro toluene as depicted in Scheme II.
The reaction involves a radical halogenation of the toluene group. The material is purified by column chromatography at each stage which makes the process more tedious and it is not viable industrially. The use of a chromatographic solvent, such as chloroform (which is a known carcinogen), is disadvantageous with respect to industrial application.
US 2003/0060630 discloses a method for making ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride from 2,3-dichloro benzaldehyde as depicted in Scheme III.
In step (b), the reduction reaction is carried out in high boiling solvents like toluene. The reduction in step (b) and the chlorination in step (c) are sluggish. Also, the chlorination reaction is exothermic and uncontrollable, which leads to formation of more impurities and thereby resulting in low yield (page 4, column 2, and page 5, column 1: 65%). Hence, this prior art process is not viable for industrial scale up.
Because of the difficulties encountered in the processes disclosed in the prior art, there is a need to develop more efficient and economical synthetic route for the preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride, which is suitable for industrial scale up. The present invention relates to a new process for the synthesis of Ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride.
An object of the present invention is to provide a novel process for the synthesis of the intermediate ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride.
Another object of the present invention is to provide novel process for synthesis of anagrelide.
Yet, another object of the present invention is to provide a simple novel process which is useful for application on an industrial scale.
SUMMARY OF THE INVENTION
The present invention provides a new process for the synthesis of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride, a compound of Formula (I)
which comprises the following steps;
(i) reducing 2,3-dichloro-6-nitro benzaldehyde Formula (III),
to form 2,3-dichloro-6-nitro benzyl alcohol of Formula (IV),
(ii) reacting 2,3-dichloro-6-nitro benzyl alcohol with suitable compound to obtain compound of Formula (V),
where R constitutes a suitable leaving group, which may not be hydrogen.
Preferably, the group R is selected from:
i) —SiR 1 3 , where R 1 is a substituted or unsubstituted alkyl. R 1 is preferably C 1 to C 6 , more preferably C 1 to C 4 straight or branched chain alkyl group. Most preferably R 1 is methyl.
ii) —CH 2 Ar, where Ar stands for aryl, preferably a substituted or unsubstituted phenyl group.
iii) —COOR 2 , where R 2 is alkyl or aryl. When R 2 is alkyl it is preferably C 1 to C 6 , more preferably C 1 to C 4 straight or branched chain alkyl. When R 2 is alkyl, it is most preferably methyl. The aryl group is preferably a substituted or unsubstituted phenyl group.
iv) sulfonates such as —SO 2 R 3 , where R 3 is alkyl or aryl. When R 3 is alkyl it is preferably C 1 to C 6 , more preferably C 1 to C 4 straight or branched chain alkyl. When R 3 is alkyl, it is most preferably methyl. The aryl group is preferably a substituted or unsubstituted phenyl group.
The most preferred —O—R groups in Formula (V) are mesylate, besylate and tosylate.
(iii) Alkylating the compound of Formula (V) with glycine ethyl ester in a suitable solvent, using a base, and then converting to a salt, preferably the hydrochloride salt, in a suitable solvent, to obtain compound of Formula (I).
It will be appreciated that step (i) is optional, in that the compound of Formula (IV) may be provided by any suitable means.
Thus, according to one aspect of the invention there is provided a process for the synthesis of a compound of Formula (V)
where R is a suitable leaving group, which may not be hydrogen, said process comprising reacting a compound of Formula (IV)
with suitable compound to obtain the compound of Formula (V).
Preferably, the reaction is carried out in the presence of an alkyl or aryl sulphonyl halide, especially a methyl sulphonyl halide, such as methyl sulphonyl chloride. Preferably also, the reaction is carried out in the presence of a base, such as triethylamine. Preferably, the reaction is carried out at a temperature of 35° C., or less.
According to another aspect of the invention there is provided a process for preparing a compound of Formula (I′),
said processing comprising alkylating a compound of Formula (V)
where R constitutes a suitable leaving group, which may not be hydrogen (preferably as described above) with glycine ethyl ester in a suitable solvent, using a base.
The compound of Formula (I′) may be converted to a salt in the presence of a suitable solvent. Most preferably, the compound of Formula (I′) is converted to the hydrochloride salt in a suitable solvent, to obtain compound of Formula (I).
The reaction temperature of the alkylation step is preferably 60° C., or lower, more preferably 40° C., or lower.
According to another aspect of the invention there is provided a compound of Formula (V):
where R is a suitable leaving group, which may not be hydrogen, and is preferably as described above.
In another aspect, the present invention provides a process to prepare anagrelide of Formula (II) which comprises the following steps:
(i) Forming a salt of the compound of Formula (I′) (the hydrochloride salt is preferred, Formula (I) using the process described above; (ii) reducing the nitro group of Formula (I) with a suitable reducing agent to convert it to an amine of Formula (VI),
(iii) reacting the compound of Formula (VI) with a cyanogen halide to form compound of Formula (VII),
wherein halide is chloro, bromo or iodo;
(iv) cyclising compound of Formula (VII), to form compound of Formula (II), i.e. anagrelide.
The anagrelide formed by the processes described above may be combined with a suitable carrier to make a pharmaceutical composition. Such compositions may be used to reduce platelet count induced by a variety of aggregating agents.
DETAILED DESCRIPTION OF THE INVENTION
The process according to the invention will now be described in more detail below.
The process for the preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride according to the invention is depicted in the reaction scheme below. Brackets indicate intermediates that could be isolated but are not usually isolated in the integrated process.
wherein R represents a suitable leaving group, wherein R is not hydrogen and preferably has the meaning described above in relation to Formula (V).
(i) 2,3-dichloro-6-nitrobenzaldehyde, of Formula (III) is reduced to give the corresponding alcohol of Formula IV. The reducing agent is preferably selected from sodium borohydride, potassium borohydride, sodium cyanoborohydride and tetramethyl ammonium borohydride. The reaction is preferably carried out in a solvent, which is preferably a C 1 to C 6 straight chain or branched chain alcohol, especially methanol, ethanol, isopropanol or n-butanol; or a chlorinated solvent such as chloroform, methylene chloride, carbon tetrachloride, ethylene chloride, with methylene chloride being preferred. The reaction is preferably carried out at a temperature ranging from 0° C. to the reflux temperature of the solvent, and the reaction time may vary from 1 to 3 hrs.
(ii) According to a particular feature of the present invention, the hydroxymethyl functionality of phenyl methyl alcohol of Formula (IV) is protected with suitable protecting group R (as discussed above in relation to Formula (IV) using variety of methods.
Various organic or inorganic bases may be employed, such as triethylamine, pyridine or potassium carbonate, with triethylamine being preferred.
For example, one method includes reacting 2,3-dichloro-6-nitro benzyl alcohol—Formula (IV)—with alkyl or aryl sulphonyl halide in the presence of a base, such as triethylamine or the like, preferably at a temperature of 35° C., or less, for a time preferably less than 8 hours. The sulphonyl halide is preferably added to the compound of Formula (IV) over an extended period of time at a temperature of 30° C., or less, with stirring. The reaction is not exothermic, which avoids impurity formation. The organic layer may then be separated, washed with an acid and neutralized with a base, then concentrated to obtain the compound of Formula (V).
The alkyl sulphonyl halide is preferably C 1 to C 6 , more preferably C 1 to C 4 straight or branched chain alkyl. The alkyl sulphonyl halide is most preferably methyl sulphonyl halide. In the aryl sulphonyl halide, the preferred aryl groups are phenyl and p-toluyl.
Steps (i) and (ii) are preferably carried out without isolating the alcohol of Formula (IV).
(iii) According to yet another embodiment of the present invention the compound of Formula (V) is alkylated with glycineethylester in an organic solvent, such as acetonitrile, using base and a catalyst preferably, dimethyl amino pyridine. Suitable bases for this reaction are carbonates or alkali metal hydroxides, preferably anhydrous potassium carbonate. Typically, the reaction is carried out at a temperature less than or equal to 60° C., more preferably less than or equal to 40° C. After completion of the reaction, the reaction mass is filtered, and concentrated under vacuum to obtain ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine, which is further converted to hydrochloride salt in suitable organic solvent such as ethyl acetate to obtain ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride, a compound of Formula (I).
In prior art processes, where the leaving group is bromo (e.g. U.S. Pat. No. 5,801,245, column 5, example 3, lines 6-25), the reaction with glycine ethyl ester hydrochloride requires 14 hrs reflux in THF-triethylamine, which requires further purification by column chromatography. Yield—87% w/w—Efficiency 60.20%.
In prior art processes, when the leaving group is chloro (e.g. US 2003/0060630, page 5 [0040]), the reaction is carried out in high boiling solvent toluene, at 80° C. for 24 hrs using 10% w/w cetyltrimethylammonium bromide, which is an expensive catalyst—Efficiency 66-71%.
In the process according to the invention, where the leaving group is mesyl or tosyl, for example, the reaction can be carried out at low temperature of 37-40° C. in acetonitrile as solvent, potassium carbonate as base and 0.2% w/w dimethyl amino pyridine as catalyst. Due to the low reaction temperature, a relatively small level of impurities is formed giving high yield and purity—Efficiency 75.52%.
In another aspect of the present invention, intermediate ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride of Formula (I), prepared by using process of the present invention, is converted to anagrelide by
(iv) Reducing nitro group of Formula (I) with suitable reducing agent to convert it to amine of Formula (VI). Various methods may be employed to carry out the nitro reduction, such as catalytic hydrogenation or metal reduction. Normally catalytic hydrogenation is carried out in the presence of noble metal catalysts, such as palladium, platinum, or Raney Nickel on a carbon support. The source of hydrogen may be hydrogen gas or a hydrogen donating compound such as ammonium formate. Metal reduction may be carried out using tin, iron, or using stannous chloride with an acid.
In the forgoing processes the preferred reduction is metal reduction using stannous chloride and a preferred acid is hydrochloric acid. The reaction is preferably carried out at a temperature of 50° C., or less. After completion of the reaction, the reaction mass is filtered, suspended in water and basified to obtain an amine of Formula (VI).
(v) Reacting the compound of Formula (VI) with cyanogen halide to form the compound of Formula (VII) where the halide is as defined above, i.e., chloro, bromo or iodo. Normally the reaction is carried out using cyanogen bromide in an aprotic inert organic solvent such as toluene, chlorobenzene, xylene, heptane and hexane. A preferred solvent is toluene. A preferred reaction temperature is from 80-150° C.
(vi) Cyclising compound of Formula (VII), to form a compound of Formula (II), i.e. anagrelide. The compound, ethyl-N-(5,6-dichloro-3,4-dihydro-2(1H) iminoquinazoline-3-acetate hydrobromide of Formula (VII), is readily converted to anagrelide of Formula (II) with an organic base, such as triethylamine or dimethylaniline. The reaction may be carried out in an inert solvent.
The intermediate compound of Formula (V) represents a novel compound, per se, and this novel intermediate forms further aspects of the present invention.
In the present invention, the reaction is carried out by protecting the hydroxymethyl functionality of compound of Formula (IV). When using methane sulphonyl chloride in methylene chloride, the reaction was less exothermic than in the prior art, and was more controllable with less impurity formation.
Overall yield:—76% (From compound III to compound I) with HPLC purity of 98.5%
EXAMPLES
Further details of the invention are given in the examples below. The examples are provided for illustration only.
Example 1
Preparation of 2,3-dichloro-6-nitro benzyl methane sulphonate, a Compound of Formula (V)
Methylene chloride (2000 ml) and sodium borohydride (120 g) were charged to a clean and dry flask and chilled to 0-5° C. Methanol (100 ml) was added slowly over a period of 20 minutes followed by 2,3-dichloro-6-nitro benzaldehyde solution (500 g in 2000 ml of methylene chloride) over a period of 2 hours maintaining the temperature at 0-5° C. and the contents were stirred at 0-5° C. for 1 hour. After completion of reaction, water (3000 ml) was added and stirred for 10 minutes. The organic layer was separated, dried over sodium sulphate and was filtered to get a clear filtrate.
To the clear filtrate triethylamine (460 ml), was slowly added over a period of 1 hour at 10-15° C., then methane sulphonyl chloride (325 ml) was added drop wise over a period of 2 hours maintaining temperature of 10-15° C. and the reaction mass was allowed to attain room temperature. Further the reaction mass was stirred at room temperature for 5 hours and after completion of reaction, the organic layer was washed with water (1000 ml) twice, followed by 1N HCl solution (1000 ml) twice, 5% Sodium bicarbonate solution (1000 ml) twice, water (1000 ml) twice and was dried over sodium sulfate. The clear organic layer was concentrated under vacuum below 40° C. to give the title compound which was used in the next step.
Example 2
Preparation of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride, a Compound of Formula (I)
2,3-dichloro-6-nitro benzyl methane sulphonate (Example 1) was dissolved in acetonitrile (2400 ml). To this reaction mass were charged anhydrous Potassium carbonate (480 g), dimethyl amino pyridine (480 mg) and glycine ethyl ester (240 g) at room temperature. The contents were stirred at 37-40° C. for 24 hours. After completion of reaction, the insolubles were filtered, washed with acetonitrile (120 ml). The clear filtrate was concentrated and stripped off using ethyl acetate (240 ml).
Further ethyl acetate (1200 ml) was added, chilled the contents to 5-10° C., adjusted the pH to 2.0 using IPA-HCl at 5-10° C. The contents were stirred at 5-10° C. for 1 hour. The solids were filtered, washed with chilled ethyl acetate (120 ml) and dried under vacuum at room temperature for 4 hours to give the title compound (595 g, 76% yield, 98.5% HPLC purity).
Example 3
Preparation of Anagrelide, a Compound of Formula (II)
a) Preparation of Ethyl-5,6-dichloro-3,4-dihydro-2[1H]-imino quinazolin-3-acetate hydrobromide
A solution of stannous chloride dihydrate (1850 gms) in concentrated HCl (6.7 liters) was added slowly to a cooled solution of ethyl-N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride (595 gms) in concentrated HCl (5.15 liters) maintaining temperature 15-20° C. over a period of 2 hours. The contents were heated slowly to 40-45° C. and stirred for 1 hour at 40-45° C. After completion of reaction, the contents were cooled to 15-20° C., maintained for 15 minutes and filtered.
The solids thus obtained were suspended in water (2.9 liters), adjusted the pH of the reaction mass to 8.0-9.0 using potassium carbonate solution (prepared by dissolving 376 gms of potassium carbonate in 4.25 liters of water) at 0-5° C., extracted into toluene (3.0 liters×3), dried over sodium sulphate and clarified.
To the clear toluene layer, added Cyanogen bromide solution (prepared by dissolving 222 gms of cyanogen bromide in 655 ml of toluene) in 30 minutes maintaining temperature 15-20° C. and stirred at 25-30° C. for 2 hours. The contents were heated slowly to 105-110° C. maintained for 16 hours at 105-110° C. After completion of reaction, the mass was cooled to 15-20° C. and stirred for 45 minutes. Filtered the material, washed with chilled toluene (1.3 liters). The material was slurried in toluene (470 ml) at 15-20° C. for 1 hour, filtered, washed with cold toluene (160 ml) and dried under vacuum at 50-60° C. for 8 hours to give the title compound (445 gms).
b) Preparation of 6,7-Dichloro-1,5-dihydroimidazo[2,1-b]quinazolin-2(3H)-one [Anagrelide]
A mixture of ethyl-5,6-dichloro-3,4-dihydro-2(1H)-iminoquinazolin-3-acetate hydrobromide (445 gms), isopropyl alcohol (4.45 liters) and triethylamine (246 ml) was refluxed for 2 hours. After completion of reaction, the mixture was cooled to 20-25° C., filtered, washed with chilled isopropyl alcohol (1.0 liters) and dried under vacuum at 50-55° C. for 6 hours to give the title compound (285 gms).
It will be appreciated that the invention described above may be modified within the scope of the claims. | The invention relates to a process for the preparation of anagrelide, and for the preparation of intermediates for use in preparing anagrelide. The invention also relates to the intermediates per se, in particular compounds of Formula (V):
where R constitutes a suitable leaving group, which may not be hydrogen. The R group may be selected from: (i) —SiR 1 3 , (ii) —CH 2 Ar, (iii) —COOR 2 , and (iv) sulfonates such as —SO 2 R 3 . | 2 |
This application is a continuation of Ser. No. 07/630,622, filed Dec. 20, 1990, now abandoned.
FIELD OF THE INVENTION
The present invention relates to digital signal transmission systems and is particularly concerned with full-duplex optical transmission of signals over an optical waveguide with a transmitter/receiver device on each end thereof.
BACKGROUND OF THE INVENTION
Communication networks often require bidirectional transmission links. The most direct implementation in fiber optics is to use two unidirectional waveguides, one waveguide for data transmission in a first direction, the other waveguide for data transmission in the reverse direction, with distinct transmit and receive devices on either end of each of the waveguides. Alternatively, a single waveguide can be used with optical splitter at opposite ends of the waveguide to provide optical paths to transmitters and receivers at each end of the waveguide. Optical splitter can be designed to have directional coupling characteristics, i.e. signals to the far end ("go" signals) can be separated from signals from the far end ("return" signals), enabling full-duplex communications. However, reflection points in the link, such as connectors, lead to cross talk between the communications paths. The suppression of crosstalk requires extra effort, such as the application of wavelength division multiplexing (WDM) or frequency division multiplexing (FDM). The former utilizes different optical carriers, the latter utilizes different electrical carriers for the go and return paths.
As an alternative, it has been suggested that a laser diode, or light emitting diode (LED) could be used as both a light transmitter and a light receiver. This would thereby remove the need for optical splitter and photodiodes at the ends of the optical waveguide to separate transmit and receive paths. The potential benefits of using a single device as both an emitter and a detector are great in that the parts count and assembly time are reduced considerably. However, transmission systems to date, using such a concept, have not been capable of full-duplex transmission.
An example of a method and apparatus that has been created for the purpose of bidirectional communication over a single waveguide can be found in U.S. Pat. No. 4,879,763 issued Nov. 7, 1989 in the name of T. H. Wood, entitled "Optical Fiber Bidirectional Transmission System", in which a bidirectional optical communications system is described using a multiple quantum well structure as both a photodetector and light modulator.
Technologies for using a laser or light emitting diode (LED) as a light emitter and detector are described in the following U.S. patents: U.S. Pat. No. 4,773,074 issued Sep. 20, 1988 in the name of Hunsperger et al., entitled "Dual Mode Laser/Detector Diode for Optical Fiber Transmission Lines", in which a semiconductor diode device for direct optical coupling to an optical signal transmission apparatus is disclosed; U.S. Pat. No. 4,195,269 issued Mar. 25, 1980 in the name of Ettenberg et al., entitled "Two-way Single Fiber Optical Communication System", in which is disclosed an injection laser whose characteristics vary upon radiation impinging on the laser such that the laser operates as a light detector; and U.S. Pat. No. 4,687,957 issued Aug. 18, 1987 in the name of V. P. O'Neil, entitled "Fiber Optic Transceiver", in which a half-duplex transceiver circuit is disclosed in which a single diode acts as both the light emitter and the light detector.
Since an optical device can only act as an emitter or detector at any one point in time, but not simultaneously, half-duplex seems inevitable for bidirectional transmission over a single fiber. The present invention proves otherwise.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a system wherein full-duplex transmission may occur over a single optical waveguide with a single transmit/receive device on each end of the optical waveguide.
Stated in other terms, the present invention is an optical apparatus for transfer of full-duplex data signals over an optical waveguide, the apparatus comprising: an electro-optic transducer means, coupled to the optical waveguide, responsive, in a first mode, to drive signal pulses to produce corresponding transmit optical signal pulses for transmission along the optical waveguide and responsive, in a second mode, to received optical signal pulses to produce detected signal pulses and reception means including decoding means, for generating a receive bit of the data signals in response to the detected signal pulses and driving means including encoding means responsive to each transmit bit of the data signals, for generating a pair of the drive signal pulses, each pair of drive signal pulses being within one bit period of the respective transmit bit of the data signals and wherein the time delay between each pulse of the corresponding pair of transmit optical signal pulses differs from that of the pair of receive optical signal pulses, and wherein the duty cycle of the transmit optical signal pulses is such that for any phase relationship between transmission of the pairs of transmit signal optical pulses and reception of the pairs of receive optical signal pulses there is no interference between at least one transmit optical signal pulse and one receive optical signal pulse of each pair and switch means for switching the electro-optic transducer means between the first mode and the second mode, for coupling the driving means to the electro-optic transducer means in the first mode, and for coupling the electro-optic transducer means to the reception means in the second mode.
The present invention also encompasses a method of transmitting full duplex data signals over a common path, the method comprising the steps of receiving over the common path a pair of receive signal pulses representing each receive bit of the full-duplex data signals and encoding each transmit bit of the data signals as a pair of drive signal pulses, the pair of drive signal pulses being within one bit period of the respective transmit bit of the data signals and transmitting over the common path a pair of corresponding transmit signal pulses in response to the drive signals, the time delay between each pulse of the pair of transmit signal pulses being different from that of the pair of receive signal pulses, and a duty cycle such that for any phase relationship between transmission of the pairs of transmit signal pulses and reception of the pairs of receive signal pulses there is no interference between at least one transmit signal pulse and one receive signal pulse of each pair.
Furthermore the invention defines a full-duplex transmission system for transfer of first and second data signals comprising: an optical waveguide for carrying optical signals and first and second electro-optic transducer means, coupled to the optical waveguide at opposite ends thereof, responsive, in a first mode, to first and second drive signal pulses, respectively, to produce first and second corresponding transmit optical signal pulses for transmission along the optical waveguide and responsive, in a second mode, to the second and first transmit optical signal pulses to produce first and second detected signal pulses and first reception means including first decoding means for generating first receive bits of the second data signals in response to first detected signal pulses and second reception means including second decoding means for generating second receive bits of the first data signals in response to second detected signal pulses and first driving means including first encoding means for generating a pair of the first drive signal pulses in response to each transmit bit of the first data signals, each pair of first drive signal pulses being within one bit period of the respective transmit bit of the first data signals and wherein the time delay between each pulse of the corresponding pair of first transmit optical signal pulses differs from that of the pair of second transmit optical signal pulses, and a duty cycle such that for any phase relationship between transmission of the pairs of first transmit optical pulses and the pairs of second transmit optical pulses there is no interference between at least one first transmit optical signal pulse and one second transmit optical signal pulse of each pair and second driving means including second encoding means for generating a pair of the second drive signal pulses in response to each transmit bit of the second data signals, each pair of second drive signal pulses being within one bit period of the respective transmit bit of the second data signals and first switch means, for switching the first electro-optic transducer means between the first mode and the second mode, for coupling the first driving means to the first electro-optic transducer means in the first mode, and for coupling the first reception means to the first electro-optic transducer means in the second mode and second switch means for switching the second electro-optic transducer means between the first mode and the second mode, for coupling the second driving means to the second electro-optic transducer means in the first mode, and for coupling the second electro-optic transducer means to the second reception means in the second mode.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be further understood from the following description, by way of example, with reference to the accompanying diagrammatic drawings in which similar reference numerals are used in the different figures to denote similar parts and in which:
FIG. 1 is a block diagram of a transmission system between a central office and an end user;
FIG. 2 is a block diagram illustrating in greater detail the functioning of the transmission system of FIG. 1;
FIGS. 3a-d are timing diagrams illustrating the relative timing of data transmission signals according to the present invention;
FIG. 4 is a timing diagram illustrating the relative timing of signals passing through an encoder means used in the transmission system of FIG. 2;
FIG. 5, which may be found on the first sheet of the drawings, is a timing diagram illustrating the relative timing of signals passing through the decoder means used in the transmission system of FIG. 2;
FIG. 6 is a state diagram illustrating the functioning of the decoder means used in the transmission system of FIG. 2.
DETAILED DESCRIPTION
FIG. 1 illustrates an example transmission system linking a central office 10 with an end user 20 via an optical waveguide 30. As illustrated, the end user 20 may communicate with the central office 10 either by digitized voice, as indicated by the telephone 21, or by data, as illustrated by the computer 22. At each end of the optical waveguide 30 is a line card block 15 and 25 respectively. Each line card block 15, 25 comprises a bidirectional electro-optic transceiver (BEOT) 14,24 which performs the receive function of converting optical signals to electrical signals and the transmit function of converting electrical signals to optical signals. Each BEOT 14,24 is coupled to the optical waveguide 30 via an electro-optic transducer means 17, 27 which converts electrical signals into light pulses when forward biased, and when reversed biased or zero biased can be used to convert light pulses to electrical signals. The electro-optic transducer means 17, 18 may be a laser, a light emitting diode (LED), or like element. The input/output (I/O) devices 18 and 28 can comprise such elements as analog to digital converters, digital to analog converters, first-in-first-out (FIFO) buffers, etc. to convert, monitor and control the data entering and leaving the BEOTs 14, 24.
FIG. 2 provides a more in-depth drawing of the block diagram of FIG. 1 further illustrating the BEOTs 14, 24. From this figure it is clear that the BEOTs 14, 24 each comprise a scrambler means 141, 241; an encoder means 142, 242; a switch means 143, 243; an amplifier means 145, 245; a clock recovery means 146, 246; a sampler means 147, 247; a decoder means 148, 248; a descrambler means 149, 249; a clock 190, 290; and an electro-optic transducer (EOT) 16, 26.
For ease of description, only BEOT 14 will be described, it being understood that the components and functioning of BEOT 24 are identical. However, it must be understood that although the BEOTs 14, 24 are conceptually identical, they will communicate with each other; each BEOT using data which has been encoded in a predetermined manner with respect to each other, as will be explained further.
The scrambler means 141, clocked by timing signals B from the clock 190, is provided to scramble any incoming data on the DATA IN G line (DATA IN R line in the case of line card block 25). The scrambler means 141 can be a standard SONET (Synchronous Optical NETwork) scrambler which is in common use in fiber optic transmission systems. The scrambled data signal C is then passed through the encoder means 142, clocked by timing signals A from the clock 190 the encoder means encodes each transmit bit of the scrambled data signal C as pairs of drive signal pulses D, the pairs of drive signal pulses being generated within a time interval equal to the bit period of the respective transmit bit of the scrambled data signal C. A control signal E is produced by the encoder means 142 which controls the switch means 143 and causes it to toggle between a transmit position Y and a receive position Z. In the transmit position Y, the pairs of drive signal pulses are passed on to the EOT 16 so that the data therein can be converted and launched into the optical waveguide 30 as the optical "go" signal. In the receive position Z, the optical "return" signal from line card block 25 is detected and converted into an electrical current by the EOT 16.
With reference to FIG. 3b, the switch means 143 is an electronic switch which is normally in the receive position Z, as illustrated by the base line 46. To transmit data, the switch means 143 is switched to the transmit position Y for short periods of time. A control signal E defines a time period for transmission by generating a transmit window 44. Pairs of drive signal pulses or "go" signal D is represented by data pulse pairs 42, 43. In response to the go signal D the electro-optic transducer means 17, emits light thus launching the optical "go" signal into the optical waveguide 30. The time periods for transmission are set such that the transmit window 44 is greater than each pulse of a transmitted data pulse pair 42, 43. This is to ensure that a) the electro-optic transceiver 16 has time to switch from the receive mode to the transmit mode and vice versa, and b) all electrical transients are kept away from the input of the sensitive amplifier means 145.
To receive data, the switch means 143 in response to the control signal E is switched back to its normal position, i.e. the receive position Z. In this position light pulses coming from the optical waveguide 30 are detected and converted into current pulses by the electro-optic transducer means 17 which is reversed, or zero, biased to thus operate as a detector. The amplifier means 145, which can be any typical amplifier, then converts the current pulses into voltage pulses After amplifying the voltage pulses they are sampled by the sampler means 147, which can be a D-type flip-flop, and processed by a clock recovery means 146, which can be a phase locked loop (PLL) circuit, to recover timing information. The clock recovery means 146 provides a clock input F for the sampler means 147 and furthermore provides a state timing signal G to the decoder means 148 which is identical to the state timing B. Once received encoded data H has been recovered from the voltage pulses it is decoded by the decoder means 148, which will be discussed in more detail further, and then descrambled by the descrambler means 149, which is typically a conventional descrambler adapted for SONET, similar to the scrambler means 141, to thus place received data on the DATA OUT R line (DATA OUT G line in the case of line card block 25).
In operation the reception of light pulses is not possible during the transmit windows 44, and conventional wisdom dictates half-duplex transmission. However, with the following discussion, it will be evident that the capability of full-duplex transmission exists.
To allow full-duplex transmission between the central office 10 and the end user 20, an encoding algorithm has been devised for the encoder means 142. The encoder means 142 encodes each transmit bit of the scrambled data signal C as one pair of drive signal pulses D, each pair of drive signal pulses D being generated within a time interval equal to one bit period of a respective transmit bit of the scrambled data signal C. The encoder means 142 divides each scrambled data signal C transmit bit period into twenty equal time intervals, each pulse of a pair of transmit optical signal pulses and each pulse of a pair of receive optical signal pulses occupies a time interval equal to one of the twenty time intervals. Preferably, the time delay between each pulse of a pair of transmit optical signal pulses differs from the time delay between each pulse of a pair of receive optical signal pulses by one quarter of a data signal bit period. Encoding of the data signals in this manner assures that although one pulse of the data pulse pair can be lost due to switching between receive and transmit modes at the EOT 16, 26, under certain phase conditions at least one of each pulse pair will be received which will be sufficient to recover the transmitted information and necessary timing information. Therefore, the "go" and "return" data encoded in this manner permit full duplex operation in the sense that under all operating conditions, i.e. all possible phasing relationships for transmit and receive signals optical, only one pulse of an incoming pulse pair may be blanked out by the EOT 16, 26 for a worst case phase relationship.
The encoding algorithm can be better understood with reference to FIGS. 3a-3d. In the "go" direction, transmit bits of the scrambled data signal C, for example logic ones, are encoded as pulse pairs 42, 43 in a 20 time period interval, i.e. a pulse will be transmitted during the second and twelfth (2, 12) time periods of the 20 time period interval, as illustrated in FIG. 3b. In the "return" direction, as viewed by line card block 15, logic ones are encoded by the encoder means 242 as pulse pairs 40, 41 in the 20 time period interval, e.g. a pulse will be transmit-ted during the second and seventh (2, 7) time periods of the 20 time period interval, as illustrated in FIG. 3a. A logic LO is transmitted if no light pulses are launched during the respective time intervals. Transmit windows 44 are provided, as described above, to allow the electro-optic transceiver 16 to switch from the receive mode to the transmit mode prior to the transmission of the "return" signal.
Alternatively, the "return" signal, as represented by data pulse pairs 40, 41, can be presented during the time periods 2 and 12 as illustrated in FIG. 3c, and the "go" signal, as represented by data pulse pairs 42, 43, can be injected during the time periods 2 and 7 as illustrated in FIG. 3d.
Consequently, with the arrangement described above, it is possible that one receive data of a pulse pair at the EOT 16 may be partially cut by the transmit window 44, and depending on what is left over for the sampler means 147, may or may not be registered. But, since the second pulse of the pulse pair is guaranteed to survive due to the encoding of the data, sufficient information is received to assert that a logic one was sent from the far end.
FIG. 4 is a timing diagram illustrating the timing of data signals into and out of the encoder 142. The state timing B is indicative of the time period of the data transmissions as discussed above. FIG. 4 illustrates the scrambled signal C fed into the encoder 142. The encoder 142 encodes the data and consequently outputs pairs of drive signal pulses D which are to be transmitted from line card block 15 to line card block 25. As is readily apparent, the pairs of drive signal pulses 42 which are output during states B or time periods, 2 and 12 and occurs approximately central to the transmit window 44.
FIG. 5 illustrates the timing of the data signals active in the decoder means 148. The decoder means 148 comprises a single integrated circuit state machine and may be a Read Only Memory (ROM). The state timing G is indicative of the time period of the data transmissions as discussed above. The received encoded data signal H is representative of the signal received from the line card block 25 and fed into the decoder means 148. Note that the receive data pulse pairs 40, 41 are presented during the second and seventh time periods of the 20 time period interval. The decoder means 148 accesses a look up table stored in the ROM to decode the received encoded data signal H and consequently output decoded data I.
The functioning of the decoder means 148 can be further understood from the state diagram of FIG. 6 and the following state machine rules.
DECODER STATE MACHINE RULES
1. Power On
states 21-31 are considered invalid;
states 1-20 are valid but out of sync will be detected;
the finite state machine (FSM) assumes state 0--out of sync (step 50).
2. State 0--Out of Sync State
FSM waits for a first `one` to be received, i.e. CDATA=1 (step 51);
if a `one` is not received, the FSM remains in state 0--out of sync (step 50);
if a `one` is received:
FSM assumes it is in position 2 of the 20 time period interval, i.e. BITCNT=2 (step 52);
FSM assumes state 3 (step 53);
an "error flag" EFLAG is initialized to `zero` (step 54);
a "received data" variable RX is initialized to `zero` (step 55);
FSM assumes a synchronized (SYNC) condition (step 56).
3. States 3 . . . 6, 8 . . . 20 (for a (2,7) encoding) (States 3 . . . 11, 13 . . . 20 for a (2,12) orthogonal coding)
if a `one` is detected, i.e. CDATA=1 for the first time (step 69):
the FSM sets the "error flag" bit EFLAG to `one`--however, the FSM stays in sync (step 70);
the FSM assumes STATE+1, i.e. the next sequential state (step 72);
if a `zero` is detected, i.e. CDATA=0, the FSM assumes STATE+1, i.e. the next sequential state (step 72);
if the "error flag" bit has previously been set, i.e. EFLAG=1 (step 68) and a `one` is detected, i.e. CDATA=1 (step 71), i.e. a second error has occured, the FSM assumes state 0--out of sync (step 50);
if the "error flag" bit has previously been set, i.e. EFLAG=1 (step 68) and a `zero` is detected, i.e. CDATA=0 (step 71), the FSM assumes STATE+1, i.e. the next sequential state (step 72).
4. States 2, 7/12
either a `one` or `zero` is valid in these states;
the data CDATA is stored in the received data variable RX, i.e. RX=CDATA (step 64);
if a `one` is detected, i.e. CDATA=1 (step 65):
a "data hold" bit is set to `one`, i.e. DHOLD=1 (step 66);
the "error flag" is reset, i.e. EFLAG=0 (step 67), i.e. the error that was previously detected was likely not an out of sync error;
if a `zero` is detected, i.e. CDATA=0 (step 65): the "data hold" bit is set to `zero`, i.e. DHOLD=0 (step 63); the FSM assumes a state of STATE+1, i.e. the next sequential state (step 72).
5. State 1
the "received data" variable is set equal to the "data hold" bit, i.e. RX=DHOLD (step 58);
the "data hold" bit is cleared, i.e. DHOLD=0 (step 59) ready for the next bit sequence;
same error checking as states 3 . . . 6, 8 . . . 20 (3 . . . 11, 13 . . . 20) (steps 68-71).
The decision as to which state (1-20) is processed is governed by step 57.
It is to be noted that as a single electro-optic transducer means 17 is to be used in the present invention as an emitter and a detector, the intrinsic (not drive circuit related) recovery time of the emitter to detector transition must be fast; i.e. in the case of an electro-optic transducer means 17 which is a laser the remaining laser-injected-carriers following laser turn-off must decay to a dark current value consistent with the required detection sensitivity of the electro-optic transceiver 16. Otherwise, a transmit-induced background photocurrent will adversely affect the received data.
Of coursse it can be readily realized that the transmission of the "go" and "return" signals could be during time periods other than (2,7) and (2, 12), respectively, or (2,12) and (2,7), respectively, as described by example above. However, to achieve full-duplex bidirectional communications over a transmission medium it is necessary to ensure that the data sent in opposite directions are encoded in the manner described, relative to each other. This ensures correct reception of the transmitted data, as well as the necessary timing information, regardless of the phasing relationships of the transmit and receive optical signals. Furthermore, as stated above, the described encoding of the data allows for full-duplex transmission over a single optical waveguide 30 with a single electro-optical transducer means 17 on each end of the optical waveguide 30, thus providing the advantage of cost savings over traditional dual or single waveguide systems, and improved transmission speeds over half-duplex transmission systems.
Numerous modifications, variations, and adaptations may be made to the particular embodiments of the invention described above without departing from the scope of the claims. | An optical apparatus for transfer of full-duplex data signals over an optical waveguide comprises electro-optic transducers, coupled to the optical waveguide at opposite ends thereof. The electro-optic transducers are responsive, in a first mode, to drive signal pulses to produce transmit optical signal pulses for transmission along the optical waveguide and responsive, in a second mode, to receive optical signal pulses detected by the electro-optic transducer means to produce detected signal pulses. Drivers, coupled to the electro-optic transducers, generate pairs of the drive signal pulses in response to each transmit bit of the data signals. Receivers, also coupled to the electro-optic transducers, generate receive bits of the data signals in response to at least one of each pair of the detected signal pulses. A switch switches the electro-optic transducer means between the first mode and the second mode, couples the driver to the electro-optic transducer means in the first mode, and couples the electro-optic transducer means to the receiver in the second mode. The time delay between each pair of the transmit optical signal pulses differs from the time delay between each pair of the receive optical signal pulses, and the duty cycle of the pulses is limited so that at any point along the optical waveguide there is no interference between at least one transmit optical signal pulse and one receive optical signal pulse of each pair. | 7 |
BACKGROUND OF THE INVENTION
This invention relates to a simplified process for the preparation of polyurethane urea elastomers in which solid, high-melting aromatic diamines are reacted with polyisocyanates or isocyanate prepolymers in a heterogeneous reaction.
The preparation of polyurethane urea elastomers from polyisocyanates, relatively high molecular weight polyhydroxyl compounds, and aromatic diamines is known. To guarantee reasonable processing times for reactive systems of such starting components, reactive aromatic isocyanates generally used on an industrial scale are preferably reacted with sluggishly reacting diamines. In practice, diamines that have been successfully used in this way are primarily aromatic diamines of which the basicity and, thus, the reactivity to isocyanates have been reduced by introduction of halogen or carboxy substituents. One example of such diamines is 3,3'-dichloro-4,4'-diaminodiphenylmethane ("MOCA") which has previously been the most widely used such diamine.
U.S. Pat. No. 3,891,606 discloses the crosslinking of isocyanate prepolymers of polyhydroxyl compounds and excess polyisocyanates with aromatic diamines in which the reactivity to isocyanate groups has been reduced by complexing with certain alkali metal salts. A disadvantage of this process is that it is confined to two special aromatic diamines. In addition, the complex between the aromatic diamine and the alkali metal salt must be prepared in a separate process step.
Another way to control the reaction rate between polyisocyanates and aromatic diamines is to carry out the reaction in an organic solvent. Processes of this type are disclosed, for example, in U.S. Pat. No. 3,926,922 and in Japanese 70/9195. A disadvantage of using organic solvents is obvious. The risk of fire and explosions is increased and the solvent must be recovered economically and ecologically in a further process step.
Before the present invention, little was known about the preparation of polyurethane ureas by reaction of polyisocyanates with aromatic diamines in heterogeneous phase. According to the prior art, aromatic diamines of relatively high melting point, which generally are of particular interest on an industrial scale, either are used in dissolved form, which involves the disadvantages just mentioned, or are reacted with polyisocyanates in the melt. The processing of aromatic diamines in the melt is described, for example, in U.S. Pat. No. 3,926,922 (mentioned above) or in German Auslegeschrift 1,122,699. German Auslegeschrift 1,122,699 relates to a process for the preparation of polyurethane elastomers by crosslinking liquid isocyanate prepolymers by reaction in molds with mixtures of primary diamines and compounds containing several hydroxyl groups. In this latter process, a dispersion of a powder-form crystalline diamine in a liquid polyester or polyether containing several hydroxyl groups or in castor oil is introduced into the prepolymer at a temperature below the melting point of the diamine. The mixture is cured as a melt by known methods at temperatures above the melting point of the diamine used in the mixture. In this process, therefore, the actual "amine crosslinking" reaction takes place in a liquid, homogeneous phase. A particular disadvantage of the process disclosed in German Auslegeschrift 1,122,699 is the need for the high temperatures which must be applied in the processing of high-melting diamines such as 1,5-naphthylenediamine (m.p. 189° C.) or 4,4'-diaminodiphenyl ether (m.p. 186° C.).
U.S. Pat. No. 3,105,062 discloses a process for the preparation of polyurethane ureas in which relatively high molecular weight preadducts containing isocyanate groups are reacted with preferably aromatic diamines in heterogeneous phase. The resultant reaction mixtures cure at a temperature at which the "two-phase system" changes into a "one-phase system". This temperature is generally in the range from 100° to 170° C. The aromatic diamines disclosed in U.S. Pat. No. 3,105,062, however, are soluble, albeit to only a limited extent, in the reaction medium (the NCO preadduct). Consequently, uncontrollable preliminary reactions take place during the mixing of the two components, even at room temperature, and the reaction mixtures thicken in a very short time and form partly paste-like formulations. These paste-like formulations are difficult to process by the standard casting method and, accordingly, must be brought into the required form by applying pressure before they are actually cured by heating. According to U.S. Pat. No. 3,105,062, the stability of the thickened reaction mixtures in storage (pot life) is sufficient for further processing (that is, molding under pressure and coating), amounting to several hours. It is apparent from the Examples that the preferred reaction mixtures are those having a maximum pot life of about one hour. Accordingly, these mixtures cannot be regarded as long-term systems. In addition, U.S. Pat. No. 3,105,062 specifically points out that the use of the disclosed diamines--present only in solid form--in the one-shot process leads to unsatisfactory polyurethane moldings. The unwanted preliminary reaction of the diamine with the diisocyanate takes place to an increased extent, the poorly soluble polyurea precipitating in the reaction mixture and no longer reacting.
German Offenlegungsschrift 2,635,400 discloses another process for the preparation of polyurethane urea elastomers in which aromatic diamines are reacted as chain-extending agents in a single-stage or multi-stage process. This process is characterized by the use of aromatic diamines having a melting point above 130° C. that are present in the reaction mixtures in solid form. The heat curing of such mixtures takes place at a temperature in the range from 80° to 120° C., that is, below the melting point of the aromatic diamine. By virtue of the choice of the corresponding diamines as chain-extending agents, the NCO-containing preadduct (also referred to as an NCO prepolymer) is not involved in a premature preliminary reaction that results in thickening of the mixtures. Accordingly, systems of this type can be readily processed even by casting. Since the pot life of these reactive systems is considerably increased, many aromatic diamines, which were difficult to process by the previously known method, may be used in this process. It can be seen from the examples of German Offenlegungsschrift 2,635,400 that the pot life of the liquid reaction mixtures ranges from a few minutes to several hours, depending on the reactivity or solubility of the aromatic diamine. For standard processing conditions, for example, in the hand casting process, these reaction mixtures, particularly those having relatively long pot lives, can generally be processed without significant difficulties. In contrast, problems arise if, as a result of machine failures or other required stoppages, there is a relatively long interruption between the preparation of the reaction mixtures and the curing phase. Accordingly, the need for long processing times at low temperature and for short curing times at elevated temperature is increasingly more urgent in practice.
The final polyurethane plastics are generally intended to exhibit favorable mechanical properties and, in many cases, a level of thermal stability adapted to a particular application. According to the prior art, the thermal stability of polyurethane elastomers depends largely on the type of chain-extending agent used. For example, if glycolic chain-extending agents are used for the preparation of elastomers, the resultant polyurethane moldings have lower thermal stability than when using compounds containing amino groups. There are, of course, also distinct differences in thermal stability within the particular type of chain-extending agents (compounds containing OH or NH 2 groups).
Accordingly, the object of the present invention was to find a process for the preparation of polyurethane ureas in which the starting components of the particular reaction systems (high molecular weight polyols or NCO preadducts and low molecular weight chain-extending agents containing NH 2 groups and, optionally, other auxiliaries and additives) remain unreacted for several weeks at room temperature or, optimally, for at least 14 days at a temperature of about 50° C. Such reaction mixtures may thus be regarded as "one-component systems" that cure only under the effect of relatively high temperatures. In addition, it is desirable that the mixtures that are capable of being cast at the processing temperature should be curable in economically useful reaction times.
The present invention is also based on the concept of finding suitable chain-extending agents containing amino groups which have only minimal solubility in the starting component (for example, in the NCO preadduct) at low temperatures but which have high solubility at relatively high temperatures, so that the polyurethane urea assumes a high molecular weight structure during the curing phase.
Another object of the present invention was to find a process for the preparation of polyurethane urea elastomers in which high-quality elastomers of high thermal stability are obtained.
It has now surprisingly been found that solid, high-melting diamines corresponding to the formula ##STR2## in which the NH 2 groups are in the o-, m- or p-position to the ether oxygen and R 1 and R 2 represent hydrogen or alkyl groups (preferably methyl groups), give reaction mixtures that are stable in storage at room temperature when processed by the one-shot process or prepolymer process. Reaction systems such as these have a stability in storage of days to weeks at about 50° C.
For compounds in which R 1 and R 2 are hydrogen and each NH 2 group is para to the ether oxygen, one-component systems having indefinite stability in storage at room temperature or at elevated temperatures of up to about 50° C. are obtained. A precondition in this regard is that the combination should be protected against the effect of atmospheric moisture in order to avoid unwanted reaction of the NCO groups with water.
SUMMARY OF THE INVENTION
The present invention relates to a process for the preparation of polyurethane urea elastomers comprising reacting
(a) compounds containing at least two isocyanate-reactive groups and having a molecular weight in the range from about 400 to about 10,000 (preferably in the range from 400 to 6,000);
(b) polyisocyanates;
(c) aromatic diamines corresponding to the formula ##STR3## wherein R 1 and R 2 are independently hydrogen or alkyl (wherein the alkyl is preferably C 1 -C 6 alkyl or more preferably methyl); and
(d) optionally, auxiliaries and additives known in polyurethane chemistry.
In the representation for diamines (c), each NH 2 group can be in the o-, m- or p-position (preferably in the p-position) relative to the ether oxygen atoms attached to the same benzene ring. The R 2 groups, of course, can be attached at any of the remaining positions on the benzene ring.
These systems may then be cured at any time by application of heat (preferably 140° to 200° C.). Polyurethane elastomers having very good mechanical properties and high thermal stability are obtained.
DETAILED DESCRIPTION OF THE INVENTION
If instead of being used according to the process of the invention, the chain-extending agents of the invention are added to the polyisocyanates or NCO preadducts in dissolved form, they behave in the same way as typical aromatic diamines. That is, the reaction mixture crosslinks after a few seconds and the resultant gel-like product can no longer be processed. Thus, the inherent chemical reactivity of the chain-extending agent (which is present in heterogeneous phase when used according to the invention) towards NCO groups of the polyisocyanates or of the relatively high molecular weight preadducts is of only minor importance to the long pot life of the reaction mixtures according to the invention. Rather, the crosslinking rate depends to a large extent on the tendency of the diamines to dissolve in the reaction mixture. Accordingly, the stability of the reaction mixtures in storage also depends to a large extent on the nature of the starting products, for example, the polyols on which the NCO preadduct is based. By using suitable polyols, it is possible to influence desirably the crosslinking time or crosslinking temperature of the mixtures.
If, for example, commercially available polypropylene glycol ethers (that is, polyethers of propylene oxide and water) are used for the preparation of the NCO preadducts, one-component systems stable in storage at room temperature are obtained in admixture with suitable diamines. However, such mixtures cure at the predetermined temperatures only after prolonged application of heat. Uncontrollable secondary reactions involving the NCO preadduct (for example, trimerization or allophanatization) can take place in the meantime, thereby producing unsatisfactory elastomers. However, this long curing time can be shortened by using, for example, polypropylene glycol ethers additionally containing ethylene oxide units as starting components. The character of the one-component system is not affected. On the other hand, the use of pure polypropylene glycol ethers is advisable when the component containing NH 2 groups shows slightly better solubility than described above.
The same observations also apply when polyesters (for example, polyadipate) are used for the preparation of the NCO preadduct. For polyesters, the processing characteristics of the mixtures can be considerably influenced by the choice of the low molecular weight glycols (that is, the esterification components).
Under no circumstances, however, should the reaction mixtures be allowed to thicken prematurely through premature polyaddition during mixing of the two reaction components (NCO preadduct and aromatic diamine) at room temperature or slightly elevated temperature.
On an industrial scale, the simplest representative of this class of compounds may readily be synthesized by the following method. The hydroquinone bis(hydroxyethyl) ether (1), which can be obtained by the reaction of two moles of ethylene oxide and one mole of p-hydroquinone, reacts with sodium hydroxide and two moles of p-nitrochlorobenzene in a suitable solvent according to methods known to those skilled in the art, such as that described in DE 3,722,499 (believed to correspond to U.S. Pat. No. 4,870,499, which is incorporated by reference). After isolation, the resultant nitro derivative (2) is hydrogenated to give the diamine end product (3) (m.p. 215° C.). ##STR4##
The diamines, which are obtained in solid form, are generally finely ground (for example, in a ball mill) until they have an average particle size of about 1 to about 100 μm (preferably 1 to 50 μm) (μm=micrometers).
Preferred starting materials for the preparation of the chain-extending agents containing NH 2 groups include 2-nitrochlorobenzene, 2-nitrofluorobenzene, 4-nitrochlorobenzene, 4-nitrofluorobenzene, 1-methyl-2-nitro-3-chlorobenzene, 1-methyl-2-nitro-3-fluorobenzene, 1-methyl-4-nitro-5-chlorobenzene, 1-methyl-4-nitro-5-fluorobenzene, 1-methyl-2-nitro-6-chlorobenzene, and 1-methyl-2-nitro-6-fluorobenzene. 4-Nitrochlorobenzene and 2-nitrochlorobenzene are particularly preferred.
Mixtures of the above-mentioned diamines with other known polyurethane chain-extending agents containing at least two isocyanate-reactive hydrogen atoms and having a molecular weight of 60 to 400 may, of course, also be used.
The solid diamine compounds described above may also be used in retarded form (for example, in accordance with German Offenlegungsschrift 3,429,149, believed to correspond to U.S. Pat. No. 4,663,415) to prepare heat-stable polyurethane ureas by the process of the invention. Thus, before they are used as chain-extending agents, the diamine compounds may be treated with small quantities of a suitable polyisocyanate, for example, in an inert solvent or preferably in suspension in a high molecular weight polyol. A thin polyurea shell is thus formed on the particle surface of the diamines, where it acts as an anti-diffusion layer. This anti-diffusion layer is destroyed by warming to a certain temperature and curing of the mixture is initiated. Reactive systems having a distinctly longer pot life than systems in which the chain-extending agent is not provided with an anti-diffusion layer are obtained with the diamine compounds thus modified (i.e., retarded) either in powder form or suspended in polyol, in combination with NCO preadducts.
Preferred isocyanate-reactive compounds (a) for the preparation of the NCO-containing preadducts are polyhydroxyl compounds having a molecular weight in the range from about 400 to about 10,000 (preferably from 600 to 6,000). Suitable polyhydroxyl compounds of this type include polyesters, polyethers, polythioethers, polyacetals, polycarbonates, and polyesteramides containing at least two (preferably two to four) hydroxyl groups of the types known for use in the preparation of homogeneous and cellular polyurethanes.
Suitable polyesters containing hydroxyl groups include reaction products of polyhydric (preferably dihydric and, optionally, trihydric) alcohols with polybasic (preferably dibasic) carboxylic acids. Instead of using polycarboxylic acids in the free acid form, it is also possible to use corresponding polycarboxylic anhydrides or corresponding polycarboxylic acid esters of lower alcohols or mixtures thereof for producing the polyesters. The polycarboxylic acids may be aliphatic, cycloaliphatic, aromatic and/or heterocyclic and may optionally be substituted (for example by halogen atoms) and/or unsaturated. Examples of suitable carboxylic acids and their derivatives are succinic acid, adipic acid, suberic acid, azelaic acid, sebacic acid, phthalic acid, isophthalic acid, trimellitic acid, phthalic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, tetrachlorophthalic anhydride, endomethylene tetrahydrophthalic anhydride, glutaric anhydride, maleic acid, maleic anhydride, fumaric acid, dimeric and trimeric fatty acids (such as oleic acid), optionally in admixture with monomeric fatty acids, terephthalic acid dimethyl ester, and terephthalic acid bis-glycol ester. Suitable polyhydric alcohols include ethylene glycol, 1,2- and 1,3-propylene glycol, 1,4- and 2,3-butylene glycol, 1,6-hexanediol, 1,8-octanediol, neopentyl glycol, cyclohexane dimethanol (i.e., 1,4-bis(hydroxymethyl)cyclohexane), 2-methyl-1,3-propanediol, glycerol, trimethylolpropane, 1,2,6-hexanetriol, 1,2,4-butanetriol, trimethylolethane, pentaerythritol, quinitol, mannitol and sorbitol, methyl glycoside, diethylene glycol, triethylene glycol, tetraethylene glycol, polyethylene glycol, dipropylene glycol, polypropylene glycols, dibutylene glycol, and polybutylene glycols. The polyesters may contain terminal carboxyl groups. Polyesters of lactones, such as ε-caprolactone, or of hydroxycarboxylic acids, such as ω-hydroxycaproic acid, may also be used. These polyester diols are preferred.
Suitable polyethers containing at least 2 (generally 2 to 8 and preferably 2 to 3) hydroxyl groups are known and can be prepared, for example, by the polymerization of epoxides, optionally, in the presence of a catalyst such as BF 3 , or by the chemical addition of these epoxides, optionally as mixtures or successively, to starter components containing reactive hydrogen atoms. Suitable epoxides include ethylene oxide, propylene oxide, butylene oxide, tetrahydrofuran, styrene oxide, or epichlorohydrin. Suitable starter components include water, alcohols, or amines, including, for example, ethylene glycol, 1,3-propylene glycol or 1,2-propylene glycol, trimethylolpropane, 4,4'-dihydroxydiphenylpropane, aniline, ammonia, ethanolamine, or ethylenediamine. Sucrose polyethers of the type described, for example, in German Auslegeschriften 1,176,358 and 1,064,938 may also be used according to the invention. Polyethers that contain predominantly primary hydroxyl groups (up to about 90% by weight, based on all of the hydroxyl groups in the polyether) are also often preferred. Polyethers modified by vinyl polymers of the kind obtained, for example, by the polymerization of styrene and acrylonitrile in the presence of polyethers (e.g., U.S. Pat. Nos. 3,383,351, 3,304,273, 3,523,093, and 3,110,695 and German Patentschrift 1,152,536) are also suitable, as are polybutadienes containing hydroxyl groups.
Suitable polythioethers include the condensation products obtained by the reaction of thiodiglycol, either alone or with other glycols, dicarboxylic acids, formaldehyde, aminocarboxylic acids, or amino alcohols. The products obtained are polythio-mixed ethers, polythioether esters, or polythioether ester amides, depending on the components used.
Suitable polyacetals include compounds obtained from the condensation of glycols, such as diethylene glycol, triethylene glycol, 4,4'-dihydroxydiphenylmethane, and hexanediol, with formaldehyde. Suitable polyacetals can also be obtained by the polymerization of cyclic acetals.
Suitable polycarbonates containing hydroxyl groups are known and can be prepared, for example, by the reaction of diols, such as 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, triethylene glycol, or tetraethylene glycol, with diarylcarbonates such as diphenylcarbonate or with phosgene.
Suitable polyesteramides and polyamides include the predominantly linear condensates obtained, for example, from polybasic saturated and unsaturated carboxylic acids or their anhydrides and polyhydric saturated and unsaturated amino alcohols, diamines, polyamines, and mixtures thereof.
Polyhydroxyl compounds already containing urethane or urea groups and optionally modified natural polyols, such as castor oil or carbohydrates (such as starch), may also be used. Addition products of alkylene oxides with phenol-formaldehyde resins or even with urea-formaldehyde resins may also be used in the process of the invention.
Representatives of the above-mentioned compounds suitable for use in accordance with the invention are described for example, in High Polymers, Vol. XVI; Polyurethanes, Chemistry and Technology by Saunders and Frisch, Interscience Publishers, New York, London, Volume I, 1962, pages 32-42 and 44-54 and Volume II, 1964, pages 5-6 and 198-199; and Kunststoff-Handbuch, Volume VII, edited by Vieweg and Hochtlen, Carl-Hanser-Verlag, Munich, 1966, pages 45-71.
It is, of course, possible to use mixtures of such compounds containing at least two isocyanate-reactive hydrogen atoms and having a molecular weight of from 400 to 10,000, for example, mixtures of polyethers and polyesters.
Suitable compounds for use as starting component (b) are aliphatic, cycloaliphatic, araliphatic, aromatic, and heterocyclic polyisocyanates of the type described, for example, by W. Siefken in Justus Liebigs Annalen der Chemie, 562, pages 75 to 136. Examples of suitable such polyisocyanates include ethylene diisocyanate, 1,4-tetramethylene diisocyanate, 1,6-hexamethylene diisocyanate, 1,12-dodecane diisocyanate, cyclobutane-1,3-diisocyanate, cyclohexane-1,3-and -1,4-diisocyanate and mixtures of these isomers, 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethylcyclohexane (German Auslegeschrift 1,202,785), 2,4- and 2,6-hexahydrotolylene diisocyanate and mixtures of these isomers, hexahydro-1,3-and/or -1,4-phenylene diisocyanate, perhydro-2,4'- and/or -4,4'-diphenylmethane diisocyanate, 1,3- and 1,4-phenylene diisocyanate, 2,4- and 2,6-tolylene diisocyanate and mixtures of these isomers, diphenylmethane-2,4'- and/or -4,4'-diisocyanate, naphthylene-1,5-diisocyanate, triphenylmethane-4,4',4"-triisocyanate, polyphenyl polymethylene polyisocyanates of the type obtained by condensing aniline with formaldehyde, followed by phosgenation and described, for example, in British Patents 874,430 and 848,671, perchlorinated aryl polyisocyanates of the type described, for example, in German Auslegeschrift 1,157,601, polyisocyanates containing carbodiimide groups of the type described in German Patentschrift 1,092,007, norbornane diisocyanates such as described in U.S. Pat. No. 3,492,330, polyisocyanates containing allophanate groups of the type described, for example, in British Patent 994,890, Belgian Patent 761 626, and published Dutch Patent Application 7,102,524, polyisocyanates containing isocyanate groups of the type described, for example, in German Patentschriften 1,022,789, 1,222,067, and 1,027,394 and German Offenlegungsschriften 1,929,034 and 2,004,048, polyisocyanates containing urethane groups of the type described, for example, in Belgian Patent 752,261 or U.S. Pat. No. 3,394,164, polyisocyanates containing acylated urea groups according to German Patentschrift 1,230,778, polyisocyanates containing biuret groups of the type described, for example, in German Patentschrift 1,101,394, British Patent 889,050, and French Patent 7,017,514, polyisocyanates produced by telomerization reactions of the type described, for example, in Belgian Patent 723,640, polyisocyanates containing ester groups of the type described, for example, in British Patents 965,474 and 1,072,956, U.S. Pat. No. 3,567,763 and German Patentschrift 1,231,688, and also reaction products of the above-mentioned diisocyanates with acetals according to German Patentschrift 1,072,385. It is also possible to use the isocyanate-group containing distillation residues obtained in the commercial production of isocyanates, optionally in solution in one or more of the above-mentioned polyisocyanates. It is also possible to use mixtures of the above-mentioned polyisocyanates.
In general, it is particularly preferred to use the commercially readily available polyisocyanates, such as 2,4- and 2,6-tolylene diisocyanate, and mixtures of these isomers ("TDI"); polyphenyl polymethylene polyisocyanates of the type obtained by condensing aniline with formaldehyde, followed by phosgenation ("crude MDI"); and polyisocyanates containing carbodiimide groups, urethane groups, allophanate groups, isocyanurate groups, urea groups, or biuret groups ("modified polyisocyanates").
The polyisocyanates or the isocyanate prepolymers prepared from the polyisocyanates mentioned above and the relatively high molecular weight and/or low molecular weight polyols mentioned above should be present in liquid form during the reaction with the powdered or suspended aromatic diamine.
If polyurethane foams are to be prepared by the process of the invention, water and/or readily volatile organic substances are used as blowing agents. Organic blowing agents include acetone, ethyl acetate, methanol, ethanol, halogen-substituted alkanes (such as methylene chloride, chloroform, ethylidene chloride, vinylidene chloride, monofluorotrichloromethane, chlorodifluoromethane, and dichlorodifluoromethane), butane, hexane, heptane, or diethyl ether. A blowing effect may also be obtained by adding compounds which decompose at temperatures above room temperature and thereby give off gases such as nitrogen, for example, azo compounds such as azoisobutyronitrile. Other examples of blowing agents and information on their use can be found in Kunststoff-Handbuch, Volume VII, edited by Vieweg and Hochtlen, Carl-Hanser-Verlag, Munich, 1966, for example, on pages 108-109, 453-455, and 507-510.
Catalysts may often also be used in the process of the invention. Suitable catalysts are known and include tertiary amines, such as triethylamine, tributylamine, N-methylmorpholine, N-ethylmorpholine, N,N,N',N'-tetramethyl ethylenediamine, 1,4-diazabicyclo[2.2.2]octane, N-methyl-N'-(dimethylaminoethyl)piperazine, N,N-dimethylbenzylamine, bis(N,N-diethylaminoethyl) adipate, N,N-diethyl benzylamine, pentamethyl diethylenetriamine, N,N-dimethylcyclohexylamine, N,N,N',N'-tetramethyl-1,3-butanediamine, N,N-dimethyl-β-phenylethylamine, 1,2-dimethylimidazole, and 2-methylimidazole.
Suitable tertiary amine catalysts containing isocyanate-reactive hydrogen atoms include triethanolamine, triisopropanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, N,N-dimethylethanolamine, and reaction products thereof with alkylene oxides, such as propylene oxide and/or ethylene oxide.
Other suitable catalysts are sila-amines containing carbon-silicon bonds, of the type described, for example, in German Patentschrift 1,229,290. Suitable such compounds include 2,2,4-trimethyl-2-silamorpholine and 1,3-diethylaminomethyl tetramethyldisiloxane.
Other suitable catalysts include nitrogen-containing bases, such as tetraalkylammonium hydroxides; alkali hydroxides, such as sodium hydroxide; alkali phenolates, such as sodium phenolate; or alkali alcoholates, such as sodium methylate. Hexahydrotriazines may also be used as catalysts.
It is also possible to use organometallic compounds, particularly organotin compounds, as catalysts according to the invention. Preferred organotin compounds are tin(II) salts of carboxylic acids, such as tin(II) acetate, tin(II) octoate, tin(II) ethylhexoate, and tin(II) laurate, and the dialkyltin salts of carboxylic acids, such as dibutyltin diacetate, dibutyltin dilaurate, dibutyltin maleate, or dioctyltin diacetate.
Further representatives of suitable catalysts and information on the way in which they work can be found in Kunststoff-Handbuch, Volume VII, edited by Vieweg and Hochtlen, Carl-Hanser-Verlag, Munich, 1966, for example, on pages 96-102.
The catalysts are generally used in a quantity of from about 0.001 to about 10% by weight, based on the total quantity of polyhydroxyl compounds (a) having a molecular weight of 400 to 10,000.
Surface-active additives (emulsifiers and foam stabilizers) may also be used in the process of the invention. Suitable emulsifiers include the sodium salts of castor oil sulfonates or even of fatty acids or salts of fatty acids with amines, such as diethylamine oleate or diethanolamine stearate. Alkali or ammonium salts of sulfonic acids, such as dodecylbenzenesulfonic acid or dinaphthylmethanedisulfonic acid, or of fatty acids, such as ricinoleic acid, or of polymeric fatty acids may also be used as surface-active additives. Suitable foam stabilizers are preferably polyether siloxanes. The structure of these compounds is generally such that a copolymer of ethylene oxide and propylene oxide is attached to a polydimethylsiloxane residue. Foam stabilizers such as these are described, for example, in U.S. Pat. No. 2,764,565.
It is also possible to use reaction retarders, for example, acidic substances such as hydrochloric acid or organic acid halides; known cell regulators, such as paraffins or fatty alcohols or dimethylpolysiloxanes; pigments or dyes; known flameproofing agents, such as tris(chloroethyl) phosphate or ammonium phosphate and polyphosphate; stabilizers against the effects of aging and weather; plasticizers; fungistatic and bacteriostatic substances; and fillers, such as barium sulfate, kieselguhr, carbon black, or whiting.
Further examples of surface-active additives and foam stabilizers, cell regulators, reaction retarders, stabilizers, flameproofing agents, plasticizers, dyes, fillers, and fungistatic and bacteriostatic substances that can optionally be used in accordance with the invention and information on the way in which these additives are used and their respective modes of action can be found in Kunststoff-Handbuch, Volume VI, edited by Vieweg and Hochtlen, Carl-Hanser-Verlag, Munich, 1966, for example, on pages 103-113.
In the process of the invention, the reaction components are reacted by the known one-shot process, the prepolymer process, or the semiprepolymer process, often using machines such as the type described in U.S. Pat. No. 2,764,565. Information on processing machines that can also be used in accordance with the invention can be found in Kunststoff-Handbuch, Volume VI, edited by Vieweg and Hochtlen, Carl-Hanser-Verlag, Munich, 1966, for example, on pages 121-205.
In the process of the invention, the quantities in which the reaction components are used are generally selected so that the molar ratio of the amount of polyisocyanates to the combined amount of the chain-extending agent and the compound containing reactive OH groups is generally between about 0.7 and about 1.5 (preferably between 0.90 and 1.15), depending on the particular method used for processing. When a prepolymer stage is involved, the percentage NCO content of the prepolymer may be from about 1.8 to about 6% by weight. The molar ratio of reactive hydrogen of the chain-extending agent to reactive OH groups may vary within wide limits and should preferably be between 0.4 and 1.5 when flexible to rigid polyurethanes are to be obtained. In addition to the diamines used in accordance with the invention, other diamines or even diols (for example, those of the type mentioned above in connection with the preparation of the polyhydroxyl compounds) may also be used as a part of the chain-extending agents. However, the molar fraction of the amine of the invention in the chain-extending agent should be between about 1 and about 0.5 (preferably between 1 and 0.8).
The process according to the invention may even be carried out in two stages. The polyol component containing at least two hydroxyl groups and having a molecular weight of 400 to 10,000 can be reacted in known manner with an excess of diisocyanate to form a preadduct containing NCO groups. The course of the reaction may be monitored by NCO titration. After the polyaddition is completed, the diamine is introduced in the form of a solid powder (particle size of about 5 to about 50 μm) using a suitable stirrer and the resultant suspension is thoroughly mixed. The solid diamine powder may, however, also first be mixed in a small quantity of the high molecular weight liquid polyol on which the NCO preadduct is based. The preferred ratio by weight of diamine to polyol is from about 1:0.5 to about 5.0:1 (preferably from 1:1 to 2:1). Preferred polyhydroxyl compounds are those in which the aromatic diamine is insoluble or only poorly soluble at relatively low temperatures (e.g, below about 100° C.) but in which the aromatic diamine becomes substantially soluble upon warming to the curing temperature (e.g., about 130° to about 200° C.). The resulting paste or pourable suspension may then be added to the NCO preadduct to form a heterogeneous mixture that can subsequently be cured. An advantage of this process is the ease at which it can be carried out.
The reaction components may also be reacted by the one-shot process. In this process, the starting components (that is, a high molecular weight polyol, the polyisocyanate, the solid diamine and, optionally, the auxiliaries and additives) may be reacted after mixing by bringing the mixture to the necessary curing temperature (i.e., about 140° to about 200° C.). Curing, however, may even take place in steps, in the first of which the reaction of the polyisocyanate with the polyol is carried out at a relatively low temperature (i.e., about 60° to about 100° C.) that is below the melting temperature of the solid diamine and at which temperature the solid diamine is only poorly soluble and does not react. A material that is moldable under pressure is initially obtained. Final curing may then take place at any time, the final physical values being reached at about 150° to about 180° C. (see Examples).
The temperature at which the chain-extending agent is added depends on the physical state of the NCO preadduct. With liquid NCO preadducts, the chain-extending agent is added, either in bulk or preferably in a polyol suspension, at room temperature. With highly active or solid NCO prepolymers, the chain-extending agent is added at a temperature at which satisfactory casting of the mixtures is guaranteed, generally in the range from about 60° to about 80° C. Under no circumstances should a premature reaction involving the NCO prepolymer and the aromatic diamine be allowed to take place, because any uncontrollable increase in the viscosity of the mixture would complicate further processing by the standard casting method. This restriction should, however, be distinguished from preliminary reactions of a stepwise preparation in which small portions of an aromatic diaminepolyol suspension can be mixed with the starting polyisocyanate in quantities such that only 0.05 to 20% NH 2 equivalents of the aromatic diamine react initially with the polyisocyanate.
The reaction mixture is degassed in vacuo shortly after addition of the diamine.
The processing of the reactive systems according to the invention depends on their physical state. Liquid systems that are pourable at room temperature can be processed by casting, optionally being briefly heated before processing, for example, to about 50° to about 70° C. Systems which are not pourable, but which still can flow, may be applied to desired substrates, for example, by means of a coating knife, and subsequently cured by heat shock. Plastic systems (pastes) may be molded under heat and pressure. Solid systems, particularly those based on relatively high-melting starting polyols (i.e., melting at about 45° to about 65° C.), are processed either under pressure in molds (injection molding) or at or above the melting temperature of the polyol. For example, the long-term stability systems prepared beforehand may be introduced in the form of solid granules into a mold heated above the melting point of the polyol (generally below about 70° C.). After the granules are melted and the mold is filled, the mold is heated to about 130° to about 200° C. and the contents cured. The curing temperature of the reactive systems of the invention is in the range from about 130° to about 200° C.
Elastomers prepared according to the invention may be used for a variety of purposes, for example, for moldings subjected to severe mechanical stressing, such as tires, rollers, V-belts, or seals that are exposed to severe thermal or chemical stressing, for hot water pipes or motors, or for the production of films, textile coatings, and polyurethane powders.
The chain-extending reaction may even be carried out in the presence of the blowing agents and additives described above, preferably in closed molds, thereby forming foams having a cellular core and a compact skin.
The elastic and semi-elastic foams that can be obtained by the process of to the invention are used, for example, as upholstery materials, mattresses, and packaging materials. By virtue of their flame resistance, the elastic and semi-elastic foams can also be used for applications in which these properties are particularly important, for example, in vehicle and aircraft construction and in transport in general. The foams may either be produced by foam molding or may be made up from slabstock foam.
The following examples further illustrate details for the process of this invention. The invention, which is set forth in the foregoing disclosure, is not to be limited either in spirit or scope by these examples. Those skilled in the art will readily understand that known variations of the conditions of the following procedures can be used. Unless otherwise noted, all temperatures are degrees Celsius and all parts and percentages are parts by weight and percentages by weight, respectively.
EXAMPLES
EXAMPLE 1 (Prepolymer process)
General procedure
The NCO-terminated preadducts were prepared by known methods from 1 mole of polyol and 2 moles of 2,4-diisocyanatotoluene ("TDI") at 60°-80° C. The course of each polyaddition reaction was followed by simple NCO titration. For one preadduct (the product prepared from polyol (b)), residual monomeric TDI that was still present in small quantities was removed using a thin-layer evaporator.
To produce the elastomers, the appropriate NCO preadduct (200 g) was thoroughly degassed with stirring at 50°-60° C. under aspirator vacuum. The diamine was then added to the NCO preadduct as a fine powder (particle size 5-50 μm). The molar ratio of NCO to OH was 1.1:1. The resultant NCO preadduct-diamine suspension could be satisfactorily processed at the temperature designated in the Table below and was thoroughly homogenized with further degassing. The reactive systems ultimately obtained were stable in storage for a few months in the absence of atmospheric moisture, both at room temperature and at elevated temperature, and showed no significant increase in viscosity during storage.
Curing took place at a temperature of 150° to 180° C. The mixtures were poured into a mold coated with release agent and were kept at 170° to 180° C. for 2 to 4 hours. Each test specimen was then removed from the hot mold. After storage for several days at room temperature, the moldings had the properties shown in the Table below.
In the Examples, a diamine corresponding to the formula ##STR5## (1,4-bis(2-(4-aminophenoxy)ethoxy)benzene) was used as the chain-extending agent containing NH 2 groups. This material was prepared, as discussed above, by the method of U.S. Pat. No. 4,870,206, for example by reaction of 1,4-bis-(2-hydroxyethoxy)-benzene with o- or p-chloronitrobenzene in the presence of alkaline and polar-aprotic solvent, and in a second step followed hydrogenation of the nitro groups to the amino groups.
The following polyols were used for the preparation of the NCO preadducts (using 2,4-diisocyanatotoluene as the polyisocyanate component):
(a) Polyester of adipic acid and ethylene glycol (molecular weight 2,000, OH value 56) Isocyanate content of NCO preadduct of 3.85%
(b) Polyester of adipic acid and a mixture of ethylene glycol and 1,4-butanediol (molar ratio 1:1) (molecular weight 2,000, OH value 56) Isocyanate content of NCO preadduct of 3.3% (after removal of TDI using a thin-layer evaporator)
(c) Polyester (hexanediol polyether ester carbonate) of diphenyl carbonate and a polycondensate of 1,6-hexanediol (molecular weight 2,000, OH value 56) (see German Offenlegungsschrift 3,717,060, believed to correspond to U.S. Pat. No. 4,808,691) Isocyanate content of NCO preadduct of 3.5%
(d) Polycaprolactone (molecular weight 2,000, OH value 56) Isocyanate content of NCO preadduct of 3.6% NCO
(e) Polytetrahydrofuran-etherdiol (molecular weight 2,000, OH value 56) Isocyanate content of NCO preadduct of 3.5%
(f) Polypropylene glycol ether (molecular weight 2,000, OH value 56)
The mechanical properties of the elastomers prepared batchwise using 200 g of each preadduct are shown in the following Table.
TABLE______________________________________MECHANICAL PROPERTIES OF ELASTOMERS Starting Polyols (a) (b) (c) (d) (e) (f)______________________________________Preadduct 3.85 3.3 3.5 3.6 3.5 3.5NCO content(%)Quantity of 31.6 27.0 28.7 29.5 28.7 28.7diamine (g)Modulus 7.4 7.0 5.5 6.2 4.5 2.5100% (MPa)Modulus 16.1 12.5 9.8 11.1 8.5 4.0300% (MPa)Tensile 40.7 45.8 21.8 24.4 15.8 8.5strength(MPa)Elongation at 550 480 400 400 380 480break (%)Tear 85.8 67.9 42.8 45.5 28.2 26.7propagationresistance(KN/m)Elasticity (%) 40 45 50 52 58 38Shore A 92 90 87 91 84 72Hardness______________________________________
EXAMPLE 2 (One-shot process)
A linear polyester based on adipic acid and ethylene glycol (molecular weight 2,000, OH value 56) (200 g, 0.1 mole) was melted at 50° to 60° C. First 1,4-butanediol (4.5 g, 0.05 mole) and then 1,4-bis(2-(4-aminophenoxy)ethoxy)benzene (19.0 g) were added in solid form with stirring to the polyester. A total of 0.3 mole of OH groups and 0.1 mole of NH 2 groups is available for polyaddition with the isocyanate. To crosslink the OH component (i.e., the polyester and 1,4-butanediol), molten 4,4'-diisocyanatodiphenylmethane ("MDI") (37.5 g, 0.15 mole) was stirred in, and, for the NH 2 component (i.e., the diamine), 1,5-diisocyanatonaphthalene ("NDI") (10.5 g, 0.05 mole) was stirred in as a powder. The melt suspension flowed freely at 50° to 60° C. and, accordingly, could be poured into a mold provided with glass fiber mats. A crosslinked, but thermoplastic material, in which the glass fiber mats were embedded, was obtained after a few hours at approximately 60° C. The reaction of the OH components with the MDI was largely over but the aromatic diamine was still unreacted. This pre-product ("prepreg") was stable in storage in the absence of atmospheric moisture both at room temperature and at elevated temperature but could be cured at any time. The prepreg was cured by molding under pressure at a crosslinking temperature of 150° to 180° C., yielding a glass-fiber-reinforced, tough end product having a Shore A hardness of 92 to 94 and particularly high thermal stability.
EXAMPLE 3 (Semiprepolymer process)
A semiprepolymer containing NCO groups (NCO content 4.9%, theoretical 5.0%) was obtained by a reaction of 800 g of a linear polyether polyol (prepared by addition of propylene oxide with water and having a molecular weight of 2,000 and an OH value of 56) with 258 g of 4,4'-diisocyanatodiphenylmethane at 80° C. using the usual method.
A 105 g portion of this semiprepolymer was thoroughly mixed at room temperature with 20 g of the solid diamine described in Example 1. The suspension, which is stable in storage at room temperature, was degassed under aspirator vacuum. The liquid reactive system was poured into a mold coated with release agent and then heated to 180° C. After 2 hours, the mixture cured and the molding could be removed from the mold.
An elastic polyurethane urea elastomer having a good surface and a Shore A hardness of 90 was obtained. | This invention relates to a process for preparing polyurethane urea elastomers by reacting (a) compounds containing at least two isocyanate-reactive groups and having a molecular weight in the range from about 400 to about 10,000; (b) polyisocyanates; and (c) aromatic diamines corresponding to the formula ##STR1## wherein R 1 and R 2 are independently hydrogen or alkyl. | 2 |
FIELD OF THE INVENTION
The present invention relates to the bottling of liquids and more particularly to a machine suitable for filling bottles of different dimensions.
BACKGROUND OF THE INVENTION
In the technology normally used, machines are known for filling bottles, for example machines sold by the company BREITNER. This type of machine is very complex and comprises numerous parts which have to be removed in order to be replaced by other parts when the format of the bottles is changed.
The object of the present invention is to provide a machine for filling bottles which can easily be adapted to a change in the type of bottle.
SUMMARY OF THE INVENTION
The metering machine according to the invention, in order to fill simultaneously a series of identical bottles moved by a continuously operating conveyor and in which a first series of bottles is brought to a first position in which they are immobilised and filled with a neutral atmosphere by means of a first series of nozzles entering the bottles and then moved to a second position in which they are immobilised and filled with a liquid by means of a second series of nozzles entering the bottles; the two series of nozzles being fixed to each other and being driven vertically in order to cause the nozzles to enter the bottles and to withdraw them therefrom and the bottles being in contact with each other when they are on the conveyor in their first and second positions, and guides adjustable in transverse position with respect to the movement of the bottles so as to align the various types of bottle moved by the conveyor underneath the nozzles, a metering machine characterised in that it comprises two practically identical alignment devices disposed one above the other and provided with a guide defining a passage slot allowing the movement of the nozzles in only one dimension parallel to the movement of the bottles in order to be able to adjust the distance between each nozzle and a series of combs each being able to be moved in a practically horizontal plane and perpendicularly to the direction of movement of the bottles in order to immobilise the nozzles in a position suited to the bottles to be filled; a means of stopping the bottles comprising a first device for immobilising the bottles, the position of which with respect to the nozzle situated furthest downstream is equal to half the diameter of the bottles disposed on the conveyor and which is intended to prevent the movement of the two series of bottles,
a first cell disposed upstream of the first immobilisation device, the position of which can be adjusted along the path according to the type of bottle moved by the conveyor and intended to check that the two series are complete so as to enable the metering cycle,
a second immobilisation device disposed upstream of the first immobilisation device and the position of which can be adjusted along the path according to the type of bottle moved by the conveyor and used to immobilise the first series of bottles when the two complete series of bottles are immobilised by the first immobilisation device and releasing the first series of bottles only when a given period of time, the start of which coincides with the release of the second series of bottles by the first immobilisation device, has elapsed in order to physically separate the first series of bottles from the second series of bottles, and
a second cell disposed downstream of the first immobilisation device, the position of which can be adjusted along the path according to the type of bottle moved by the conveyor and intended to indicate that the series of filled bottles has left the second position and to actuate the functioning of the first immobilisation device so as to keep the two series of bottles in an immobile position underneath the nozzles.
BRIEF DESCRIPTION OF THE DRAWINGS
A particular embodiment of a machine according to the invention will now be described with reference to the accompanying drawings in which:
FIG. 1 shows diagrammatically the various functions carried out by a metering machine;
FIG. 2 shows, in perspective and partially cut away, a part of the device for aligning the nozzles according to the invention;
FIGS. 3 and 4 show an embodiment of the mechanism for positioning and immobilising the bottles which can be used in the invention.
DETAILED DESCRIPTION OF THE INVENTION
As can be seen in the different figures, the metering machine 1 comprises a conveyor 2 intended to move bottles 3 which are placed thereon. Advantageously, the conveyor is designed so as to move continuously, the movement of the bottles being able to be interrupted by introducing a stop on the path. At this moment, the bottom of the bottle slides on the surface of the conveyor 2.
The metering machine comprises a metering assembly 4, provided with several nozzles 5 suitable for entering the bottles. The entry of the nozzles 5 into the bottles 4 is obtained by a vertical downward movement of the metering assembly 4, shown by the arrow A. The nozzles 5, when they are inside the bottles, serve to introduce the appropriate fluids into the bottles. After filling of the bottles the nozzles are moved to their uppermost position as shown diagrammatically by the arrow B.
In a particular embodiment, the liquid to be packaged in the bottles being sensitive to oxygen, it is necessary to fill the bottles with a neutral atmosphere, for example nitrogen, before filling the bottle with the liquid to be packaged. The metering machine is therefore divided into two parts. A first part 10 comprising a first series of nozzles connected to a reservoir 11 containing a neutral atmosphere, for example nitrogen. A second part 20 comprising a second series of nozzles connected to a reservoir 21 containing the liquid to be packaged. To simplify the operation of the metering machine, the two parts 10 and 20 are fixed to each other.
Advantageously, lateral guides, shown schematically in FIG. 1 by the reference numeral 30, are disposed above the conveyor. These guides enable the neck of the bottle to be directed in correct register with the nozzles.
According to the invention, it is desired to be able to use, on this type of machine, bottles which do not have the same diameter. It is therefore necessary to modify the position of the various nozzles, to adjust the transverse guides and to modify the operating cycle of the metering machine.
Reference will now be made to FIG. 2, which shows diagrammatically and in perspective a part of an alignment device 40 used in the metering assembly 4. The alignment device 40 comprises a mounting 41, such as, for example, two rods, fixed to the metering assembly 4. This mounting supports, on the one hand, the guide 42 defining a passage slot 43 and, on the other hand, two supports 44.
The passage slot 43 is adapted so as to receive the nozzles 5 and to limit the movement of these nozzles in a direction parallel to the path of movement of the bottles. Advantageously, one of the surfaces 49 of the slot in contact with the nozzles is flexible and deformable so as to exert sufficient force on the nozzles to maintain them in position when they are subjected to any other external force apart from gravity. This arrangement allows an easy positioning of the nozzles by an operator desiring to modify their respective positions.
Advantageously the flexible surface is obtained by means by a strip of rubber.
The supports 44 are provided with fingers 45 on which combs 46 are able to slide in a plane parallel to the conveyor, practically horizontal and in a direction practically perpendicular to the path of the bottles. The combs 46 have cut-outs 47 intended to receive the nozzles 45. Advantageously, each comb 46 is suited to a particular type of bottle. The cut-outs 47 in each comb are spaced apart by a distance equal to the distance between spouts for bottles disposed one against the other on the conveyor.
The embodiment of the alignment device 40 therefore allows an easy change in the relative positions of the nozzles with respect to each other. This positioning is obtained by withdrawing the combs last used, choosing new combs and positioning the nozzles by moving the latter in a direction parallel to the path followed by the bottles and then engaging the nozzles and corresponding combs so as to immobilise the nozzles.
Since the filling of the bottles comprises in reality two distinct filling phases, one with a neutral atmosphere and the other with the product to be packaged, it is necessary to provide a mechanism 50, shown in more detail and in plan view in FIG. 4, to position and immobilise the bottles. This mechanism must be simple, reliable and easy to adjust according to the diameter of the bottles. The mechanism 50 comprises a first immobilisation device such as a ram 51, preferably fixed, the position of which depends on the position of the nozzle which is furthest downstream, and a first cell 55 situated upstream. The cell 55, preferably of the infrared type, receives IR radiation reflected by the bottles. Obviously another type of cell may be used.
The ram 51, when it is in the projecting position, as shown in FIG. 4, is situated on the path of the bottles so as to immobilise them in spite of the continuous operation of the conveyor belt 2. The cell 55 is situated upstream, at a sufficient distance from the ram 51 to ensure that the metering station comprises a sufficient number of bottles. When the bottles are immobilised by the ram 51 and the cell 55 does not detect the presence of bottles, the metering machine is stopped. Advantageously, the number of bottles disposed between the ram 51 and cell 5 affords a self-sufficiency of the machine corresponding to two metering cycles.
Preferably, the cell 55 detects the presence of bottles at the spout. This is shown diagrammatically by the system of orthogonal axes C shown in FIG. 4. In this way it is possible to ensure that the type of bottle disposed on the conveyor corresponds to the desired bottles.
The mechanism 50 also comprises a second immobilisation device such as a ram 52, the position of which can be adjusted along the path (as shown diagrammatically by the double arrow D) according to the type of bottle moved by the conveyor. This second ram 52, disposed upstream of the first ram 51, enables one series of bottles to be separated physically from another series. The second ram 52 is disposed so as to immobilise the series of bottles disposed upstream and into which the neutral atmosphere has been introduced. This ram 52 is put in the extended position during the metering operation. It enables the bottles which are filled with the liquid to be packaged to be separated physically from the bottles which are filled, for example, with nitrogen. Once the metering is finished, the first ram 51 is withdrawn or retracted so as to release the series of bottles full of the liquid to be packaged, whilst the second ram 52 is in the extended position. This enables the conveyor 2 to physically separate the bottles full of liquid from the bottles full of nitrogen. After a given period, the second ram 52 is retracted (as shown in FIG. 4), thus releasing the other bottles. The conveyor 2 then moves all the bottles.
A second cell 56, disposed downstream of the first ram 51 at a distance approximating to the number of bottles filled with the liquid to be packaged, enables the passage of the said bottle to be detected. The position of this cell 56 must be adjusted by a movement shown diagrammatically by the double arrow E in FIG. 4, according to the type of bottle moved by the conveyor 2. This detection actuates the first ram 51, which is returned to an extended position so as to prevent the movement of the bottles to be filled. After immobilisation of the bottles, the metering operation can commence and the second ram can be disposed in the extended position in order to be able to separate the full bottles physically from the bottles to be filled. Because of the relatively low precision which is of the order of a mm, the relative positioning of the second ram 52 and second cell 56 is obtained by register adjustment with a visual index. However, the use of a finger entering a recess formed in a guide rail can be envisaged. The positioning of the first cell 55 serving to detect the neck of the bottles can be obtained by means of a template 58 with holes 57 produced in a thick plate. The cell is disposed inside a cylindrical part able to enter the holes in the template according to the type of bottle which it is intended to move by means of the conveyor 2. The use of a template with holes enables the position of the first cell 55 to be modified very easily.
The modified metering machine according to the invention allows the use of bottles with different diameters. It is therefore necessary to provide bottle guides 30 adjustable in position so that the necks of these bottles always follow the same path within the metering station. This unique path makes it possible not to have to modify the position of the nozzles in two directions at right angles to each other.
Advantageously, the guides consist of bars 31 able to be moved perpendicularly to the path of the bottles in a plane parallel to the plane of the conveyor. In a particularly advantageous embodiment the ends of each bar 31 are provided with a position adjustment system. The adjustment system can take the form shown diagrammatically in FIG. 3. A support 32 fixed to the frame of the dosing machine holds a sleeve 33 so that its axis is practically perpendicular to the path followed by the bottles and in a plane parallel to the plane of the conveyor. A rod 34 connected to the bar 31 is able to slide in the sleeve 33. Advantageously the bar 31 is pivoted at 38 on the rod 34. The rod 34 has a collar 35 against which a spring 36 comes to bear. The rod 34 is thus pushed so as to come into contact with a cam 37 rotatably mounted on the support 32. Advantageously, the cam 37 may be in the form of an eccentric disc. The cam 37 may have, at its top, reference marks as well as recesses in which a pin affording the locking of the cam in its desired position is able to fit. Obviously any other adjustment device may be used. The adaptation of the metering machine according to the invention when the bottles to be filled are being changed takes only a very short time, approximately 30 seconds.
If desired, position sensors can be disposed at the cells 55 and 56, ram 52, guide bars 31 and combs 46. The sensors can be connected to a control device, such as, for example, a microprocessor, so as to alert the operator and prevent the operation of the metering machine if the various components to be adjusted are not all disposed in their position corresponding to the same type of bottle. | A machine for the filling bottles, particularly bottles of varying dimensions.
The metering machine comprises two identical devices placed one on top of the other, with combs, allowing the rapid, simple and easy adjustment of the nozzles used for metering, and a device for controlling the cycle which is easy to adjust according to the size of the bottles moved by the conveyor. | 1 |
FIELD OF THE INVENTION
This invention relates generally to a rod guide, and more particularly to an improved rod guide having increased gripping power, suitable for both rotating and reciprocating rod applications.
BACKGROUND OF THE INVENTION
In the hydrocarbon recovery industry, pumps are used at the lower ends of wells to pump oil to the surface through production tubing positioned within a well casing. Power is transmitted to the pump from the surface using a rod string positioned within the production tubing. Rod strings include both “reciprocating” types, which are axially stroked, and “rotating” types, which rotate to power progressing cavity type pumps. The latter type is increasingly used, particularly in wells producing heavy, sand-laden oil or producing fluids with high water/oil ratios.
Both reciprocating and rotating rods benefit from the use of rod guides to protect the interior surface of the production tubing. In practice, sucker rods and production tubing do not hang perfectly concentrically within a well, in part because well bores are never perfectly straight. Direct contact between the rod and the production tubing during reciprocation or rotation, especially while immersed in a harsh fluid environment, would otherwise cause expensive damage to the tubing and the rod. Rod guides are therefore placed between the rod and the tubing as a low cost sacrificial wear member.
Some rod guides have a plurality of fins projecting radially toward the ID of the production tubing, to center the rod within the tubing. The space between fins then provides a flow path for drilling fluid or hydrocarbon production flowing through the tubing. U.S. Pat. No 6,152,223 to Abdo describes such a rod guide, incorporating a low-friction wear material and a fin construction affording generous flow through. Other rod guides have a generally cylindrical outer surface having an OD substantially less than the ID of the production tubing, such that there is ample space between the guide and the tubing as a flow path. The disadvantage of this type of guide is there is less erodible wear volume (“EWV”) in the guide, which leads to greater frequency of replacement and associated costs.
Many rod guides require at least some assembly to the rod prior to being transported to the field where they will be used. U.S. Pat. No. 5,941,312 to Vermeeren and U.S. Pat. No. 5,339,896 to Hart, et. al, each disclose examples of such “partially field-installable” rod guides. A spool is mechanically bonded to the rod in a shop or manufacturing facility. When in the field, an outer rod guide body may be later snapped over the spool affixed to the rod.
The Hart patent describes a rod guide having embodiments for use with both rotating and reciprocating rods. The embodiment of the outer guide body depends on whether it is to be used with a reciprocating or rotating rod. For example, for a rotating embodiment, the body and spool may rotate freely with respect to each other, which is generally preferred for all rotating type rod guides. As the rod rotates, the spool remains stationary with respect to the rod, while the outer body is free to rotate about the spool to remain nearly stationary with respect to a sidewall of the production tubing, minimizing wear between the body and the tubing, and between the spool and the rod. The majority of the wear instead occurs between the low cost sacrificial spool and guide body. For a reciprocating embodiment, the spool may include an elongate projection, and the outer guide body may include a slot for mating with the projection, such that the guide body does not rotate with respect to the spool.
To minimize manufacturing and assembly costs, some existing rod guides can be installed entirely in the field. U.S. Pat. No. 4,858,688 to Edwards, et al. and U.S. Pat. No. 5,494,104 to Sable each disclose examples of such “fully field-installable” rod guides. In each of these, a generally unitary body is provided with a bore for tightly positioning about a rod, and an access channel is provided from an outer surface of the body to the bore, allowing the guide to be forcibly “snapped-on” in the field. A problem inherent to each of these rod guides is that the single-piece body must be flexed when snapped onto the rod, weakening the gripping power of the guide. The Sable patent strives to minimize this drawback, by providing a non-circular bore to place more material at the area of highest flex. Although this potentially improves the gripping power of the guide, the presence of the access channel remains a source of structural weakness during the service life of the guide. A further shortcoming of these single-piece snap-on rod guides is that a single-piece body is generally best suited for reciprocating-type rods, and is non-ideal for use with rotating type rods.
U.S. Pat. No. 4,343,518 discloses another type of fully field-installable rod guide that does not require an access channel for installation. Instead, the rod guide comprises two half sections which are adapted to be lockingly clamped together. One half section has grooves and the other half section includes flanges having complementary tapered surfaces so that when the two half sections are moved together vertically the flanges are wedged in the grooves to clamp the two half sections together about the rod. The tapered surfaces are very narrow, however, and do not alone produce sufficient gripping power. The half sections may use inner ridges on semi-circular recesses for contacting the rod, to cause the recesses to deform into an elliptical shape to resist slippage. Another shortcoming of the rod guide is that it is described for use only with a reciprocating type rod, and is unsuitable for use with a rotating type rod.
A rod guide is desired that is fully field-installable, useful with both reciprocating and rotating rods, and having an improved mechanism for attaching the guide to the rod.
SUMMARY OF THE INVENTION
A field-installable rod guide is disclosed for a rod having an outer rod surface and movable within an oilfield tubular having an interior tubular surface for driving a downhole pump to pump liquids to the surface through the oilfield tubular.
In one embodiment the rod guide comprises a body including first and second interfitting body members. The first body member has an outer wear surface; a pair of circumferentially spaced outer tapered surfaces radially inward of the outer wear surface and tapering radially along an axial direction, the outer tapered surfaces extending circumferentially a combined at least 70 degrees toward one another from circumferentially outer locations no greater than 180 degrees apart to circumferentially inner locations; and an inner rod-engagement surface radially inward of the outer tapered surfaces, for gripping the outer rod surface. The second body member has an outer wear surface, an inner taper-engagement surface radially inward of the outer wear surface, for axially slidably engaging the outer tapered surfaces of the first body member, to urge the first and second body member radially inward toward one another and to deform at least a portion of the first body member radially inward toward a rod gripping position about the rod; and an inner rod-engagement surface radially inward of the inner taper-engagement surface for gripping the outer rod surface. A locking member may be included for axially locking the first and second body member with respect to one another.
The second body member may also have a pair of circumferentially spaced outer tapered surfaces radially inward of the outer wear surface and tapering radially along an axial direction, the outer tapered surfaces extending circumferentially a combined at least 70 degrees toward one another from circumferentially outer locations no greater than 180 degrees apart to circumferentially inner locations. Likewise, the first body member may have an inner taper-engagement surface radially inward of its outer wear surface, for axially slidably engaging the pair of outer tapered surfaces of the second body member, to both urge the first and second body member radially inward toward one another and deform at least a portion of the second body member radially inward toward a rod gripping position about the rod.
The tapered surface outer locations of the first body member may be circumferentially spaced less than 5 degrees from adjacent tapered surface outer locations of the second body when the body is in the rod gripping position. Each outer tapered surface may circumferentially extend at least about 35 degrees.
Radially projecting portions may be included along the inner rod-engagement surfaces for increasing friction between the body and the rod. These may comprise axially-spaced ribs or a knurled surface.
For use especially with rotating type rod guides, a sleeve may be included for positioning about the first and second body member while in the rod gripping position. The sleeve may include an inner wear surface for slidably contacting the outer wear surfaces of the first and second body members, and an outer wear surface for slidably contacting the interior tubular surface of the oilfield tubular. One or more stops on the body limit axial motion of the sleeve with respect to the body.
A plurality of fins may be included for centering the rod within the interior tubular surface of the oilfield tubular. The fins may be included directly on the body, especially for reciprocating rod guides, or on the sleeve, for rotating rod guides.
The foregoing is intended to summarize the invention, and not to limit nor fully define the invention. The aspects of the present invention will be more fully understood and better appreciated by reference to the following description and drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a preferred embodiment for a rotating type rod guide, with both body members slid together to form the body and an outer sleeve about the body.
FIG. 2 shows a perspective view of one of the body members of FIG. 1 .
FIG. 3 shows a perspective view of the body members of FIG. 1 partially slid together.
FIG. 4 shows a perspective view of both body members of FIG. 1 fully slid together to form a body.
FIG. 5 shows a perspective view of the sleeve of FIG. 1 .
FIG. 6 is a perspective view of a less preferred embodiment of a reciprocating type rod guide not having a sleeve.
FIG. 7 shows the rod guide including a pair of axially spaced seal grooves.
FIG. 8 shows the rod guide including a pair of axially spaced seal members received by a respective one of the axially spaced seal grooves.
FIG. 9 shows a sleeve embodiment including a locking bridge for limiting outward flexing of the sleeve.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows a preferred embodiment for a rotating type rod guide 10 , assembled with interfitting first and second body members 12 , 14 slid together to form a generally cylindrical body 13 , and an outer sleeve 16 positioned about the body 13 . The rod guide 10 in general protects the rod and an interior bore of an oilfield tubular while the rod is moved within the tubular to power a pump. The rod guide embodied in FIG. 1 is particularly useful as a rotating type rod guide, because the body 13 may rotate freely within the sleeve 16 discussed below.
FIG. 2 shows in greater detail the first body member 12 of FIG. 1 . The first body member 12 is preferably substantially identical to the second body member 14 , and for the purpose of discussion the first and second body members 12 , 14 may be assumed to include the same features, except where noted. The first body member 12 includes an outer wear surface 20 , at least one outer tapered surface 22 radially inward of the outer wear surface 20 , tapering radially along an axial direction, and an inner rod-engagement surface 24 radially inward of the outer tapered surface 22 , for gripping an outer surface of a rod (not shown). The second body member 14 includes the outer wear surface 20 , an inner taper engagement surface 26 radially inward of the outer wear surface 20 , for axially slidably engaging the at least one outer tapered surface 22 of the first body member 12 , and the inner rod-engagement surface 24 radially inward of the inner taper engagement surface 26 . Because the body members 12 , 14 of this preferred embodiment are substantially identical, each of them thus includes the outer wear surface 20 , the outer tapered surface 22 , the inner rod-engagement surface 24 , and the inner taper-engagement surface 26 .
FIG. 3 illustrates how the first and second body member 12 , 14 cooperate. The first body member 12 is shown partially slid together with the second body member 14 , between which a rod may be positioned (not shown). As the body members 12 , 14 are axially slid together, the inner taper engagement surface 26 on one body member 12 , 14 axially slidably engages the at least one outer tapered surface 22 of the other body member 12 , 14 . This engagement draws the body members 12 , 14 toward a strong, frictional engagement about the rod.
FIG. 4 shows a perspective view of body members 12 , 14 fully slid together to form the body 13 . The body 13 thus has the substantially continuous outer wear surface 20 comprising the outer wear surfaces 20 of the individual body members 12 , 14 . The body is locked together with optional locking members, which are shown as a radially projecting snap 15 on the first body member 12 (see FIG. 2 ) and a corresponding recess 17 on the second body member 14 (see FIG. 3 ) for receiving the snap 15 . This gripping position is discussed in more detail below, in terms of how the rod guide 10 allows a tight, secure fit that is capable of withstanding large axial and rotational forces.
FIG. 5 shows a perspective view of the sleeve 16 used in the embodiment of FIG. 1 . The sleeve 16 has a plurality of radially projecting fins 32 . The sleeve 16 includes an inner wear surface 28 for slidably contacting the outer wear surface 20 of the body 13 and an outer wear surface 30 on a radially outward portion of the plurality of fins 32 in the embodiment shown. In less preferred embodiments fins 32 may be excluded, and an outer surface located at a radially outermost location 31 may alternatively serve as the outer wear surface. The outer wear surface 30 is for contacting the interior tubular surface of the oilfield tubular (not shown). One or more stops 34 are preferably included on the body 13 for limiting axial motion of the sleeve 16 with respect to the body 13 . The stops 34 as shown are a pair of axially spaced load shoulders 34 spaced a distance equal or greater than a length of the sleeve 16 . An access channel 36 is also preferably included with the sleeve 16 , for permitting installation of the sleeve 16 on the assembled body 13 . As shown, the access channel 36 passes radially through the sleeve 16 , partially severing the sleeve 16 to create circumferential side surfaces 54 , 56 , and extends longitudinally from one end 50 of the sleeve 16 to an opposing end 52 of the sleeve 16 . Although the channel 36 in a relaxed state may be more narrow than an OD of the body 13 , the channel 36 permits flexibly spreading of the sleeve 16 to move apart circumferential side surfaces 54 , 56 and pass the body 13 through the access channel 36 . The channel 36 may also be merely a cut, having a small or even nominally zero thickness, such that no appreciable spacing exists between circumferential side surfaces 54 , 56 . Thus, by spreading the sleeve 36 , such as by flexing by hand, the sleeve 16 may be installed about the body 13 . The spreading force applied to the sleeve 16 may then be released, allowing the sleeve to retract about the body 13 .
Because the channel 36 allows outward flexing of the sleeve 16 , the sleeve 16 may flex and move about the body 13 during use. This creates a possibility of increased wear between the sleeve 16 and the body 13 , and the possibility that the sleeve 16 may inadvertently come off the body 13 . To decrease the chance of these occurring, a locking bridge may be included, as shown generally at 60 in the cross-sectional view of the sleeve embodiment of FIG. 9 . The locking bridge 60 may selectively bridge the access channel 36 to at least limit outward spreading of the sleeve 16 , i.e., at least limit circumferential separation of circumferential side surfaces 54 , 56 , and in some embodiments to draw the circumferential side surfaces 54 , 56 toward one another. For example, as shown, the locking bridge 60 comprises a male member 62 secured to the sleeve 16 and a female member 64 secured to the sleeve 16 for lockingly receiving the male member 62 . The locking bridge 60 may comprise a plurality of members axially spaced along the sleeve, or the locking bridge 60 may have an axial length that is a considerable fraction of the length of the sleeve, such as between 50-100% of the length of the sleeve.
In the preferred embodiment shown, the male member 62 and the female member 64 are positioned within the access channel 36 between arcuate surfaces 66 , 68 , each secured to a respective one of the circumferential side surfaces 54 , 56 . The male member 62 locks into a similarly shaped female member 64 , bridging the channel 36 , and limiting spreading of the sleeve 16 . Preferably, this locking moves circumferential side surfaces 54 , 56 into contact with one another, to seal or at least limit passing of sand, fluid, and debris through the channel 36 . In other embodiments, the locking bridge may be secured elsewhere on the sleeve 16 , such as on arcuate surface 66 , to draw surfaces 54 , 56 toward one another and bridge the channel 36 . For example, in one embodiment (not shown), two members may be secured to the surface 66 opposite the channel 36 from one another, and a buckle included for fastening the two members, to both bridge the channel 36 and preferably draw surfaces 54 , 56 toward one another.
Progressive cavity pumps are sometimes used in sand applications because they are able to move fluid with sand therein. FIGS. 7 and 8 show another embodiment of the rod guide 10 including a pair of axially spaced seal assemblies indicated generally at 33 , circumferentially sealing between the body 13 and the sleeve 16 , each seal assembly 33 being positioned at opposing ends of the outer wear sleeve 16 . Each seal 37 ( FIG. 8 ) seals with a respective one of a pair of axially spaced circumferential grooves 35 ( FIG. 7 ). The grooves 35 are preferably positioned radially outward of the outer wear surfaces 20 , for increasing resistance to intrusion by sand. The seals 37 are preferably elastomeric o-rings, but may also be other types of seals known in the art, such as lip seals.
In other embodiments (not shown), the seal assemblies 33 can instead be located on or adjacent to load shoulders 34 . For example, a grooves can be included on shoulder 34 , and still accommodate a circular seal, such as an o-ring or lip seal, to seal with sleeve ends 50 , 52 .
FIG. 6 illustrates a less preferred alternative embodiment of a rod guide 100 for a reciprocating type rod. Body members 112 , 114 include the same features described for engaging body members 12 , 14 of the rotating type rod guide 10 , but lack the sleeve 16 or stops 34 of that other embodiment. Radially projecting fins similar to fins 32 may be included (but are not shown) directly on the body 13 . However, some embodiments having a sleeve 16 as in FIGS. 1-5 may also be used with a reciprocating type rod. This would decrease tooling and associated costs, because the same body 13 and sleeve 16 may then be used for both rotating and reciprocating type rods. Because the sleeve 16 may already have fins 32 , use of the sleeve 16 with reciprocating rods would eliminate the need for a separate rod guide embodiment having fins directly on the body 13 .
The at least one outer tapered surface 22 of the first and second body members 12 , 14 are preferably a pair of circumferentially spaced outer tapered surfaces 22 , as shown in FIG. 1 . The pair of outer tapered surfaces 22 should circumferentially extend at least a combined 70 degrees from circumferentially outer locations 40 no greater than 180 degrees apart to circumferentially inner locations 42 . The outer tapered surfaces 22 preferably extend at least a combined 90 degrees, as shown. Individually, each outer tapered surface 22 should extend circumferentially at least 35 degrees, and preferably at least 45 degrees as shown, i.e. the distance between the outer location 40 and inner location 42 of each tapered surface 22 is preferably at least 35-45 degrees. As best seen in FIG. 3 , the circumferentially outer locations 40 of the first body member 12 may be spaced very closely (preferably less than 5 degrees) to adjacent circumferentially outer locations 40 of the second body member, creating a substantially continuous outer tapered surface 22 . This novel geometry is largely responsible for the rod guide's strong engagement with the rod. First, the circumferentially outer locations 40 of the tapered outer surfaces 22 cause the body members to deform inwardly in proximity to the circumferentially outer locations 40 . This deformation pinches the rod at these locations 40 and may induce a non-circular inner rod-engagement surface 24 , to increase frictional engagement with the rod. Second, because opposing tapered surfaces 22 circumferentially extend to circumferentially inner locations 42 spaced less than 180 degrees, the opposing tapered surfaces 22 induce a radially inward force component to draw the body members 12 , 14 radially inward toward one another about the rod. Third, because each tapered surface 22 preferably extends at least 45 degrees, and a combined distance of at least about 90 degrees, a gripping force is applied over a large area of the rod. As compared with the prior art, this causes a stronger total force and results in a very robust engagement with the rod. As discussed further below, these features are therefore highly important for use with reciprocating type rod guides, which may experience higher forces downhole than do rotatable rod guides.
As best seen in FIGS. 3 and 4 , an intermediate flange 44 may be included, extending between the pair of outer tapered surfaces 22 of the first and second body members 12 , 14 . The intermediate flange 44 defines a portion of the outer wear surface 20 . An intermediate channel 46 may also be included, dividing a portion of the outer wear surface 20 , such that the channel 46 on one body member 12 , 14 receives the intermediate flange 44 on the other body member 12 , 14 . The intermediate flange 44 of one body member 12 , 14 preferably substantially fills the intermediate channel of the other body member 12 , 14 , forming a substantially continuous combined outer wear surface 20 along a circumferential direction. In simple terms, this feature is what helps the substantially identical body members 12 , 14 “fit together” to form a single body 13 having a continuous outer wear surface 20 .
In the preferred embodiments, as discussed, the body members 12 , 14 are substantially identical. Thus, each body member 12 , 14 has an outer wear surface 20 , a pair of outer tapered surfaces 22 , an inner taper engagement surface 26 for engaging the outer tapered surfaces 22 of the other body member 12 , 14 , and an inner rod-engagement surface 24 . In less preferred embodiments, however, the invention may work conceptually with less symmetry and identity between parts. At a minimum, the first body member 12 should include the outer wear surface 20 , the at least one outer tapered surface 22 , and the inner rod-engagement surface 24 , and the second body member 14 should include the outer wear surface 20 , the inner taper-engagement surface 26 , and the inner rod-engagement surface 24 . In other words, only one of the body members 12 , 14 needs the outer tapered surface 22 , and the other of the body members 12 , 14 needs the taper-engagement surface 26 .
A reciprocating type rod guide 100 may require greater holding power than a rotating type guide 10 , due to the large axial forces of the former as compared with the low rotational forces of the latter. Thus, the aspects of the invention discussed above whereby the outer tapered surfaces 22 provide large gripping power is particularly advantageous for reciprocating type guides 100 .
Although specific embodiments of the invention have been described herein in some detail, it is to be understood that this has been done solely for the purposes of describing the various aspects of the invention, and is not intended to limit the scope of the invention as defined in the claims which follow. Those skilled in the art will understand that the embodiment shown and described is exemplary, and various other substitutions, alterations, and modifications, including but not limited to those design alternatives specifically discussed herein, may be made in the practice of the invention without departing from the spirit and scope of the invention. | A field-installable rod guide for a rod moveable within an oilfield tubular having an interior tubular surface for driving a downhole pump to pump liquids to the surface through the oilfield tubular. The rod guide comprises a body including interfitting body members. An outer tapered surface on one body member is engaged by an inner taper-engagement surface on the other body member, to urge the body members toward a rod gripping position about the rod. The mechanism disclosed provides a particularly strong engagement with the rod, so that the rod guide may be used for either reciprocating or rotating rods. For rotating type rod guides, an outer sleeve may be included about the body. | 4 |
FIELD OF THE INVENTION
The present invention relates generally to detecting and logging signals from a TV remote control that can later be reviewed.
BACKGROUND OF THE INVENTION
Television filtering devices known as V-chips have been provided that can be used to prevent certain programs from being displayed on a TV. A parent, for example, can instruct the V-chip not to display programs with certain ratings. In this way, a parent can ensure that certain programs will not be viewed by a child when the parent is away.
It will readily be appreciated that V-chips depend on the ratings of programs. These ratings are not assigned by the parent, but rather by the broadcaster or content provider or some other external agency, meaning that all parents in essence are at the mercy of the rating discretion that is exercised by a third party or unknown entity. It happens that many programs which are given normally acceptable ratings, e.g., “general audience” ratings, might in fact be highly objectionable to some parents. Violent cartoons, music shows featuring profane, infantile chants, and the like all might be given ratings that skirt under the levels set by the parents for blocking objectionable content through V-chip or similar blocking technology.
As recognized herein, one way to empower parents to address the above problem is to provide them with a way to review what their child has viewed while alone. As further understood herein, tracking a child's channel selections can be challenging if not impossible with existing TVs.
SUMMARY OF THE INVENTION
An interceptor includes a processor and an infrared interceptor receiver receiving TV channel commands originating from a TV remote control. The receiver communicates the commands to the processor. In response, the processor accesses a database to correlate the commands to TV programs and to generate a log of programs displayed on a TV, with the log being displayed on an output device.
In some embodiments the processor and receiver are in an interceptor housing that is separate from the TV. Thus, the TV includes a TV wireless command receiver separate from the interceptor receiver. In another embodiment the processor and receiver are in a TV housing, with the processor being implemented by a TV processor and with the receiver being implemented by a TV wireless command receiver. In still other embodiments, the interceptor housing does not implement a set-top box, while in still other embodiments the interceptor housing does implement a set-top box.
If desired, in non-limiting implementations in response to detecting a power on signal originated by the remote control, the processor sends a command to the TV to cause the TV to tune to a predetermined channel. An extender may be provided for receiving IR signals from a TV remote control and relaying the signals in RF to an extender on the interceptor. The extender on the interceptor transforms the signals from RF to IR.
In another aspect, a method for logging television use includes receiving channel change signals from a TV remote control, correlating the channel change signals to TV programs, and displaying a log of the programs to a user. If desired, the log can be displayed only upon input of proper authentication information.
In another aspect, a system includes a TV defining a TV chassis and a remote control configured for sending wireless command signals to the TV. A set-top box communicates with the TV and defines a STB housing. An interceptor is in a housing that can be separate from the TV chassis and set-top box housing and that receives signals from the remote control. The interceptor logs the signals.
The details of the present invention, both as to its structure and operation, can best be understood in reference to the accompanying drawings, in which like reference numerals refer to like parts, and in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a non-limiting hardware block diagram of a system in accordance with present principles, with portions of the STB and TV cutaway for clarity; and
FIG. 2 is a flow chart of non-limiting logic in accordance with present principles.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring initially to FIG. 1 , a system is shown, generally designated 10 , which includes a television 12 defining a TV chassis 13 and receiving, via a set-top box (STB) 14 defining a STB housing 15 , audio video TV programming from a head-end 16 , such as a cable or satellite head-end, over a wired or wireless link 17 . The STB 14 and TV 12 are examples of receivers. “Set-top box” also includes set-back boxes. While the STB 14 is shown separately housed from the chassis 18 of the TV 12 , it is to be understood that the functionality of the STB 14 may be incorporated into the chassis 18 .
As shown, the STB 14 includes a STB processor 20 and a computer readable medium 22 such as volatile or non-volatile solid state storage, disk storage, tape storage, or other type of electronic storage medium or logic circuitry that typically can be executed by the processor 20 . The STB 14 typically includes a wireless receiver such as an infrared (IR) receiver 24 for receiving channel, volume, and other commands from a hand-held wireless transceiver 26 on a TV remote control 28 . The receiver 24 communicates with the STB processor 20 . Likewise, a TV wireless receiver 30 may be provided on the TV housing and may communicate with the TV processor discussed below for sending commands from the remote control 28 to the TV processor.
Additionally, as shown the TV 12 typically includes a TV processor 32 and data storage medium 34 . Video may be presented on a display 36 of the TV 12 , e.g., a flat panel matrix display, cathode ray tube, or other appropriate video display.
A wireless interceptor 38 is shown that includes an interceptor receiver 40 communicating with an interceptor processor 42 . The interceptor processor 42 may communicate with an electronic storage medium 44 , which can bear data and logic executable by the interceptor processor 42 . If desired, a display 46 may be provided on the interceptor 38 .
Furthermore, an extender receiver 48 can be provided on the interceptor 38 in non-limiting embodiments, and the extender receiver 48 can communicate wirelessly by, e.g., radiofrequency with an extender 50 that may be physically positioned near, e.g., just in front of, the TV receiver 30 to receive IR command signals, transform them into RF, and send the transformed signals to the extender receiver 48 of the interceptor 38 for conversion, back to IR if desired. The process can be reversed between the receiver 48 and extender 50 . In any case, this facilitates hiding the interceptor 38 from view of children if desired.
As also shown in FIG. 1 , the interceptor 38 may communicate with a database 52 to obtain channel-by-channel program information correlated by time. The database 52 may be accessed over the Internet or it may be stored on, e.g., the TV medium 34 and/or STB medium 22 in electronic program guide (EPG) format.
It is to be understood that the logic shown herein is implemented on one or more of the TV 12 , and/or STB 14 , and/or interceptor 38 . It is to be further understood that the interceptor 38 may be physically integrated with the TV 12 or STB 14 , and thus in some implementations the logic set forth below may be executed by the STB processor 20 and/or the TV processor 32 , with a physically separate interceptor omitted. It, may now be understood that the interceptor 38 may be provided as shown as a standalone device in an interceptor housing 39 that does not require retrofitting of existing TVs and STBs, and thus may not communicate at all with the TV 12 . In other embodiments the interceptor 38 may communicate with the TV 12 only for purposes of displaying a channel history on the TV display 36 , and in still other embodiments the TV processor 32 and/or STB processor 20 can be programmed to execute the logic set forth below.
Turning now to FIG. 2 , to synchronize the interceptor 38 with the channel of the TV (or equivalently, when the channel is being controlled by signaling the STB 14 , the channel of the STB), when the interceptor detects a power-on signal at block 54 from the remote 28 to the TV 12 (or STB 14 ), the interceptor 38 commands the TV 12 (or STB 14 ) to tune to a predetermined channel at block 56 . The interceptor 38 may be provided with an IR or RF transmitter for this purpose, as appropriate.
Since the interceptor 38 is now synchronized with the TV 12 (or STB 14 ) by forcing the TV/STB into a state known to the interceptor 38 , all later channel up/down commands snooped from the remote control 28 can be used to ascertain the accessed channel. The interceptor 38 checks whether it has missed a transmission (and hence made an error for the previous log entry) by comparing sequence numbers in the transmitted packets.
For example, if the present sequence number of packets from the remote control 28 that the interceptor 38 has sniffed/snooped from the wireless medium is #4324, and the last sequence number interceptor 38 saw was #4322, then the interceptor 38 can assume it has missed a transmitted command, in which case it may resynch with the TV/STB by repeating the process at block 56 . In addition, if the interceptor 38 detects an “acknowledge” packet sent from the TV/STB to the remote control 28 but did not see the packet that is being acknowledged, the interceptor 38 may similarly assume it has missed a packet from the remote control to the TV/STB, and resynchronize accordingly.
If desired, to prevent bypassing the interceptor 38 by manually changing channels using the “channel up/down” buttons on the TV chassis 13 and/or on the STB housing 15 , a keyword protected menu option of disabling the “channel up/down” buttons on the TV chassis/STB housing may be provided. Or, the channel up/down buttons on the chassis 13 /housing 15 may be mechanically disabled by, e.g., depositing adhesive onto them.
Alternate synchronization methods may be used. For example, in addition to or in lieu of the above, the interceptor 38 may also perform speech recognition on the TV sound, and then compare the recognized speech to a database containing soundtrack/closed captioned information of the program it thinks is being watched, to confirm that the user is watching the same channel. If a discrepancy exists, the interceptor 38 may either try to resynchronize by finding which program is actually being watched (by comparing speech recognition of TV sound with soundtrack of the channel obtained from a database or closed caption information), or the interceptor 38 may simply force the TV/STB into a known channel by transmitting a “tune to channel x” command to the TV.
Once synchronized, the logic can move to block 58 to receive IR (or RF) wireless channel signals from the remote 28 . The channel signals can include channel up/down signals as well as channel number signals. The signals preferably are timestamped at block 60 , so that when each channel is tuned to and the length of time it is tuned to, along with the channel number itself, preferably is recorded in a data log.
At block 62 , the database 52 preferably is accessed to correlate the channel numbers to associated programs by, e.g., program name and/or rating and/or other program metadata. The log showing the times and channel numbers/programs to which the TV/STB were tuned can be presented at block 64 on, e.g., the TV display 36 or the display 46 of the interceptor 38 . The display of the log may be permitted only upon receipt of proper authentication information, e.g., a parental password, so that only authorized people can view the log.
In non-limiting implementations, recognizing that Internet Protocol addresses can be tracked, data from the International Standard Audiovisual Number (ISAN) system, which may be part of the program metadata, can be used to create the log.
In another implementation, the log generated by the interceptor 38 can be provided for a fee to third parties such as TV ratings agencies.
When the present interceptor logic is implemented by the STB 14 (e.g., in a set-back box implementation), tuning data can be obtained using a universal serial bus (USB) link from the TV 12 to the STB 14 , and since a broadband connection may also be provided between the two components, the STB 14 can implement the logic of FIG. 2 , and also to provide this viewer preference data to third parties if the user chooses.
While the particular TV REMOTE CONTROL SIGNAL LOG is herein shown and described in detail, it is to be understood that the subject matter which is encompassed by the present invention is limited only by the claims. | An interceptor detects command signals from a TV remote control and logs the signals. The signals can be correlated not just to channel number but also to programs by accessing a program/channel database. A log of channels/programs that have been viewed by, e.g., a child can thus be obtained and viewed by a parent. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority under 35USC§120 of allowed US non-provisional patent application Ser. No. 10/932,309, filed Sep. 2, 2004, bearing the same title, the specification of which is hereby incorporated by reference.
TECHNICAL FIELD
[0002] The invention relates to a system and method for testing and repairing installed wiring harnesses.
BACKGROUND OF THE INVENTION
[0003] An electrical wiring harness typically comprises a bundle of individual connector wires of varying gauges, impedances and types, all arranged and distributed at different locations within an installation, such as a transport vehicle. Such wiring harnesses are usually bound together in order to facilitate the installation, repair and maintenance of the wires. The transport vehicle industry, especially the aviation and the automobile industries, makes extensive use of such wiring assemblies.
[0004] In the aircraft industry, wiring harnesses are used to interconnect the various components and subassemblies located within an aircraft. The number of possible electrical interconnections within a harness grows exponentially with the number of wires and connectors. Therefore, electrical problems within a harness are incredibly hard to identify and locate, especially for already installed harnesses.
[0005] In the prior art, a typical method of testing an installed harness is by using a ringing cable. Unfortunately, such a method is inconvenient as it presents numerous drawbacks. Such a method requires that a plurality of operators be deployed at various connection points along the wiring harness, their locations being chosen in accordance with electrical schematics, and the operators communicating and coordinating testing procedures through walkie-talkies. With prior art methods, the operators have to ring cables, one at a time, which requires many operators for complex or multiple connections.
[0006] Another prior art method of testing a wiring harness involves connecting devices to the installed harness via cables and performing the testing. However, such a method requires installation of interface cables and other components from the system for testing. Additionally, it requires the deployment of many operators and the use of maintenance manuals, which makes the process time-consuming, expensive and prone to human error.
[0007] Another problem in the prior art is that of keeping accurate records of the results of testing and maintenance procedures. Currently, such information is manually recorded by operators into wiring diagrams and/or work orders, a practice which is prone to errors and omissions and which does not allow for analysis of the data recorded over time.
[0008] Testing devices such as TDR testing units have been developed to test wiring harnesses, one wire at a time. Unfortunately, prior art TDR methods do not allow for performing testing on multiple wires at a time, which proves to be time consuming and does not allow for gathering complete and accurate information regarding the wires.
[0009] There exists therefore a need for a system and a method for testing an installed wiring harness, which is time and cost efficient.
[0010] Additionally, there exists a need for a system and method for testing an installed wiring harness, which is not prone to human error.
[0011] Furthermore, there exists a need for adequate documentation following testing procedures.
[0012] According to an embodiment, there is provided a method for testing an installed wiring harness, comprising: providing a signal source testing module at a first connection point in the wiring harness; providing a measurement termination testing module at a second connection point in the wiring harness; providing a central management module for controlling the testing modules to coordinate the testing modules to send testing signals from the first connection point to the second connection point, after disconnecting electrical power between the connection points, for performing tests and recording test measurements of the installed wiring harness; and the signal source testing module and measurement termination testing module for sending the test measurements to the management module.
[0013] According to an embodiment, there is provided a system for offline testing of an installed wiring harness, comprising: at least a first and a second testing module, having: a communication module for receiving test specifications and for sending test measurements; testing equipment for generating the test measurements from the test specifications; each of the first and second testing modules being adapted for connection at a connection point in the wiring harness; a central network management module, having: a communication module for providing the test specifications to the testing modules and for receiving the test measurements; and a test management module for controlling the testing modules.
SUMMARY OF THE INVENTION
[0014] Accordingly, an object of the present invention is to provide a system and method for testing an installed wiring harness, which allows automated testing of multiple lines simultaneously, thereby reducing the time and the cost of the testing procedure.
[0015] It is another object of the present invention to provide a system and method for testing an installed wiring harness, which is automated, thereby eliminating human error.
[0016] It is yet another object of the present invention to provide a system and method for testing an installed wiring harness which allows to produce automatically standardized maintenance reports and electronic logbook.
[0017] According to an aspect of the invention, there is provided a method for testing an installed wiring harness, comprising: providing a signal source testing module at a first connection point in the wiring harness; providing a measurement termination testing module at a second connection point in the wiring harness; providing a central management module for controlling the testing modules to coordinate the testing modules to send testing signals from the first connection point to the second connection point, after disconnecting electrical power between the connection points, for performing tests and recording test measurements of the installed wiring harness; and the signal source testing module and measurement termination testing module for sending the test measurements to the management module.
[0018] According to another aspect of the invention, there is provided a system for offline testing of an installed wiring harness, comprising: at least a first and a second testing module, having: a communication module for receiving test specifications and for sending test measurements; testing equipment for generating the test measurements from the test specifications; each of the first and second testing modules being adapted for connection at a connection point in the wiring harness; a central network management module, having: a communication module for providing the test specifications to the testing modules and for receiving the test measurements; and a test management module for controlling the testing modules.
[0019] According an embodiment, there is provided an assembly for interfacing an existing harness connector of an installed wiring harness to a test module, the assembly comprising: a harness-specific connector for connecting to the existing harness connector; a test box connector module connected to the harness-specific connector and for connecting to a test module, the test box connector module comprising a key which is unique to the test box connector module and which is used to identify the test box connector module when connected to the test module.
[0020] According an embodiment, there is provided a method for identifying a test box connector module used in testing an installed wiring harness comprising an existing harness connector, the method comprising: connecting the test box connector module to a test module; detecting a key which is unique to the test box connector module thereby determining the identity of the test box connector module; sending the identity of the test box connector module to a user interface.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] 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:
[0022] FIG. 1 is a block diagram of an automated harness scanner system according to a preferred embodiment of the present invention;
[0023] FIG. 2 is a block diagram of a test module connected to a wiring harness according to a preferred embodiment of the present invention;
[0024] FIG. 3 is a block diagram of an analysis module according to a preferred embodiment of the present invention;
[0025] FIG. 4 is a diagram of an automated harness scanner system having a central management system and distributed test modules according to a preferred embodiment of the present invention.
[0026] FIG. 5 is a schematic diagram of two test modules installed in a wiring harness, testing a wire showing a break point.
[0027] FIG. 6 is a graph of an exemplary TDR return signal obtained when applying a pulse input signal to a wire without shielding defects.
[0028] FIG. 7 is a graph of an exemplary TDR return signal obtained when applying a pulse input signal to a wire with shielding defects.
[0029] It will be noted that throughout the appended drawings, like features are identified by like reference numerals.
DETAILED DESCRIPTION
[0030] As illustrated in FIG. 4 , the present invention is a fully portable automated test system allowing verification of any type of installed wiring harness 27 using a new open platform architecture for the transport industry. Even though the testing system shown in FIG. 4 is used for testing a wiring harness installed in a plane, the testing system could also be used for testing a wiring harness installed in any other installation for which periodical testing, diagnosis and maintenance is required. Such other installations might include, but are not limited to, boats, ships, trains, cars, etc.
[0031] In the preferred embodiment of the present invention, the automated testing system is a distributed network, comprising a plurality of test modules 31 which are connected to the wiring harness 27 at the location of existing harness connectors 29 . The test modules 31 are in communication with a central Network Management System (NMS) 10 , from which the test modules 31 receive information regarding the testing of the wiring harness 27 and to which they send back test results following completion of testing.
[0032] In one embodiment of the present invention the test modules 31 communicate with the NMS 10 over a wireless connection, using a protocol such as TDMA in order to support a large number of test modules 31 , such as in the case of testing a wiring harness 27 having a plurality of connectors at different locations. It is however within the scope of the present invention that the test modules 31 send and receive information through a cable connection.
[0033] The NMS 10 is preferably a computer system having input means, display means and storage means and/or other components well-known to those skilled in the art. In the preferred embodiment of the present invention, the computer system includes, for example, a central processing unit (CPU), random access memory (RAM), read-only memory (ROM), as well as various peripheral devices, each connected to a local bus system. Also coupled to the local bus system are a mass storage device, a keyboard, a pointing device (mouse, trackball, touchpad, etc.), a communication device, etc. The communication device is any device allowing the computer system 11 to communicate with a remotely located device over a communication link, such as a telephone modem, cable modem, ISDN, wireless, etc.
[0034] Now, with respect to FIG. 1 , the preferred architecture of the NMS 10 according to the present invention will be described. The data management module 13 contains all the software required to interface with external storage module 14 as well as the NMS data storage 12 . The external storage 14 contains an electronic logbook unique to each transport vehicle, which contains all transport vehicle electrical information, wiring harness signature and past test results. The NMS storage 12 contains all the historical data, statistical variation data and modeling information for a particular wiring harness 27 . The data management module 13 is a software configuration management tool allowing to control and validate information to be stored in the transport vehicle electronic logbook and NMS storage 12 . Compression data algorithms are preferably used for storing and managing data in an efficient manner on the storage units 12 , 14 .
[0035] The data management module 13 receives data from a signature builder module 11 . The signature builder module 11 generates a wiring harness signature for a given transport vehicle harness 27 based on manufacturing specs. The module 11 generates a listing of the transport vehicle wiring harness basic characteristics and properties in terms of material, gauge, length, resistance, impedance, tolerance, conductivity, cross-talk, insulation and many more. The wiring harness signature may be uploaded by transferring raw data from the transport vehicle manufacturer database. This can be achieved by directly accessing the database or by providing the manufacturing specs on a CD-ROM to the system. Alternatively, the wiring harness signature can be generated by connecting the testing system to the transport vehicle wiring harness 27 . In the case the wiring harness signature is generated, it is the artificial intelligence module 15 that provides it to the data management module 13 .
[0036] The artificial intelligence module 15 is a self-learning tool for optimization which enables modification of its own program based on its learning experience. The artificial intelligence module 15 provides diagnosis and recommendations based on historical data, models and test data results received from the test modules 31 through the communication module 21 .
[0037] As shown in FIG. 3 , in the preferred embodiment of the present invention, the artificial intelligence module 15 includes a signature update module 49 and an analysis module 51 . The signature update module 49 manages historical data, statistical data and signature updates from test results received from test modules 31 . If a signature is not available for a given installed wiring harness 27 , the signature module 49 allows building a signature by performing a series of test and gathering a set of electrical characteristics of the wiring harness 27 . When the signature update module 49 receives the test results from all the test modules 31 and no signature is available for a specific transport vehicle wiring harness 27 , then it will generate and store the harness signature. The signature update module 49 will propose signature changes to the Data Management module 13 by requesting the storage of all information previously detected and measured such as connectivity table, Netlist, which describes the connectivity of the wiring harness, or the wire mapping between each connection point, and includes each of the wires' physical attributes, and all electrical characteristics measured and provided by test modules 31 in the format of a harness signature.
[0038] The electrical harness signature contains information that is unique for each wire of the wiring harness 27 . The harness signature for each wire describes the electrical characteristics of that particular wire. In the preferred embodiment of the present invention, the harness signature is a multiple-dimensional array. Table 1 illustrates an exemplary harness signature structure:
[0000]
TABLE 1
VARIABLE
TYPE
CONNECTION
DYNAMIC MULTIPLE DIMENSION
ARRAY
WIRE SPECIFICATION
ARRAY
DC MEASUREMENTS
ARRAY
AC MEASUREMENTS
ARRAY
SWR MEASUREMENTS
ARRAY
SWR RETURN SIGNALS
DYNAMIC MULTIPLE DIMENSION
ARRAY
TDR RETURN SIGNALS
DYNAMIC MULTIPLE DIMENSION
ARRAY
SPECTRUM IMPEDANCE
DYNAMIC MULTIPLE DIMENSION
MEASUREMENTS
ARRAY
[0039] The connection variable is a dynamic, multiple-dimension array containing information in wire connection to other points in the wiring harness 27 . The wire specification variable is an array of manufacturer specifications, such as conductor material, shielding material, gauge, insulation, conductance, dilatation, etc.
[0040] The “DC measurements” variable is preferably an array containing measured voltage and current values, as well as resistance and conductance values.
[0041] The “AC measurements” variable is another array containing voltage and current values measured for different AC input signals. In the preferred embodiment of the present invention, sinusoidal signals of 1 kHz, 100 kHz and 1 MHz of 1 V peak-to-peak are used as input signals. The AC measurements include values of calculated impedance.
[0042] The “SWR measurements” variable is an array containing time delay values for the return signal from an input sinusoidal signal. In the preferred embodiment of the present invention, sinusoidal signals of 1 kHz, 100 kHz and 1 MHz of 1 V peak-to-peak are used as input signals. The SWR measurements also include values of calculated conductor length or break point based on the Doppler equations.
[0043] The “SWR return signals” variable is a dynamic multiple dimension array containing all sample data points for the return signal from an input sinusoidal signal.
[0044] The “TDR return signals” variable is a dynamic multiple dimension array containing all sample data points for the return signal from an input pulse signal, sent at various frequencies, preferably at 1 KHz, 100 KHz and 1 MHz.
[0045] The “Spectrum impedance measurements” variable is another dynamic multiple dimension array containing measured impedance values, in polar and vector form, for a 1-V peak-to-peak input sinusoidal signal. Preferably, the input sinusoidal is varying over a frequency spectrum from 1 KHz to 1 MHz in steps of 50 KHz. This array contains as well calculated Nyquist plot data over the 1 KHz to 1 MHz spectrum.
[0046] The artificial intelligence module 15 also includes an analysis module, which is a self-learning module with the capability to give a diagnosis and recommendation on a transport vehicle wiring harness 27 . The analysis module 51 receives test results from the test modules 31 . Also, this module 51 receives the harness signature and statistical data from the signature update module 49 . Then, this module retrieves the wiring harness model from the NMS storage 12 through the data management module 13 to perform a diagnosis and recommendation. The diagnosis/recommendation is sent to the test management module 17 . Finally, this module will decide to send or not a new harness model analysis to the data management module 13 based on the new learning experience.
[0047] The test management module 17 sends the test specification regarding the measurements to be performed by each of the test modules of the system. The test management module 17 is also in communication with an analysis module 15 for receiving either a diagnosis or recommendations and a harness signature for the wiring harness 27 . The test management module can also provide this information for the operator through a report module 23 or a user interface module 25 .
[0048] The test management module 17 communicates with the network of distributed test modules 31 through a communication module 21 . In the preferred embodiment of the present invention, the communication module is a transmitter (emitter/receiver) communicating to each test module 31 using a STAR configuration. The module 21 is a HUB assigning and managing all frequencies, signal strength, power and time slots in the testing system.
[0049] The report module 23 is an automated tool used to format special printouts, such as metallic labels, cable prints, as well as parts and inventory numbers. The report module 23 may also be used as a tool for generating Quality Assurance and maintenance reports including the test results collected during a given test session or past test results. The report module 23 receives all the information required from the test management module 17 .
[0050] The user interface module 25 controls all the man machine interfaces required for data input and output. It can display on-line schematic diagrams, Netlists and any wire characteristics and properties, as well as the transport vehicle electronic logbook.
[0051] The maintenance management module 19 is an assistance tool to any operator using the automated testing system. It provides a step-by-step procedure to guide the operator in testing a transport vehicle wiring harness 27 for a specific vehicle sub-system. The maintenance management module 19 , through the user interface module 25 , prompts the operator by asking which sub-system to test and provides the user with information regarding the number of test modules required, where to connect them and their location within the transport vehicle.
[0052] In a first step, the operator would identify a faulty subsystem within the wiring harness 27 , by using on-board computers with built-in self-test (BITES) capabilities. If the subsystem cannot be identified by the BITES, the operator will review indicators, sensors information as well as the pilot's flight book to identify the subsystem.
[0053] The operator will then load a specific CD-ROM aircraft logbook in the computer, which contains all wiring harness information for the particular aircraft. The system first prompts the operator to enter the aircraft sub-system to test. Then, the HS2000 maintenance program replies with the number of test modules 31 and test box connectors modules required to perform the test as well as the locations of aircraft connectors to be tested.
[0054] The operator then disconnects the aircraft-specific harness connector 29 from the aircraft wiring harness 27 and connects the test module 31 with the appropriate connector module 33 . Then, the operator powers on the test module 31 , at which time the test module is automatically assigned a system ID by the NMS. The system ID contains a time slot, frequency and signal strength according to the TDMA protocol. This procedure is repeated for all test modules 31 to be connected.
[0055] After having installed all test modules 31 , the operator then returns to the computer to start the testing routine. If any problems occurred during installation, the system will notify the operator. Otherwise, the operator is prompted to start the test. In this example, the operator starts the landing gears controls sub-system test on the computer and receives the test results indicating any electrical wiring problems, faults and their locations.
[0056] The operator will then visually inspect the locations at which the problems/faults have been identified. Then, the operator will carry on the repair (splice, solder, connector).
[0057] Then the operator returns to the system 10 to retest the sub-system under test and the system provides a new set of test results from the electrical wiring harness. If no other problems are detected, the new harness signature is recorded in the system 10 .
[0058] As a last step, the operator returns to the aircraft and connects all harness-specific connectors 29 to aircraft harness 27 equipment. Then, the operator re-runs the BITES on the sub-system under test or directly performs some trials on the aircraft harness 27 equipment. If problems are identified on the aircraft harness 27 equipment, then the operator restarts the testing procedures.
[0059] If no problem occurs, a work order will be issued with the details of the repairs, validated by maintenance quality controls, and registered in the company database. Also, the new electrical harness signature, schematics updates, notes and all other aircraft changes will be recorded in the aircraft electronic logbook, which as in this example, could be a CDROM. Finally, the aircraft electronic logbook is stored in the aircraft. In the example, the logbook is on CDROM and kept in the aircraft.
[0060] A test module 31 is the component that contains all testing equipment required in order to generate the measurements data to support any test specifications. The Test Specification information received from the NMS 10 , through the communication module 47 , is processed by the measurement management module 45 and sent to the appropriate testing units.
[0061] As shown in FIG. 4 , test modules 31 connect to a harness-specific connector 29 through a connector module 33 . Each connector module 33 can be customized for a specific type of harness connector 29 or can be of a generic standard connector type. A connector module 33 can be connected to more than one harness-specific connector 29 . The connector module 33 is auto-detected and controlled by the measurement management control module 45 to identify the number and type of harness-specific connectors 29 available to be connected to the test modules 31 . Then, the information about the connectors available for test is sent to the test manager module 17 . The harness-specific connectors 29 connected to the test box connector module 33 are switched and scanned by the multiplexer module 35 .
[0062] The multiplexer module is a circuit switch multiplier, which can be cascaded as needed to achieve a predetermined number of test points. It is controlled by the measurement management module 45 and redirects any signals to the right harness-specific connector 29 wires to be tested.
[0063] The measurement management control (MMC) module 45 receives, through the communication module 47 , test Specification from the NMS 10 . The MMC module 45 determines which testing units 37 , 39 , 41 , 43 are required to produce raw data measurements. The module 45 then coordinates and synchronizes the testing units to avoid any interference. The MMC module 45 detects the test box connector module 33 connected to the test modules 31 using a hardware coded key, which is unique to each test box connector module 33 . The MMC module 45 sends the list of connectors available to connect the harness specific connector module 29 to the NMS 10 . Then, the operator will know which connector on the test box connector module 33 to plug the harness specific connector 29 . Also, the MMC module 45 controls the connector selections and the wires scanning for each connector. Finally, it produces, stores and sends test results information to the NMS 10 . The test results are produced by equipment measurements, but also by correlating the measurements received from the Standing Wave Ratio (SWR) module 39 , Time Domain Reflectometry 41 and spectrum impedance 43 modules. Such combined information is used specifically for shielding wire detection, cross-talk and coupling problems. Signal data processing is used on the return signal from the SWR module 39 , TDR module 41 and Spectrum Impedance module 43 to extract and store the information required to characterize the actual condition of the wire. Then, information from the three modules are correlated and aligned with a transmission line model and wire specification under test. Finally, the information is sent to NMS 10 to compare with the previous harness signature and to get a diagnosis.
[0064] In the preferred embodiment of the present invention, the initial harness signature is generated from specifications given by the electrical harness manufacturer or tests performed on the harness. Whenever a test is performed on the wiring harness 27 and a previous signature exists, the signature comparison is performed as follows. First, a Netlist comparison is performed to verify all connectivity differences between the existing signature “connection” variable and the new measurements. The Al module 15 will perform the comparison. At the same time, the “DC measurements” and “AC measurements” variables are used to determine whether any “open or “short” problems are present within the harness. If any are detected, the Al module 15 uses the “SWR measurements” from the signature to determine the break point location of “open” or “short” within the length of the wire. As per FIG. 5 , the system uses a test box unit “TBU” at each end of the wire, giving more precision as to the location of the break point within the length of the conductor.
[0065] The Al module 15 then uses the “SWR return signals”, “TDR return signals” and “Spectrum impedance measurements” in order to detect shielding defects. The information provided by the “TDR return signals” data and the “Spectrum impedance measurements” is used with correlation algorithms well known in the art to detect a shielding defect. Whenever a shield defect has been identified, the Al module 15 determines its exact location by using the “SWR return signals” data. Signal processing including moving range, correlation and data mining algorithms are used in order to detect the location of a shielding problem.
[0066] FIG. 6 illustrates the “TDR return signal” from a previous harness signature, in which no shielding defect is present. FIG. 7 shows the “TDR return signal” received after performing a series of measurements on the same harness after some time. FIG. 7 shows a shielding defect present in one of the wires.
[0067] In the preferred embodiment of the present invention, the Al module 15 uses previously stored “TDR return signal” data to compare the received “TDR return signal” data. If a shielding problem is detected, then the Al module 15 applies correlation and data mining algorithms to the received “TDR return signals” data and the received “Spectrum impedance measurements” to determine the size of the shielding defect. The Al module 15 then uses “SWR return signals” data with moving range/Doppler algorithms to determine the location of the shielding defect. The Al module 15 can use the other variables data in the received signature whenever more data or calculations are required by the Al models to determine the size or location of shielding defect.
[0068] In the case in which the analysis of the received “TDR return signal” data shows a difference when compared to the stored “TDR return signal” data, the significance of the change is assessed in order to determine the gravity of the problem. At the time of analysis of the data, the relationship between the physical wire characteristics and the electrical properties of the wire being tested would be taken into account. The relationship between the two would be used to assess the impact of a change in the physical wire characteristics on the electrical properties of the wire. Another factor taken into account by the Al module 15 when performing the assessment is the actual use of the wire being tested. For example, the type of voltage and current carried by the wire would play a role in determining the sensitivity of the electrical properties of the wire to changes in its physical characteristics. Such a complete assessment performed by the Al module 15 would allow to provide different diagnostics and recommendations depending on the gravity of the detected problem. In one case, upon detecting a shielding defect in a wire being tested, the Al module 15 might recommend that the wire be replaced, in other cases, the Al module 15 might recommend that the wire simply be submitted to a visual inspection, while in other cases, the change would simply be recorded in the electrical signature without signaling a defect. It is knowledge about the use of the wire within the harness system 27 that would allow the Al module 15 to set different pass/fail thresholds for different types of wire and to make recommendations accordingly.
[0069] Now, returning to FIG. 2 , the communication module 47 receives test specifications from the NMS 10 and sends back test results. In the preferred embodiment of the present invention, the communication module 47 is a slave transceiver (Transmitter/Receiver). The module 47 receives information from the NMS 10 and passes it to the MMC module 45 .
[0070] In the preferred embodiment of the present invention, and as shown in FIG. 2 , a test module 31 includes testing units such as: a circuit switch and polarity analyzer module 37 , a standing wave ratio (SWR) module 39 , a TDR module 41 and a spectrum impedance module 43 .
[0071] The main functions of the circuit switch and polarity analyzer module 37 are to perform a continuity test and an active electronic components verification test. Also, this module 37 performs all DC testing of the transport vehicle wiring harness 27 . The module 37 contains the following two sub-modules: a circuit switch analyzer and a polarity analyzer.
[0072] The circuit analyzer performs a continuity check for all possible harness connections and produces a mapping connection, which is stored in a table. The polarity analyzer performs a test to verify any active components like transistor, diode or semi-conductors in the wiring harness 27 . The polarity analyzer verifies and determines the direction of the current and gathers all the raw data required by the Al module 15 .
[0073] The standing wave ratio module 39 is a testing unit, which sends a pure sinusoidal wave through each conductor of the wiring harness 27 and measures the return in terms of time, voltage and sinusoidal shape. It contains a unique “Transmission Line Model” specific to the transport vehicle industry and a state-of-art data signal processing system in order to analyze the return signal. The SWR module 39 can calculate the break point of a conductor in the wiring harness 27 using Doppler equations. This module 39 generates raw data measurements required by the NMS 10 for providing a diagnosis of the wiring harness 27 .
[0074] The Time Domain Reflectometry (TDR) module 41 is a testing unit, which sends a small amplitude pulse through each conductor of the wiring harness 27 in order to characterize it. It uses Fast Fourier Transforms (FFT) and Laplace Transforms to compute and produce raw data measurements and a state-of-art data signal processing system to extract and analyze the return signal.
[0075] The spectrum impedance module 43 is a testing unit, which measures AC resistance with different signal voltage over a spectrum of specific frequencies. The spectrum impedance module 43 produces polar and vector representations for each wire impedance over a specific frequency spectrum (Nyquist plot). Also, the spectrum impedance module 43 uses a state-of-art of data signal processing system to extract and analyze the return signal for each frequency. The module 43 generates raw data required by the NMS 10 and stores the information in a table. In the preferred embodiment of the present invention, this module 43 has auto-range calibration abilities using the successive approximation method.
[0076] The embodiments of the invention described above are intended to be exemplary only. The scope of the invention is therefore intended to be limited solely by the scope of the appended claims. | The present document describes an assembly for interfacing an existing harness connector of an installed wiring harness to a test module, the assembly comprising: a harness-specific connector for connecting to the existing harness connector; a test box connector module connected to the harness-specific connector and for connecting to a test module, the test box connector module comprising a key which is unique to the test box connector module and which is used to identify the test box connector module when connected to the test module. There is described a method for identifying a test box connector module used in testing an installed wiring harness comprising an existing harness connector, the method comprising: connecting the test box connector module to a test module; detecting a key which is unique to the test box connector module thereby determining the identity of the test box connector module; sending the identity of the test box connector module to a user interface. | 6 |
[0001] This application takes priority from U.S. provisional application 60/969,009 filed Aug. 30, 2007.
BACKGROUND
[0002] Barriers are used in many industrial and commercial applications for a variety of purposes. They are often used as barricades to cordon off areas, as safety harnesses on storage racks, etc. The barriers are assembled from barrier elements formed into a mesh or net. The barrier elements are usually straps, ropes or chains, and are made of nylon, polypropylene, cotton, or other material.
SUMMARY
[0003] Mounting straps for a barrier are provided. The barriers comprise an intersecting mesh of barrier elements and an outer edge at the perimeter of the barrier. The mounting straps are attachable to the outer edge of the barrier. The mounting straps comprise at least one finished hole and are anchorable to frame elements by fastening mounting hardware through one of the mounting strap's finished holes.
[0004] In embodiments in which the mounting straps have two finished holes, each mounting strap is anchorable by wrapping the mounting strap around frame elements, aligning the two finished holes to overlap, and fastening mounting hardware through both aligned finished holes. Alternatively the mounting straps could be fastened to anchoring hardware that is in turn anchored to the frame elements.
[0005] Those skilled in the art will realize that this invention is capable of embodiments different from those shown and described herein and that details of the devices and methods can be changed in various manners without departing from the scope of this invention. Accordingly, the drawings and descriptions are to be regarded as including such equivalent embodiments as do not depart from the spirit and scope of this invention.
BRIEF DESCRIPTION OF DRAWINGS
[0006] For a more complete understanding and appreciation of this invention, and its many advantages, reference will be made to the following detailed description taken in conjunction with the accompanying drawings.
[0007] FIG. 1 is a perspective view of a barrier having a plurality of mounting straps attached to all sides of the barrier;
[0008] FIG. 2 is a close up view of one mounting strap attached to the barrier shown in FIG. 1 in which the mounting strap has three finished holes;
[0009] FIG. 3 is a close up view of the mounting strap shown in FIG. 2 in which the mounting strap is anchored to a slotted frame element with mounting hardware fastened to the mounting strap through one finished hole;
[0010] FIG. 4 is a perspective view of a barrier having a plurality of mounting straps attached to two sides of the barrier in which the barrier is anchored between two vertical slotted frame elements;
[0011] FIG. 5 is a close up view of the mounting strap shown in FIG. 2 in which the mounting strap is anchored to a frame element by wrapping the mounting strap around the frame element, aligning the two finished holes to overlap, and fastening mounting hardware through the two aligned finished holes;
[0012] FIG. 6 is a perspective view of a barrier having a plurality of mounting straps attached to one side of the barrier in which the barrier is hanging from a horizontal frame element and the mounting straps are anchored to the frame element by fastening mounting hardware through two finished holes as shown in FIG. 5 ;
[0013] FIG. 7 is a perspective view of a barrier having a plurality of mounting straps attached to three sides of the barrier in which the barrier is anchored to anchoring hardware by fastening mounting hardware through two finished holes, and the anchoring hardware in turn anchored to three sides of a passageway;
[0014] FIG. 8A is a close up view of a mounting strap anchored to anchoring hardware that is an eyebolt;
[0015] FIG. 8B is a close up view of a mounting strap anchored to anchoring hardware that is an O-ring;
[0016] FIG. 8C is a close up view of a mounting strap anchored to anchoring hardware that is a D-ring;
[0017] FIG. 8D is a close up view of a mounting strap anchored to anchoring hardware that is a hook;
[0018] FIG. 8E is a close up view of a mounting strap anchored to anchoring hardware that is a spring clip;
[0019] FIG. 8F is a close up view of a mounting strap anchored to anchoring hardware that is a clamp;
[0020] FIG. 8G is a close up view of a mounting strap anchored to anchoring hardware that is a carabineer;
[0021] FIG. 9 is a close up of a mounting strap that is stitched to the outer edge of a barrier;
[0022] FIG. 10 is a close up of a mounting strap that is riveted to the outer edge of a barrier;
[0023] FIG. 11 is a close up of a mounting strap that is bolted to openings in the outer edge of a barrier; and
[0024] FIG. 12 is a close up of a mounting strap that is an extension of the barrier elements of a barrier.
DETAILED DESCRIPTION
[0025] Referring to the drawings, some of the reference numerals are used to designate the same or corresponding parts through several of the embodiments and figures shown and described. Corresponding parts are denoted in different embodiments with the addition of lowercase letters. Variations of corresponding parts in form or function that are depicted in the figures are described. It will be understood that variations in the embodiments can generally be interchanged without deviating from the invention.
[0026] FIG. 1 shows a barrier 10 having a plurality of barrier elements 12 that are arranged into a mesh. The barrier elements 12 shown in FIG. 1 are ropes, but they can be straps, chains, or any other appropriate elements. In any case the barrier elements 12 can be fixed at their overlapping intersections if called for by the particular application. An outer edge 14 is attached to the perimeter of the barrier 10 by stitches, rivets, or other fastening methods. (If the barrier 10 were made of straps, the outer edge 14 can be the outermost straps of the barrier elements 12 of the barrier 10 .) A plurality of mounting straps 16 are attached to the outer edge 14 . The barrier 10 in FIG. 1 is shown with mounting straps 16 on the perimeter of the barrier 10 , but, as demonstrated herein, it will be understood that mounting straps 16 may be installed on any number of sides as required for the particular application. Each mounting strap 16 is attached to the outer edge 14 with fasteners 15 . In FIG. 1 , the fasteners 15 are stitches, but as shown herein, other methods of attachment are also possible.
[0027] As shown in FIG. 2 , each mounting strap 16 has at least one finished hole 18 located along its length. The embodiment shown in FIG. 2 has three finished holes 18 that are reinforced with metal grommets 20 . The length of the mounting straps 16 and the number of finished holes 18 can be varied depending on the application or the amount of adjustability required. The mounting strap 16 can be made of nylon, polypropylene, cotton, or other appropriate material.
[0028] The mounting straps 16 give users the option of setting up barriers quickly and easily in a variety of ways. For example, FIG. 3 shows a mounting strap 16 a anchored directly to a frame element 22 a that has openings 24 a formed in it. Each mounting strap 16 a is anchorable to the frame element 22 a by fastening mounting hardware 26 a through a finished hole 18 a that is aligned with an opening 24 a in the frame element 22 a . In FIG. 3 , the mounting hardware 26 a comprises a nut 28 a , a bolt 30 a and a washer 32 a , but other types of hardware can be used as required by the particular application. FIG. 4 shows a barrier 10 a having a plurality of mounting straps 16 a attached to two sides of the barrier 10 a in which the mounting straps 16 a are anchored to two vertical frame elements 22 a of storage rack 34 a . The vertical frame elements 22 a have openings 24 a to which the finished holes 18 a of the mounting straps 16 a are aligned and through which mounting hardware 26 a is fastened.
[0029] The mounting straps can be used to anchor barriers in other ways and for other applications. In FIG. 5 a mounting strap 16 b is anchored to a frame element 22 b , such as a pole, the support beam of a storage rack, the I-beam of building, etc. The mounting strap 16 b is wrapped around the frame element 22 b and two finished holes (hidden behind the mounting hardware 26 b ) are aligned to overlap. Mounting hardware 26 b is fastened through the aligned finished holes 18 b . In FIG. 5 , the mounting hardware 26 b comprises a nut 28 b , a bolt 30 b and a washer 32 b , but other types of hardware can be used as required by the particular application. FIG. 6 shows a barrier 10 b having a plurality of mounting straps 16 b attached to one side of a barrier 10 b in which the mounting straps 16 b are anchored to a horizontal frame element 22 b as described in FIG. 5 , above.
[0030] As shown in FIG. 7 , where mounting straps 16 c cannot be wrapped around or anchored directly to support components, the mounting straps 16 c of a barrier 10 c can be fastened to anchoring hardware 36 c that are in turn anchored to frame elements 22 c . In FIG. 7 the barrier 10 c has a plurality of mounting straps 16 c attached to three sides of the barrier 10 c . Each mounting strap 16 c has a pair of finished holes (hidden behind the mounting hardware 26 c ). Each mounting strap is wrapped around anchoring hardware 36 c and the finished holes are aligned and fastened to the anchoring hardware 36 c with mounting hardware 26 c . The anchoring hardware 36 c can in turn be anchored to frame elements 22 a , in this case the frame of a doorway.
[0031] FIGS. 8A-8G show close ups of examples of different kinds of anchoring hardware 36 c - i that can be used. The anchoring hardware 36 c - i can variously be anchored directly to a surface or be anchored to various other hardware devices (not shown) such as clips, quick clamps, spring clamps, eye-bolts, hooks, etc. FIG. 8A-8G shows a mounting strap 16 c - i fastened to anchoring hardware 36 c - 1 that are an eyebolt, an O-ring, a D-ring, a hook, a spring clip, a clamp, and a carabineer, respectively. Other combinations of mounting hardware are readily apparent.
[0032] Mounting straps can be attached to barriers in different ways. FIG. 9 shows a close up of a barrier 10 j showing a pair of mounting straps 16 j that are attached to the outer edge 14 j of the barrier 10 j with fasteners 15 j that are stitches. FIG. 10 shows a pair of mounting straps 16 k attached to the outer edge 14 k of a barrier 10 k with fasteners 15 k that are rivets. FIG. 11 shows a pair of mounting straps 16 l attached to a barrier 10 l with fasteners 15 l that are bolts through openings 38 l in the outer edge 14 l . The mounting straps can also be extensions of the barrier elements 12 m that are secured to the outer edge 14 m with fasteners 15 m that are stitches as shown in FIG. 12 .
[0033] This invention has been described with reference to several preferred embodiments. Many modifications and alterations will occur to others upon reading and understanding the preceding specification. It is intended that the invention be construed as including all such alterations and modifications in so far as they come within the scope of the appended claims or the equivalents of these claims. | Mounting straps for a barrier are provided. The barriers comprise an intersecting mesh of barrier elements and an outer edge at the perimeter of the barrier. The mounting straps are attachable to the outer edge of the barrier. The mounting straps comprise at least one finished hole and are anchorable frame elements by fastening mounting hardware through one of the mounting strap's finished holes. | 4 |
This application claims the benefit of U.S. Provisional Applications No. 60/739,253, filed Nov. 23, 2005 and No. 60/779,791 filed on Mar. 3, 2006.
This invention was made in the performance of a contract with the Office of Naval Research (Contract No. N00014-04-C-0477) and the United States Government has rights in the invention. This invention relates to radio systems and in particular radio systems having features to minimize radio interference.
BACKGROUND OF THE INVENTION
In many radio communications systems it is desirable to maintain continuous bi-directional data transfer (full duplex operation) between two stations. Cellular telephone systems and wireless computer networking systems are examples of two such systems. Currently, in these applications, maintaining the full duplex mode of operation requires that the telephone or radio modem transmit on one frequency range (or band) and receive on another frequency range. This technique is termed frequency diversity. For instance, a cellular telephone may operate in a frequency range around a nominal 800 MHz. That range may extend from about 790 MHz to 810 MHz. The particular telephone may transmit in the lower region of the 800 MHz frequency range (for example 792 MHz to 798) while simultaneously receiving in the upper region of the 800 MHz frequency range (for example 802 MHz to 808 MHz). The frequencies used are usually separated by adequate guard-band (in this example 798 MHz to 802 MHz) so that frequency-selective filters can be used to isolate the transmitter from the receiver while at the same time coupling both the transmitter and receiver to a common antenna. This approach is also known as frequency diplexing. Other techniques, such as the use of circulators, time diversity techniques, spread spectrum codes, or polarization selectivity, have also been employed to separate the transmit signals from the receive signals for full duplex operation, over a single antenna.
During full duplex operation it is crucial that the desired signal from the antenna that appears at the receiver input be stronger than the leakage signal from the transmitter (at the receiving frequency) that appears at the receiver input. For a typical 1-watt (+30 dBm) transmitter, and a received signal strength of −70 dBm at the antenna, the transmitter power at the receiver's frequency must be suppressed by at least 100 dB at the input to the receiver. This is usually achieved by requiring that transmitters have strict limitations on out-of-band emissions, by receiving in a frequency band isolated and separate from that of the transmitter, and by employing high gain antennas to boost the received signal power. If the transmitter power is not suppressed sufficiently at the receiver input, then the sensitivity of the receiver is deteriorated, even though operation may still be possible at some impractically high receive signal levels. Power levels at the receiver input from communication signals captured by the antenna are often in the range of −90 to −20 dBm, so insufficient suppression of the transmitter output will limit the useful range of the receiver and the distance over which full duplex radio communication may be established.
In military radios, due to the spread-spectrum coding and modulation schemes, the signals are spread over several octaves of bandwidth and are at power levels reaching hundreds of watts in CW. For example, the military SINCGARDS radios operate in the 30-88 MHz range at a maximum output power of 50 W per radio. In a cluster of 4 radios, operating simultaneously on a vehicular platform, there exists a worst-case scenario, in which 1 radio is receiving and 3 radios are transmitting, that produces 150 W of transmitting power to interfere with the receiving radio. The issues of co-site interference here are prevalent and enormous. A solution to these co-site issues is the quasi-circulator.
Circulators are known in the industry and provide a means of coupling both a transmitter and a receiver to a common antenna. A circulator is a three-port ferrite (magnetic) device that operates over some RF (radio frequency) bandwidth, and is illustrated schematically in FIG. 1 . A circulator preferentially and circularly transfers power from Port 1 to Port 2 , from Port 2 to Port 3 , and from Port 3 to Port 1 , hence the name. Power input to Port 1 of a circulator will appear mostly at Ports 2 and very little at Port 3 . Typically, about 20 dB less of input power appears at Port 3 . FIG. 2 shows Circulator 14 used to isolate a transmitter from a receiver, and to couple both to a common antenna. In this instance, the circulator provides 20 dB of isolation between the transmitter and receiver. 20 dB of isolation is usually insufficient to prevent power from the transmitter from interfering with a desired signal received from the antenna, so bandpass filters 15 and 16 are added to the transmit and receive signal paths, and frequencies of operation are chosen such that the transmitter signal passes through bandpass filter 15 , but is blocked by bandpass filter 16 , which in turn only passes the received signal from the Antenna 3 . The use of bandpass filters 15 and 16 can suppress the transmitter power that enters the receiver by another 40 dB. This improves the isolation between transmitter and receiver to 60 dB, which is often enough to allow simultaneous transmission and reception of signals. This prior art implementation requires the use of widely separated frequencies for transmit and receive, to take advantage of the isolation provided by bandpass filtering. However, magnetic circulators are not available at all frequency ranges, especially at VLF, LF, HF, VHF and UHF band, and even if available they do not cover a wide bandwidth and can not handle high power.
Antenna polarization selectivity can be used to provide isolation between transmitter and receiver in a full duplex radio, but similar to the circulator approach described above, polarization selectivity usually provides only about 20 dB of isolation between the transmitter and the receiver. Systems which use polarization selectivity to isolate the transmitter and receiver usually also separate the frequencies of operation and employ band pass filtering on the transmitter output and receiver input to provide additional isolation.
FIG. 3 shows the circuit schematic of a Wilkinson divider. These dividers are sometime called “splitters”. Radio power dividers of this type were described in a 1959 paper by Ernest J. Wilkinson. FIG. 3 shows features of a 3-port Wilkinson divider available from suppliers such as Werlatone with offices in Brewster N.Y. These devices can be used as a power splitters as well as power combiners.
Prior art patents describing techniques for providing isolation include U.S. Pat. No. 4,051,475, Radio Receiver Isolation System issued to Campbell; U.S. Pat. No. 4,174,506, Three-port lumped-element circulator comprising bypass conductor issued to Ogawa; and U.S. Pat. No. 4,704,588, Microstrip Circulator with Ferrite and Resonator in Printed Circuit Laminate issued to Kane. No prior art has been shown to adequately address co-site interference mitigation for a system in which multiple like radios are operated in a multi-octave band at very high power levels.
What is needed is a better system for providing radio isolation, in scenarios within which the problem of co-site interference is highly prevalent and harmful.
SUMMARY OF THE INVENTION
The present invention provides a multi-coupler system for isolating radio signals in a transceiver, that includes a transmitter and a receiver, to permit simultaneous transmit by the transmitter and receive by the receiver through a single antenna in the exact same or nearby frequency ranges. This is done so that in-coming receive signals, transmitted from a remotely located radio, being detected by the receiver is much stronger than the portion of the transmit signal unintentionally coupled over by the co-site (or co-located) transmitter. The invention uses a special electronic circuit, termed the quasi-circulator, to couple the antenna to both the co-located receiver and the transmitter. The invention can also be used to couple several transceivers to a single antenna. The quasi-circulator circuit includes a simulated antenna load with an impedance matched to the antenna impedance. The circuit also includes a transformer with its primary side fed asymmetrically by the antenna so that it can pass the desired receive signal with minimum attenuation. The transformer's primary is on the other hand fed symmetrically from both sides by equally small portions of the transmit power from the co-site transmitter, but these signals are 180 degrees out of phase and cancel almost completely in the transformer. The quasi-circulator works, in an unsymmetrical manner as far as the desired receive signal is concerned and in a symmetrical manner as far as the undesired co-site transmit signal is concerned, so that the receiver connected to the secondary side of the transformer receives the desired signal from the remote radio at a much higher sensitivity than it receives the leakage portion of the co-site transmit signal. Thus the invention provides a reduction in excess of 40 to 50 dB in the strength of the co-site transmitter signal at the receiver input, while leaving the signal captured by the antenna reduced by only 3 dB at the input to the receiver electronics.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a prior art circulator.
FIG. 2 shows a prior art circulator located in a transceiver system.
FIG. 3 shows features of a prior art Wilkinson divider.
FIG. 4 is a block diagram showing features of the present invention.
FIG. 5 shows more details of a preferred embodiment of the present invention.
FIGS. 6 a , 6 b and 6 c show how radio energy circulates in the preferred embodiment.
FIG. 7 shows test results showing isolation of more than 70 dB in an idealized situation.
FIG. 8 shows a multi-transceiver embodiment.
FIG. 9 shows an embodiment with high transmit power.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Quasi-Circulator
A block diagram of a preferred embodiment of the present invention which Applicant refers to as a quasi-circulator is shown in FIG. 4 . A detailed diagram of the FIG. 4 embodiment is shown in FIG. 5 . The principal components of the system are: transmitter 1 , receiver 2 , antenna 3 , and quasi-circulator 4 . The principal components of quasi-circulator are: matched load 5 , balun transformer 6 , three 3 dB splitters 8 , 9 a and 9 b and two 10 dB amplifiers 7 a and 7 b . Transmit radio signals from co-site transmitter 1 are divided equally by 3 dB splitter 8 into two paths, one leading to toward antenna 3 and one leading toward matched antenna load 5 . Signals received by from antenna 3 are also equally divided by 3 dB splitter 9 a into two paths, one leading toward matched load 5 and the other leading toward receiver 2 . The signals from antenna 3 and co-site transmitter 1 circle in the quasi-circular to reach receiver 2 using different paths and are thus affected by the quasi-circulator favorably and non-favorably, respectively.
Wilkinson Divider
As shown in FIG. 5 , three off-the-shelf three-port Wilkinson dividers 8 , 9 a and 9 b are used as power splitters. Details of the Wilkinson divider are shown in FIG. 3 . Each port of the Wilkinson divider is of 50-Ohm characteristic impedance. Port 1 is connected to Port 2 by a quarter-wave transmission-line transformer of 70.7-Ohm characteristic impedance. Port 1 is similarly connected to Port 3 by a quarter-wave transformer of 70.7-Ohm characteristic impedance. Port 2 and Port 3 are separated by an isolation resistor of 100-Ohms. When a signal enters Port 1 , it will be split evenly between Port 2 and 3 . The power levels at Port 2 and 3 are half (3 dB down) of the input power less by the insertion loss of the device. Typically, in practical implements of the Wilkinson divider, the power at Port 2 or 3 is 3.2 dB down from the input power at Port, with 0.2 dB being attributed to insertion loss. When a signal enters either Port 2 (or Port 3 ), half of the input power less the insertion loss appears at Port 1 and very little appears at Port 3 (or Port 2 ). Port 2 and Port 3 are thus isolated from one another. The isolation between Port 2 and Port 3 are due to the phasing effects of the two 70.7-Ohm quarter-wave transformers and 100-Ohm resistor. Intuitively, each quarter-wave section adds a 90 degree phase shift to the signal traveling along it. Two quarter-wave sections therefore insert a phase shift of 180 degrees. A signal traveling through the two quarter-wave sections thus cancels with its equal counterpart which in turn travels directly across the resistor. This cancellation causes the desired isolation effect in the Wilkinson divider. Typically, in practical implements of the Wilkinson divider, the isolation between Port 2 and 3 is in the order of 30 dB.
Circling Signals
With reference to FIG. 6 a , the captured energy from antenna 3 (arrow 60 ) passes through splitter 9 a and almost one half appears at the left side of splitter 9 a where it is amplified by low noise amplifier 7 a and presented to the top of balun transformer 6 . This is represented by the thick arrow 63 pointing from right to left, along the top path of FIG. 6 a . Almost one half of the captured antenna energy appears at the right side of Splitter 9 a and continues down the right side path through splitter 8 (arrow 61 ), splitter 9 b , and low noise amplifier 7 b (arrow 62 ), before finally reaching the bottom of balun transformer 6 . By the time the power taking this right hand path reaches the bottom of balun transformer 6 , it is much lower in magnitude (the reduction is estimated to be greater than 50 dB) than that taking the preferential left hand path through Splitter 9 a to the top of balun transformer 6 . The reduction in power of the signal along the bottom path is due to the isolations of the power dividers. The paths of these signals, originated from antenna 3 , are not symmetrical thus allow the propagation of the received signal to the intended destination which is receiver 2 . Since the two signals along the top and bottom path are greatly out of amplitude balance, there is only a 3 dB reduction in power of the received signal, captured at antenna 3 , as it reaches receiver 2 .
Co-Site Transmitter Power is Cancelled in Quasi-Circulator
Similarly, as shown in FIG. 6 b , the transmit power from transmitter 1 is divided equally by power divider 8 , 9 a and 9 b between the radiating antenna 3 and the simulated antenna load 5 . These are illustrated by the two arrows 64 and 67 pointing toward antenna 3 and simulated load 5 and 65 and 66 pointing from right to left, one along the top path and the other bottom path. The change in the arrow thickness of 65 and 66 visually illustrates the effect of reduction in leakage power due to the isolations of power divider 9 a and 9 b , although the drawings are not to scale. The amount of energy, that is not radiated into the air through Antenna 3 or absorbed by simulated antenna load 5 or absorbed in the isolation resistors of the Wilkinson splitters, travels to the left toward receiver 2 . These two substantially equal signals, along the top path 65 and bottom path 66 , are combined in balun transformer 6 with one side 180 degrees out of phase with the other. The differential ports of the balun transformer 6 thus cancel the energy from the two identically similar paths from the co-site transmitter 1 to receiver 2 . Thus, with good phase and amplitude matching between the top path—from transmitter 1 to receiver 2 (containing Antenna 3 )—and the bottom path—from transmitter 1 to receiver 2 (containing simulated antenna load 5 ), most of the co-site transmit energy that would otherwise leak over to the receiver is cancelled before it enters receiver 2 , even though receiver 2 and transmitter 1 are physically allowed to share the same antenna.
Cancelling Unwanted Signals
An additional benefit of the quasi-circulator is the return loss from antenna 3 mismatch, and any noise or harmonics introduced by amplifiers in transmitter 1 are also cancelled or substantially reduced before entering receiver 2 . FIG. 6 c illustrates how reflected energy (arrow 68 ) from Antenna 3 can be imitated by the use of simulated antenna load 5 (arrow 71 ) so that the reflection of the antenna can also be cancelled before it enters the receive radio. In the preferred embodiment, the simulated antenna load 5 is a static circuit which possesses the same reflection coefficient as that of the antenna. However, in other embodiments, simulated antenna load 5 can be a dynamically tunable circuit that imitates the operations of an antenna on the move or within a varying surrounding. The simulated antenna load 5 is therefore a powerful feature which allows an advantageous degree of freedom for dealing with practical environmental effects. This environment-mitigation feature is unique to the quasi-circulator and very powerful in breadth of applications.
In other words, the simulated antenna load 5 can be utilized to approximate the response of the antenna in both the static and dynamic senses. In the static sense, the matched load can be manufactured to offer the impedance response that is precisely that of the antenna, as measured within an anechoic chamber, over the frequency band of interest and at the rated power level. This configuration of the matched load is basic in nature and can be used in most common scenarios. However, when a communication system is intended for a mobile application, the platform upon which the antenna coupler and antenna are mounted operates dynamically. In the dynamic sense, the antenna radiation pattern and reflection are strong functions of the surroundings. Applicant envisions that in such cases, the matched load can be dynamically optimized by means of a calibration algorithm before each use. The calibration routine is a test sequence that can be devised to take into account the operational characteristics of the antenna along with the environmental effects of surroundings and circumstances. Once the calibration routine is exercised, the matched load can be considered to be the most optimized representation of the antenna under the circumstances of deployment, over the frequency band of interest and at the rated power level. The goal of the optimization routine is for maximum transmitter-to-receiver isolation. The means with which the matched load is to be optimized are resistor, inductors, capacitors and transmission lines that are variable in values, phases and characteristic impedances. These variable components are needed so that both the magnitude and phase of the impedance offered by the matched load are tunable.
Net Result
The net result is a reduction of the leakage from the co-site transmitter to the receiver by 40 to 50 dB or more, while reducing the desired received signals from the antenna to the receiver by only 3 dB. Since the signal emitted by transmitter 1 is split between antenna 3 and matched antenna load 5 , by traversing through two power splitters, the transmitter power delivered to antenna 3 is reduced by 6 dB. In preferred embodiments the radios would be configured to simultaneously transmit and receiver voice and/or data over the exact same bandwidth. Quasi-circulator 4 operates on the concept of passive cancellation due to symmetry, hence is signal waveform independent. However, different spread spectrum codes and modulation techniques for the transmitted and the received signals may be employed to further enhance the isolation of the co-site transmit and receive signals beyond the 50 dB that is achieved by quasi-circulator 4 .
Prototype with Off-the-Shelf Components
The specific components used in the prototype referred to above are listed below. The prototype multi-coupler system includes a 200 W quasi-circulator that operates in the 30-88 MHz frequency range. Quasi-circulator 4 was built using splitters from Werlatone (Part No. D7105-10); a hybrid transformer from Wide Band Engineering (Part No. A65B 30-500); 50-ohm resistive load from JFW Industries (part No. 50T-242); and low noise amplifiers from Triquint (part No. TGA 2801). In this embodiment, the antenna of interest was the US Marine Corp OE-254 with an input impedance of 50-ohm. Therefore, the resistive load from JFW was an adequate matched load to emulate the antenna behavior. FIG. 7 shows the measured performance of the 200 W quasi-circulator, built for the 30-88 MHz range, when tested with two matched 50 ohm resistive loads, with one of the 50 ohm loads in the place of the antenna. In this test, the isolation is better than 70 dB. In practical applications, in which a real antenna are used, the isolation between transmit and receive paths is expected to be in the order of 50 dB realistically. Also, qualitative tests by Applicants with the prototype version of the present invention verified the functional performance of the quasi-circulator in the field. The prototype was tested using SINCGARS radios with the US Marines Corp., 3 rd Marine Regiment, at Kaneohe Bay. Applicants were able to successfully receive a weak SINCGARS signal in the presence of three co-site SINCGARS transmitting signals, with each transmitter outputting at the 50 W power level. Applicants estimate that the isolation in these actual field conditions is in the range of 40 to 50 dB.
Multi-User Co-Site System
FIG. 8 shows a deployment of quasi-circulator 4 in a multi-user co-site system, in which multiple transceivers namely TR 1 , TR 2 , TR 3 and TR 4 are attached to the same antenna 3 via switches, splitter/combiner and appropriate amplifiers. For instance, in FIG. 8 , transceivers 12 , 13 and 14 are toggled to the transmit mode through switches 8 , 9 and 10 , while transceiver 11 is toggled to the receive mode through switch 7 . Normally, every transceiver rests in the receive mode and is keyed to the transmit mode when needed. All the transmitting transceivers are routed to antenna 3 through combiner 6 , power amplifier 1 and quasi-circulator 4 . All the receiving transceivers are routed from Antenna 3 through quasi-circulator 4 , low noise amplifier 2 and splitter 5 . In this configuration, quasi-circulator 4 is used to isolate the transmitting transceivers from their receiving counterparts. In our implementation for the 30-88 MHz frequency range, the 4-way divider was bought from Werlatone (Part No. D5920-10) and the switches were bought from Pulsar Microwave (part No. SW2AD-A33).
Modifications and Improvements
Those who are skilled in the art can reference the schematic diagram shown in FIG. 5 and use a variety of circuit elements to practice the present invention. Certain modifications and improvements will therefore occur to those skilled in the art upon reading the foregoing description. The embodiment described herein is based on a specific architecture but the present invention is not so limited, however.
Also, those are skilled in the art will recognize that the circuit elements as shown in FIG. 5 are conventional splitters, hybrid transformer, resistive load and low noise amplifiers which are commercially available through numerous suppliers. Therefore, those skilled in the art can readily realize the quasi-circulator by purchasing, and assembling these components, from companies such as Anaren, Filtran, M/A-COM, MCCI, Mini-circuits, or Werlatone. It must be noted that the catalog of companies listed here is not exhaustive by any means. It is included here to illustrate the fact that the components employed in the construction of the quasi-circulator are common and basic components which are widely available in the RF and microwave industry.
In applications where the transmit power is much greater than 200 W, a configuration as shown in FIG. 9 is more desirable. In FIG. 9 , only one low-noise amplifier is used and it is situated on the secondary winding of the transformer. At such a location, the low noise amplifier will not be prematurely saturated by the transmitter leakage energy. However, the penalty of configuration in FIG. 9 is 6 dB loss along the receive path, instead of 3 dB, and 6 dB loss along the transmit path.
Certain other modifications and improvements will therefore occur to those skilled in the art upon reading the foregoing description. The embodiment described herein is based on a specific architecture but the present invention is not so limited. As indicated above the present invention can be utilized with other well-known radio isolation techniques. It should be noted that the catalog of companies listed here is not exhaustive by any means. It is included here to illustrate the fact that the components employed in the construction of the quasi-circulator are common and basic components which are widely available in the radio frequency and microwave industry. The techniques can also be applied to produce jamming devices to jam other radios while leaving a receiver isolated from the jamming noise. So the scope of the invention should be determined by the appended claims and their legal equivalence. | A multi-coupler system for isolating radio signals in a transceiver, that includes a transmitter and a receiver, to permit simultaneous transmit by the transmitter and receive by the receiver through a single antenna in the exact same or nearby frequency ranges. This is done so that in-coming receive signals, transmitted from a remotely located radio, being detected by the receiver is much stronger than the portion of the transmit signal unintentionally coupled over by the co-site (or co-located) transmitter. The invention uses a special electronic circuit, termed the quasi-circulator, to couple the antenna to both the co-located receiver and the transmitter. The invention can also be used to couple several transceivers to a single antenna. The quasi-circulator circuit includes a simulated antenna load with an impedance matched to the antenna impedance. The circuit also includes a transformer with its primary side fed asymmetrically by the antenna so that it can pass the desired receive signal with minimum attenuation. The transformer's primary is on the other hand fed symmetrically from both sides by equally small portions of the transmit power from the co-site transmitter, but these signals are 180 degrees out of phase and cancel almost completely in the transformer. | 7 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from Korean Patent Application No. 10-2009-0101324, filed on Oct. 23, 2009 in the Korean Intellectual Property Office, the disclosure of which is incorporated herein by reference.
BACKGROUND
[0002] 1. Field
[0003] Apparatuses and methods consistent with the exemplary embodiments relate to a display apparatus which can simultaneously display a plurality of images such as a two-dimensional image or a three-dimensional image, and an image display method therein.
[0004] 2. Description of Related Art
[0005] In general, the outside world is seen by human eyes in three dimensions having widths, lengths and heights. A one-dimensional image and a two-dimensional (2D) image have no significant difference therebetween to human eyes. However, a three-dimensional (3D) image is significantly different to human eyes as compared to the one- and two-dimensional images.
[0006] Recently, 3D image display technologies have been actively developed and commercialized in the field of photography, films, televisions, television games, or the like. Generally, the 3D image display technologies provide a stereoscopic effect using a binocular parallax, which is a major factor in producing the stereoscopic effect in a short distance.
[0007] There are two viewing types for a stereoscopic image, that is, a glasses type and a non-glasses type. The glasses type uses shutter glasses or polarized glasses to view the stereoscopic image.
[0008] Meanwhile, users may have different preferences between the 2D image and the 3D image. For example, certain users who are not accustomed to the 3D image may prefer the 2D image because they feel a vertigo effect while viewing the 3D image, whereas other users who are accustomed to the 3D image may prefer the 3D images because they feel that the 2D image is monotonous. Further, certain users who are accustomed to the 3D image may prefer a specific 3D image, for example, having a depth characteristic. In these cases, a display apparatus which provides either of the 2D image or the 3D image can not satisfy a variety of preferences of users.
SUMMARY
[0009] Accordingly, it is an aspect of the exemplary embodiments to provide a display apparatus which can simultaneously display a two-dimensional (2D) image and a three-dimensional (3D) image, and an image display method therein.
[0010] Another aspect of the exemplary embodiments is to provide a display apparatus which can simultaneously display a plurality of 3D images having different attributes.
[0011] Additional aspects of the exemplary embodiments will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the exemplary embodiments.
[0012] According to an aspect of an exemplary embodiment, there is provided: a display apparatus including: a signal receiving part which receives a first image signal; an image processing part which generates a second image signal and a third image signal based on the received first image signal, and which processes the second and the third image signals to be displayed; a display part which displays images respectively based on the second and third image signals processed in the image processing part; and a controller which controls the image processing part to generate the second and the third image signals, to display the image based on the second image signal in a first region of the display part, and to display the image based on the third image signal in a second region of the display part, the third image signal including a first left-eye image and a first right-eye image generated on the basis of the first image signal, and the image based on the third image signal being displayed in a 3D mode.
[0013] The controller may control the image processing part, if the first image signal is a 2D image signal, so that the first image signal is converted into 3D to generate the third image signal, and so that the image based on the second image signal is displayed in a 2D mode.
[0014] The controller may control the image processing part, if the first image signal is a 3D image signal including a second left-eye image and a second right-eye image, so that the second image signal is generated on the basis of the second left-eye image or the second right-eye image, and the image based on the second image signal is displayed in the 2D mode.
[0015] The controller may control the image processing part so that the second image signal includes a third left-eye image and a third right-eye image, the image based on the second image signal is displayed in the 3D mode, and an alternating display order of the third left-eye image and the third right-eye image is opposite to an alternating display order of the first left-eye image and the first right-eye image.
[0016] The controller may control the image processing part so that the second image signal includes a third left-eye image and a third right-eye image, the image based on the second image signal is displayed in the 3D mode, and the image based on the second image signal and the image based on the third image signal have different stereoscopic effects.
[0017] Depth information corresponding to the second image signal may be different from depth information corresponding to the third image signal.
[0018] The 3D mode may correspond to a viewing mode using shutter glasses or polarized glasses.
[0019] The controller may control the image processing part so that the second image signal includes a third left-eye image and a third right-eye image, the image based on the second image signal is displayed in the 3D mode, and wherein the 3D mode of the image based on the second image signal corresponds to a glasses type, and the 3D mode of the image based on the third image signal corresponds to a non-glasses type.
[0020] The controller may control the image processing part so that the second image signal includes a third left-eye image and a third right-eye image, the image based on the second image signal is displayed in the 3D mode, and wherein the 3D mode of the image based on the second image signal corresponds to a viewing mode using shutter glasses and the 3D mode of the image based on the third image signal corresponds to a viewing mode using polarized glasses.
[0021] The controller may control the image processing part so that the image based on the second image signal is displayed in a Picture In Picture (PIP) mode, a Picture Out Picture (POP) mode, or a Picture By Picture (PBP) mode.
[0022] The controller may control the image processing part so that the image based on the third image signal is displayed in a PIP mode, a POP mode, or a PBP mode.
[0023] According to an aspect of another exemplary embodiment, there is provided an image display method for a display apparatus, the method including: receiving a first image signal; generating a second image signal and a third image signal based on the received first image signal and processing the generated second image signal and the generated third image signal to be displayed in a display part; and displaying an image based on the second image signal in a first region of the display part, and displaying an image based on the third image signal including a first left-eye image and a first right-eye image in a second region of the display part in a 3D mode.
[0024] If the first image signal is a 2D image signal, the first image signal may be converted into 3D to generate the third image signal, and wherein the image based on the second image signal may be displayed in a 2D mode.
[0025] If the first image signal may be a 3D image signal including a second left-eye image and a second right-eye image, the second image may be generated on the basis of the second left-eye image or the second right-eye image, and the image based on the second image signal may be displayed in a 2D mode.
[0026] The second image signal may include a third left-eye image and a third right-eye image, the image based on the second image signal may be displayed in the 3D mode, and an alternating display order of the third left-eye image and the third right-eye image may be opposite to an alternating display order of the first left-eye image and the first right-eye image.
[0027] The second image signal may include a third left-eye image and a third right-eye image, the image based on the second image signal may be displayed in the 3D mode, and the image based on the second image signal and the image based on the third image signal may have different stereoscopic effects.
[0028] Depth information corresponding to the second image signal may be different from depth information corresponding to the third image signal.
[0029] The 3D mode may correspond to a viewing mode using shutter glasses or polarized glasses.
[0030] The second image signal may include a third left-eye image and a third right-eye image and the image based on the second image signal may be displayed in the 3D mode, and wherein the 3D mode of the image based on the second image signal corresponds to a glasses type viewing mode and the 3D mode of the image based on the third image signal corresponds to a non-glasses type viewing mode.
[0031] The second image signal may include a third left-eye image and a third right-eye image and the image based on the second image signal may be displayed in the 3D mode, and wherein the 3D mode of the image based on the second image signal corresponds to a viewing mode using shutter glasses and the 3D mode of the image based on the third image signal corresponds to a viewing mode using polarized glasses.
[0032] The image based on the second image signal may be displayed in a PIP mode, a POP mode, or a PBP mode.
[0033] The image based on the third image signal may be displayed in a PIP mode, a POP mode, or a PBP mode.
[0034] According to an aspect of another exemplary embodiment, there is provided a display apparatus including: a first signal receiving part which receives a first image signal; a second signal receiving part which receives a second image signal; an image processing part which processes the received first image signal and the received second image signal to be displayed; a display part which displays images respectively based on the first image signal and the second image signal processed in the image processing part; and a controller which controls the image processing part to display a first image based on the first image signal in a first region of the display part and to display a second image based on the second image signal in a second region of the display part, the first image being displayed in the first region in a 3D mode and including a left-eye image and a right-eye image.
[0035] The first image signal may include a broadcast signal.
[0036] The first image signal may include a signal transmitted from an external device by the HDMI 1.4 specification.
[0037] According to an aspect of still another exemplary embodiment, there is provided an image display method in a display apparatus, the method including: receiving a first image signal and a second image signal, the first image signal including a left-eye image and a right-eye image; processing the received first image signal and the received second image signal to be displayed in a display part; and displaying an image based on the first image signal in a 3D mode in a first region of the display part, and displaying an image based on the second image signal in a second region of the display part.
[0038] The first image signal may include a broadcast signal.
[0039] The first image signal may include a signal transmitted from an external device by the HDMI 1.4 specification.
[0040] According to exemplary embodiments, a 2D image and a 3D image can be simultaneously displayed, and a plurality of 3D images having different attributes can be simultaneously displayed, to thereby satisfy a variety of user preferences.
BRIEF DESCRIPTION OF DRAWINGS
[0041] The above and/or other aspects will become apparent and more readily appreciated from the following description of the exemplary embodiments, taken in conjunction with the accompanying drawings, in which:
[0042] FIG. 1 illustrates a configuration of a display apparatus according to an exemplary embodiment;
[0043] FIG. 2 illustrates a state that images are displayed in a display apparatus according to an exemplary embodiment;
[0044] FIG. 3A illustrates left-eye images and right-eye images which are displayed in a display apparatus according to an exemplary embodiment, in the case of using shutter glasses;
[0045] FIG. 3B illustrates left-eye images and right-eye images which are displayed in a display apparatus according to an exemplary embodiment, in the case of using polarized glasses;
[0046] FIG. 3C illustrates left-eye images and right-eye images which are displayed in a display apparatus according to an exemplary embodiment, in the case of using no stereoscopic glasses;
[0047] FIG. 4 illustrates a display of three-dimensional images having different depth information in a display apparatus according to an exemplary embodiment;
[0048] FIG. 5 illustrates a case that display orders of left-eye images and right-eye images in a main screen and a sub screen are different from each other, in a display apparatus according to an exemplary embodiment;
[0049] FIG. 6 illustrates a configuration of a display apparatus according to another exemplary embodiment;
[0050] FIG. 7 illustrates a state that images are displayed in a display apparatus according to another exemplary embodiment;
[0051] FIG. 8 is a flowchart illustrating an operational process of a display apparatus according to an exemplary embodiment; and
[0052] FIG. 9 is a flowchart illustrating an operational process of a display apparatus according to another exemplary embodiment.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0053] Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout. The exemplary embodiments are described below so as to explain the present inventive concept by referring to the figures. Redundant description to different exemplary embodiments may be omitted for simplicity of description.
[0054] FIG. 1 illustrates a configuration of a display apparatus 10 according to an exemplary embodiment. Referring to FIG. 1 , the display apparatus 10 includes a signal receiving part 100 , an image processing part 110 , a display part 120 and a controller 130 .
[0055] The signal receiving part 100 may receive a single image signal or a plurality of image signals. The image signal includes a 2D image signal for display of a 2D image or a 3D image signal for display of a 3D image.
[0056] The image processing part 110 processes the image signal received in the signal receiving part 100 to be displayed. Further, the image processing part 110 may convert a 2D image signal into a 3D image signal, and a 3D image signal into a 2D image signal. For example, if the signal receiving part 100 receives a left-eye image and a right-eye image for display of a 3D image, the image processing part 110 may process only the right-eye image, and thus, a 2D image can be displayed using the 3D image signal.
[0057] If the signal receiving part 100 receives a single 2D image signal, the image processing part 110 may convert the received 2D image signal to generate a 3D image signal. Furthermore, if the received image signal is a 3D image signal, the image processing part 110 may convert the received 3D image signal to generate a 2D image signal. In addition, in the case that one image signal is received, the image processing part 110 may perform processing so that an image based on the received image signal and an image based on a converted image signal are displayed.
[0058] The display part 120 displays images on a screen on the basis of the image signal processed in the image processing part 110 .
[0059] The controller 130 controls the image processing part 110 to display a variety of images. That is, the controller 130 controls the image processing part 110 to convert the 2D image signal and the 3D image signal, or to convert an attribute of the 3D image signal, to be displayed.
[0060] FIG. 2 illustrates a state that images are displayed in the display apparatus 10 according to an exemplary embodiment. The display apparatus 10 according to the present exemplary embodiment may display a plurality of images at the same time, for example, in a Picture In Picture (PIP) mode, a Picture Out Picture (POP) mode, or a Picture By Picture (PBP) mode. As shown in FIG. 2 , a PIP screen 220 includes a large main screen 200 and a small sub screen 210 arranged inside of the main screen 200 , which are simultaneously displayed. A POP screen (not shown) includes a main screen (not shown) and a sub screen (not shown) arranged outside of the main screen 200 , which are simultaneously displayed. A PBP screen 230 includes two split screens, that is, a main screen 200 and a sub screen 210 having the same size, which are simultaneously displayed. The display apparatus 10 may simultaneously display, for example, a 2D image on the main screen 200 and a 3D image on the sub screen 210 , and vice versa.
[0061] For example, if a plurality of 2D image signals is received, a part of the 2D image signals may be converted into a 3D image signal, and images based on the remaining 2D image signal and the converted 3D image signal may be simultaneously displayed. Further, if a plurality of 3D image signals is received, a part of the 3D image signals may be converted into a 2D image signal, and images based on the remaining 3D image signal and the converted 2D image signal may be simultaneously displayed. Further, 3D images having different attributes may be displayed on the main screen 200 and the sub screen 210 , respectively, so that a user can select his or her preferred image. Here, the different attributes in the 3D images may refer to difference in depth between the 3D images or difference in display order between the 3D images, which will be described in more detail hereinafter.
[0062] FIG. 3A illustrates left-eye images and right-eye images displayed in the display apparatus 10 according to an exemplary embodiment, in the case of using shutter glasses. A stereoscopic image is obtained by displaying the left-eye images and the right-eye images. To this end, the left-eye images and the right-eye images may be alternately displayed in the order of a first left-eye image L 1 , a first right-eye image R 1 , a second left-eye image L 2 , a second right-eye image R 2 , and so on. Such a display order of the left-eye images and the right-eye images is suitable for viewing a stereoscopic image through the shutter glasses. The shutter glasses operate in synchronization with images displayed in the display apparatus 10 . For example, if a left-eye image is displayed, a left-eye shutter of the shutter glasses is opened and a right-eye shutter thereof is closed. Similarly, if a right-eye image is displayed, the right-eye shutter is opened and the left-eye shutter is closed. Through repetition of these processes, a user can view a stereoscopic image from the images displayed in the display apparatus.
[0063] FIG. 3B illustrates left-eye images and right-eye images displayed in the display apparatus 10 according to an exemplary embodiment, in the case of using polarized glasses.
[0064] When viewing a stereoscopic image through the polarized glasses, the display apparatus 10 displays left-eye images and right-eye images in rows. For example, in the case the a single screen is formed of a plurality of image rows, left-eye images L may be displayed in odd rows and right-eye images R may be displayed in even rows. Here, the display order of the left-eye images L and right-eye images R may be different in another exemplary embodiment. The stereoscopic image which is viewed through the polarized glasses has different polarizations between the left-eye images and the right-eye images. Thus, when a user views the left-eye images and the right-eye images through the polarized glasses having different polarizing plates, the left-eye images and the right-eye images are separately viewed, to thereby provide the stereoscopic image.
[0065] FIG. 3C illustrates left-eye images and right-eye images displayed in the display apparatus 10 according to an exemplary embodiment, in the case of no stereoscopic glasses.
[0066] In this respect, a non-glass type refers to viewing a stereoscopic image without stereoscopic glasses. In this case, there are provided elements for splitting left-eye images and right-eye images in front of a screen on which the images are displayed. A user can view the left-eye images with a left eye and the right-eye images with a right eye, to thereby feel a stereoscopic image. The non-glass type may include a parallax barrier type, a lenticular type, or the like. In the case of the non-glass type, the left-eye images and the right-eye images are displayed in columns. For example, in the case that a screen is formed of a plurality of image columns, left-eye images L may be displayed in odd columns and right-eye images R may be displayed in even columns. The display order may be different in another exemplary embodiment.
[0067] FIG. 4 illustrates a display of 3D images having different depth information in the display apparatus 10 according to an exemplary embodiment. 3D images using the binocular parallax has a characteristic that a stereoscopic effect and a comfort conflict with each other. Further, since a mechanism for recognizing a stereoscopic image is quite complex, even images having the same depth may provide different stereoscopic effects and comforts. Thus, if a user has a selection for depths of 3D images, the user can comfortably enjoy his or her preferred stereoscopic effect. To this end, the display apparatus 10 according to the preset exemplary embodiment may display 3D images having different depths on the main screen 200 and the sub screen 210 , respectively. For example, as shown in FIG. 4 , a 3D image having a first depth may be displayed on the main screen 200 , and a 3D image having a second depth may be displayed on the sub screen 210 . Thus, the user can select images having his or her preferred depths while viewing the main screen 200 and the sub screen 210 , so that the user can view a stereoscopic image having his or her preferred depth through a full screen.
[0068] FIG. 5 illustrates a case that display orders of left-eye images and right-eye images in a main screen and a sub screen are different from each other, in the display apparatus 10 according to an exemplary embodiment. In the case that a user views a stereoscopic image through the shutter glasses, a left-eye shutter and a right-eye shutter of the shutter glasses are opened and closed in synchronization with a point of time when the left-eye image and the right-eye image are displayed in a screen of the display apparatus.
[0069] However, if the synchronization is not achieved, the user cannot view a definite stereoscopic image. Thus, in the display apparatus 10 according to the present exemplary embodiment, the user can adjust the synchronization of the shutter glasses to match the displayed images. For example, the left-eye images and the right-eye images are alternately displayed in the order of a first left-eye image L 1 , a first right-eye image R 1 , a second left-eye image L 2 , a second right-eye image, and so forth on the main screen 200 , and are displayed in the order of the first right-eye image R 1 , the first left-eye image L 1 , the second right-eye image R 2 , the second left-eye image, and so forth on the sub screen 210 . That is, the left-eye images and the right-eye images having the reverse display orders are simultaneously displayed on the main screen 200 and the sub screen 210 , respectively.
[0070] The user may change the opening and closing order of the left-eye shutter and the right-eye shutter of the shutter glasses while viewing the main screen 200 and the sub screen 210 . In this way, the user can synchronize the shutter glasses with the images displayed in the display apparatus 10 .
[0071] FIG. 6 illustrates a configuration of a display apparatus 20 according to another exemplary embodiment. Referring to FIG. 2 , the display apparatus 20 includes a signal receiving part 100 , a High Definition Multimedia Interface (HDMI) receiving part 600 , an image processing part 110 , a display part 120 , and a controller 130 .
[0072] The HDMI receiving part 600 receives an image signal from an external device such as a Blu-ray Disk (BD) player or a DVD player. For example, the image signal provided from the external device may be a 3D image signal transmitted by the HDMI 1.4 specification. In the case that the signal receiving part 100 receives a 2D image signal and the HDMI receiving part 600 receives a 3D image signal, the display apparatus 20 may simultaneously display a 2D image and a 3D image. In this case, the 2D image may be a broadcast image.
[0073] FIG. 7 illustrates a state that images are displayed in the display apparatus 20 according to an exemplary embodiment. If the HDMI receiving part 600 receives a 3D image signal from the external device such as a BD player, the controller 130 may perform a control so that a 3D image is displayed on a main screen 200 . Furthermore, if the signal receiving part 100 receives a 2D image signal, the controller 130 may perform a control so that a 2D image is displayed on a sub screen 210 . For example, even though a broadcast signal is a 2D image signal, if a 3D image signal is received from the external device, a 2D image and a 3D image can be simultaneously displayed.
[0074] FIG. 8 is a flowchart illustrating an operational process of the display apparatus 10 according to an exemplary embodiment. Referring to FIG. 8 , if the signal receiving part 100 receives one or more image signals which includes a 3D image signal (S 600 ), the image processing part 110 processes the received image signal(s) to be displayed. In this respect, if one image signal is received, the image processing part 110 generates a plurality of image signals using the received image signal (S 610 ). The plurality of generated image signals may include a 2D image signal and a 3D image signal. Then, the controller 130 controls the image processing part 110 to display images on the basis of the plurality of image signals (S 630 ).
[0075] In this respect, for example, if the received image signal is a 2D image signal, images based on a converted 3D image signal and the 2D image signal may be displayed. Furthermore, if the received image signal is a 3D image signal, images based on a converted 2D image signal the 3D image signal may be displayed. Moreover, the 3D image may include a 3D image converted from a 2D image, a 3D image obtained by changing a display order of a left-eye image and a right-eye image, 3D images differing in depth information, or the like.
[0076] FIG. 9 is a flowchart illustrating an operational process of the display apparatus 20 according to another exemplary embodiment. Referring to FIG. 9 , if the HDMI receiving part 600 receives a 3D image signal and the signal receiving part 100 receives a 2D image signal (S 900 ), the image processing part 110 processes the received image signals to be displayed (S 910 ). Then, the controller 130 performs a control so that a 3D image is displayed in a first region of a screen and a 2D image is displayed in a second region of the screen (S 920 ). In this respect, the first region may be a main screen, and the second region may be a sub region, which may be displayed in a PIP form, a POP form, or the like.
[0077] While exemplary embodiments have been described as implemented by a display apparatus 10 or 20 , it is noted that all embodiments are not limited thereto. For example, in another exemplary embodiment, an image processing apparatus (such as a set-top box or a general or special purpose computer) may process the image signals as described above to be output and displayed on two or more regions of a separate display apparatus. Furthermore, while exemplary embodiments have been described to display image signals on a main screen and a sub screen, it is understood that all embodiments are not limited thereto. For example, in another exemplary embodiment, a display part may display the image signals in more than two screens (e.g., one main screen and two or more sub screens).
[0078] While not restricted thereto, the exemplary embodiments can also be embodied as computer-readable code on a computer-readable recording medium. The computer-readable recording medium is any data storage device that can store data that can be thereafter read by a computer system. Examples of the computer-readable recording medium include read-only memory (ROM), random-access memory (RAM), CD-ROMs, magnetic tapes, floppy disks, and optical data storage devices. The computer-readable recording medium can also be distributed over network-coupled computer systems so that the computer-readable code is stored and executed in a distributed fashion. Also, the exemplary embodiments may be written as computer programs transmitted over a computer-readable transmission medium, such as a carrier wave, and received and implemented in general-use digital computers that execute the programs. Moreover, while not required in all aspects, one or more units of the display apparatus 10 or 20 can include a processor or microprocessor executing a computer program stored in a computer-readable medium, such as a local storage.
[0079] Although a few exemplary embodiments have been shown and described, it will be appreciated by those skilled in the art that changes may be made in these exemplary embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents. | A display apparatus which can simultaneously display a plurality of images such as a two-dimensional image or a three-dimensional image, and an image display method therein, the display apparatus including: a signal receiving part which receives a first image signal; an image processing part which generates a second image signal and a third image signal based on the first image signal; a display part which displays images based on the second and third image signals; and a controller which controls the image processing part to generate the second and third image signals, to display the image based on the second image signal in a first region of the display part, and to display the image based on the third image signal in a second region of the display part, the third image signal including a left-eye image and a right-eye image generated from the first image signal. | 7 |
This application is a continuation of application Ser. No. 08/135,841, filed Oct. 7, 1993, which is a continuation of U.S. application Ser. No. 07/840,149, filed Feb. 24, 1992, now abandoned, which is a divisional of U.S. application Ser. No. 07/393,749, filed on Aug. 15, 1989, now U.S. Pat. No. 5,091,171, which is a continuation-in-part of U.S. application Ser. No. 06/945,680, filed on Dec. 23, 1986, now abandoned.
FIELD OF THE INVENTION
This invention relates generally to therapeutic treatment as well as preventive measures for cosmetic conditions and dermatologic disorders by topical administration of amphoteric compositions or polymeric forms of alpha hydroxyacids, alpha ketoacids and related compounds. We initially discovered that alpha hydroxy or keto acids and their derivatives were effective in the topical treatment of disease conditions such as dry skin, ichthyosis, eczema, palmar and plantar hyperkeratoses, dandruff, acne and warts.
We have now discovered that amphoteric compositions and polymeric forms of alpha hydroxyacids, alpha ketoacids and related compounds on topical administration are therapeutically effective for various cosmetic conditions and dermatologic disorders.
BRIEF DESCRIPTION OF THE PRIOR ART
In our prior U.S. Pat. No. 3,879,537 entitled "Treatment of Ichthyosiform Dermatoses" we described and claimed the use of certain alpha hydroxyacids, alpha ketoacids and related compounds for topical treatment of fish-scale like ichthyotic conditions in humans. In our U.S. Pat. No. 3,920,835 entitled "Treatment of Disturbed Keratinization" we described and claimed the use of these alpha hydroxyacids, alpha ketoacids and their derivatives for topical treatment of dandruff, ache, and palmar and plantar hyperkeratosis.
In our prior U.S. Pat. No. 4,105,783 entitled "Treatment of Dry Skin" we described and claimed the use of alpha hydroxyacids, alpha ketoacids and their derivatives for topical treatment of dry skin. In our recent U.S. Pat. No. 4,246,261 entitled "Additives Enhancing Topical Corticosteroid Action" we described and claimed that alpha hydroxyacids, alpha ketoacids and their derivatives, could greatly enhance the therapeutic efficacy of corticosteroids in topical treatment of psoriasis, eczema, seborrheic dermatitis and other inflammatory skin conditions.
In our more recent U.S. Pat. No. 4,363,815 entitled "Alpha Hydroxyacids, Alpha Ketoacids and Their Use in Treating Skin Conditions" we described and claimed that alpha hydroxyacids and alpha ketoacids related to or originating from amino acids, whether or not found in proteins, were effective in topical treatment of skin disorders associated with disturbed keratinization or inflammation. These skin disorders include dry skin, ichthyosis, palmar and plantar hyperkeratosis, dandruff, Darier's disease, lichen simplex chronicus, keratoses, ache, psoriasis, eczema, pruritus, warts and herpes.
In our most recent patent application Ser. No. 945,680 filed Dec. 23, 1986 and entitled "Additives Enhancing Topical Actions of Therapeutic Agents" we described and claimed that incorporation of an alpha hydroxyacid or related compound can substantially enhance therapeutic actions of cosmetic and pharmaceutical agents.
SUMMARY OF THE INVENTION
There is no doubt that alpha hydroxyacids, alpha ketoacids and related compounds are therapeutically effective for topical treatment of various cosmetic conditions and dermatologic disorders including dry skin, acne, dandruff, keratoses, age spots, wrinkles and disturbed keratinization. However, the compositions containing these acids may irritate human skin on repeated topical applications due to lower pH of the formulations. The irritation may range from a sensation of tingling, itching and burning to clinical signs of redness and peeling. Causes for such irritation may arise from the following:
Upper layers of normal skin have a pH of 4.2 to 5.6, but the compositions containing most alpha hydroxyacids or alpha ketoacids have pH values of less than 3.0. For example, a topical formulation containing 7.6% (1M) glycolic acid has a pH of 1.9, and a composition containing 9% (1M) lactic acid has the same pH of 1.9. These compositions of lower pH on repeated topical applications can cause a drastic pH decrease in the stratum corneum of human skin, and provoke disturbances in intercorneocyte bondings resulting in adverse skin reactions, especially to some individuals with sensitive skin.
Moreover, with today's state of the art it is still very difficult to formulate a lotion, cream or ointment emulsion which contains a free acid form of the alpha hydroxyacid, and which is physically stable as a commercial product for cosmetic or pharmaceutical use.
When a formulation containing an alpha hydroxyacid or alpha ketoacid is reacted equimolarly or equinormally with a metallic alkali such as sodium hydroxide or potassium hydroxide the composition becomes therapeutically ineffective. The reasons for such loss of therapeutic effects are believed to be as follows:
The intact skin of humans is a very effective barrier to many natural and synthetic substances. Cosmetic and pharmaceutical agents may be pharmacologically effective by oral or other systematic administration, but many of them are much less or totally ineffective on topical application to the skin. Topical effectiveness of a pharmaceutical agent depends on two major factors; (a) bioavailability of the active ingredient in the topical preparation and (b) percutaneous absorption, penetration and distribution of the active ingredient to the target site in the skin. For example, a topical preparation containing 5% salicylic acid is therapeutically effective as a keratolytic, but that containing 5% sodium salicylate is not an effective product. The reason for such difference is that salicylic acid is in bioavailable form and can penetrate the stratum corneum, but sodium salicylate is not in bioavailable form and cannot penetrate the stratum corneum of the skin.
In the case of alpha hydroxyacids, a topical preparation containing 5% glycolic acid is therapeutically effective for dry skin, but that containing 5% sodium glycollate is not effective. The same is true in case of 5% lactic acid versus 5% sodium lactate. The reason for such difference is that both glycolic acid and lactic acid are in bioavailable forms and can readily penetrate the stratum corneum, but sodium glycollate and sodium lactate are not in bioavailable forms and cannot penetrate the stratum corneum of the skin.
When a formulation containing an alpha hydroxyacid or alpha ketoacid is reacted equimolarly or equinormally with ammonium hydroxide or an organic base of smaller molecule the composition still shows some therapeutic effects for certain cosmetic conditions such as dry skin, but the composition has lost most of its potency for other dermatologic disorders such as wrinkles, keratoses, age spots and skin changes associated with aging.
It has now been discovered that amphoteric compositions containing alpha hydroxyacids, alpha ketoacids or related compounds, and also the compositions containing dimeric or polymeric forms of hydroxyacids overcome the aforementioned shortcomings and retain the therapeutic efficacies for cosmetic conditions and dermatologic disorders. The amphoteric composition contains in combination an amphoteric or pseudoamphoteric compound and at least one of the alpha hydroxyacids, alpha ketoacids or related compounds. Such amphoteric system has a suitable pH, and can release the active form of an alpha hydroxyacid or alpha ketoacid into the skin. The dimeric and polymeric forms of alpha, beta or other hydroxyacids in non-aqueous compositions have a more desired pH than that of the monomeric form of the hydroxyacids. The non-aqueous compositions can be formulated and induced to release the active form of hydroxyacids after the compositions have been topically applied to the skin. The cosmetic conditions and dermatologic disorders in humans and animals, in which the amphoteric compositions containing the dimeric or polymeric forms of hydroxyacids may be useful, include dry skin, dandruff, acne, keratoses, psoriasis, eczema, pruritus, age spots, lentigines, melasmas, wrinkles, warts, blemished skin, hyperpigmented skin, hyperkeratotic skin, inflammatory dermatoses, skin changes associated with aging and as skin cleansers.
DETAILED DESCRIPTION OF THE INVENTION
I. Amphoteric and Pseudoamphoteric Compositions
Amphoteric substances by definition should behave either as an acid or a base, and can be an organic or an inorganic compound. The molecule of an organic amphoteric compound should consist of at least one basic and one acidic group. The basic groups include, for example, amino, imino and guanido groups. The acidic groups include, for example, carboxylic, phosphoric and sulfonic groups. Some examples of organic amphoteric compounds are amino acids, peptides, polypeptides, proteins, creatine, aminoaldonic acids, aminouronic acids, lauryl aminopropylglycine, aminoaldaric acids, neuraminic acid, desulfated heparin, deacetylated hyaluronic acid, hyalobiuronic acid, chondrosine and deacetylated chondroitin.
Inorganic amphoteric compounds are certain metallic oxides such as aluminum oxide and zinc oxide.
Pseudoamphoteric compounds are either structurally related to true amphoteric compounds or capable of inducing the same function when they are incorporated into the compositions containing alpha hydroxyacids or ketoacids. Some examples of pseudoamphoteric compounds are creatinine, stearamidoethyl diethylamine, stearamidoethyl diethanolamine, stearamidopropyl dimethylamine, quaternary ammonium hydroxide and quaternium hydroxide.
The amphoteric composition of the instant invention contains in combination an alpha hydroxyacid or alpha ketoacid and an amphoteric or pseudoamphoteric compound. There are two advantages of utilizing an amphoteric or the like compound in the therapeutic composition containing an alpha hydroxy or ketoacid. These are (a) the overall pH of the composition is raised, so that the composition becomes less or non-irritating to the skin and (b) some alpha hydroxy or ketoacid molecules react with the amphoteric compound to form a quadruple ionic complex which acts as buffering system to control the release of alpha hydroxy or ketoacid into the skin, therefore, eliminating the skin irritation and still retaining the therapeutic efficacies.
The following are some examples. 2-Hydroxyethanoic acid (glycolic acid) 1M aqueous solution has pH 1.9. The pHs of compositions change to 3.0 and 3.2 when arginine 0.5M and creatinine 0.5M respectively are incorporated into the formulations. 2-Hydroxypropanoic acid (lactic acid) 1M aqueous solution has pH 1.9. The pHs of compositions change to 3.1 and 6.9 when arginine 0.5M and 1.0M respectively are incorporated into the formulations. 2-Methyl 2-hydroxypropanoic acid (methyllactic acid) 1M aqueous solution has pH 1.9. The pHs of compositions change to 3.3, 3.4 and 3.2 when 0.5M each of arginine, creatinine and 4-aminobutanoic acid respectively are incorporated into the formulations. 2-Hydroxybutane-1,4-dioic acid (malic acid) 1M aqueous solution has pH 1.8, but the pH of the composition changes to 3.0 when creatinine 0.5M is incorporated into the formulation.
Ideally, an amphoteric compound should contain both anionic and cationic groups or functional groups capable of behaving both as an acid and a base. Although inorganic amphoteric compounds such as aluminum oxide, aluminum hydroxide and zinc oxide may be utilized, organic amphoteric compounds have been found to be more efficient in formulating therapeutic compositions of the instant invention.
Organic amphoteric and pseudoamphoteric compounds may be classified into three groups, namely (a) amino acid type, (b) imidazoline and lecithin amphoterics and (c) pseudoamphoterics and miscellaneous amphoterics.
(a) Amino acid type amphoterics. Amphoteric compounds of amino acid type include all the amino acids, dipeptides, polypeptides, proteins and the like which contain at least one of the basic groups such as amino, imino, guanido, imidazolino and imidazolyl, and one of the acidic groups such as carboxylic, sulfonic, sulfinic and sulfate.
Glycine is a simple amphoteric compound which contains only one amino group and one carboxylic group. Lysine contains two amino groups and one carboxylic group. Aspartic acid contains one amino group and two carboxylic groups. Arginine contains one amino group, one guanido group and one carboxylic group. Histidine contains one amino group, one imidazolyl group and one carboxylic group. Taurine contains one amino group and one sulfonic group. Cysteine sulfinic acid contains one amino group, one carboxylic group and one sulfinic group. The amino group of an amphoteric compound may also be substituted, such as in betaine which is a glycine N,N,N-trimethyl inner salt.
Glycylglycine is a simple dipeptide which contains one free amino group and one free carboxylic group. Glycylhistidine is also a dipeptide which contains one free amino group, one imidazolyl group and one free carboxylic group.
The representative amphoteric compounds of amino acid type may be listed as follows: Glycine, alanine, valine, leucine, isoleucine, serine, threonine, cysteine, cystine, methionine, aspartic acid, asparagine, glutamic acid, glutamine, arginine, lysine, 5-hydroxylysine, histidine, phenylalanine, tyrosine, tryptophan, 3-hydroxyproline, 4-hydroxyproline and proline.
The related amino acids include homocysteine, homocystine, homoserine, ornithine, citrulline, creatine, 3-aminopropanoic acid, theanine, 2-aminobutanoic acid, 4-aminobutanoic acid, 2-amino-2-methylpropanoic acid, 2-methyl-3-aminopropanoic acid, 2,6-diaminopimelic acid, 2-amino-3-phenylbutanoic acid, phenylglycine, canavanine, canaline, 4-hydroxyarginine, 4-hydroxyornithine, homoarginine, 4-hydroxyhomoarginine, β-lysine, 2,4-diaminobutanoic acid, 2,3-diaminopropanoic acid, 2-methylserine, 3-phenylserine and betaine.
Sulfur-containing amino acids include taurine, cysteinesulfinic acid, methionine sulfoxide and methionine sulfone.
The halogen-containing amino acids include 3,5-diiodotyrosine, thyroxine and monoiodotyrosine. The imino type acids include pipecolic acid, 4-aminopipecolic acid and 4-methylproline.
The dipeptides include for example, glycylglycine, carnosine, anserine, ophidine, homocarnosine, β-alanyllysine, β-alanylarginine. The tripeptides include for example, glutathione, ophthalmic acid and norophthalmic acid. Short-chain polypeptides of animal, plant and bacterial origin containing up to 100 amino acid residues include bradykinin and glucagon. The preferred proteins include for example protamines, histones and other lysine and arginine rich proteins.
(b) Imidazoline and lecithin amphoterics. The amphoteric compounds of imidazoline derived type are commercially synthesized from 2-substituted-2-imidazolines obtained by reacting a fatty acid with an aminoethylethanolamine. These amphoterics include cocoamphoglycine, cocoamphopropionate, and cocoamphopropylsulfonate. The amphoteric compounds of lecithin and related type include for example, phosphatidyl ethanolamine, phosphatidyl serine and sphingomyelin.
(c) Pseudoamphoterics and miscellaneous amphoterics. Many pseudoamphoteric compounds are chemically related or derived from true amphoterics. For example, creatinine is derived from creatine. Other pseudoamphoteric compounds may include fatty amide amines such as stearamidoethyl diethylamine, stearamidoethyl diethanolamine and stearamidopropyl dimethylamine. Other pseudoamphoteric related compounds include quaternary ammonium hydroxide and quaternium hydroxide.
In accordance with the present invention, the alpha hydroxyacid, the alpha ketoacids and the related compounds which are incorporated into amphoteric or pseudoamphoteric compositions for cosmetic conditions and dermatologic disorders may be classified into three groups.
The first group is organic carboxylic acids in which one hydroxyl group is attached to the alpha carbon of the acids. The generic structure of such alpha hydroxyacids may be represented as follows:
(Ra)(Rb)C(OH)COOH
where Ra and Rb are H, F, Cl, Br, alkyl, aralkyl or aryl group of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 25 carbon atoms, and in addition Ra and Rb may carry OH, CHO, COOH and alkoxy group having 1 to 9 carbon atoms. The alpha hydroxyacids may be present as a free acid or lactone form, or in a salt form with an organic base or an inorganic alkali. The alpha hydroxyacids may exist as stereoisomers as D, L, and DL forms when Ra and Rb are not identical.
Typical alkyl, aralkyl and aryl groups for Ra and Rb include methyl, ethyl, propyl, isopropyl, butyl, pentyl, octyl, lauryl, stearyl, benzyl and phenyl, etc. The alpha hydroxyacids of the first group may be divided into (1) alkyl alpha hydroxyacids, (2) aralkyl and aryl alpha hydroxyacids, (3) polyhydroxy alpha hydroxyacids, and (4) polycarboxylic alpha hydroxyacids. The following are representative alpha hydroxyacids in each subgroup.
(1) Alkyl Alpha Hydroxyacids
1. 2-Hydroxyethanoic acid (Glycolic acid, hydroxyacetic acid) (H)(H)C(OH)COOH
2. 2-Hydroxypropanoic acid (Lactic acid) (CH 3 )(H)C(OH)COOH
3. 2-Methyl 2-hydroxypropanoic acid (Methyllactic acid) (CH 3 )(CH 3 )C(OH)COOH
4. 2-Hydroxybutanoic acid (C 2 H 5 )(H)C(OH)COOH
5. 2-Hydroxypentanoic acid (C 3 H 7 )(H)C(OH)COOH
6. 2-Hydroxyhexanoic acid (C 4 H 9 )(H)C(OH)COOH
7. 2-Hydroxyheptanoic acid (C 5 H 11 )(H)C(OH)COOH
8. 2-Hydroxyoctanoic acid (C 6 H 13 )(H)C(OH)COOH
9. 2-Hydroxynonanoic acid (C 7 H 15 )(H)C(OH)COOH
10. 2-Hydroxydecanoic acid (C 8 H 17 )(H)C(OH)COOH
11. 2-Hydroxyundecanoic acid (C 9 H 19 )(H)C(OH)COOH
12. 2-Hydroxydodecanoic acid (Alpha hydroxylauric acid) (C 10 H 21 )(H)C(OH)COOH
13. 2-Hydroxytetradecanoic acid (Alpha hydroxymyristic acid) (C 12 H 25 )(H)C(OH)COOH
14. 2-Hydroxyhexadecanoic acid (Alpha hydroxypalmitic acid) C 14 H 29 )(H)C(OH)COOH
15. 2-Hydroxyoctadecanoic acid (Alpha hydroxystearic acid) (C 16 H 34 )(H)C(OH)COOH
16. 2-Hydroxyeicosanoic acid (Alpha hydroxyarachidonic acid) (C 18 H 37 )(H)C(OH)COOH
(2) Aralkyl And Aryl Alpha Hydroxyacids
1. 2-Phenyl 2-hydroxyethanoic acid (Mandelic acid) (C 6 H 5 )(H)C(OH)COOH
2. 2,2-Diphenyl 2-hydroxyethanoic acid (Benzilic acid) (C 6 H 5 )(C 6 H 5 )C(OH)COOH
3. 3-Phenyl 2-hydroxypropanoic acid (Phenyllactic acid) (C 6 H 5 CH 2 )(H)C(OH)COOH
4. 2-Phenyl 2-methyl 2-hydroxyethanoic acid (Atrolactic acid) (C 6 H 5 )(CH 3 )C(OH)COOH
5. 2-(4'-Hydroxyphenyl) 2-hydroxyethanoic acid (4-Hydroxymandelic acid) (HO--C 6 H 4 )(H)C(OH)COOH
6. 2-(4'-Chlorophenyl) 2-hydroxyethanoic acid (4-Chloromandelic acid) (Cl--C 6 H 4 )(H)C(OH)COOH
7. 2-(3'-Hydroxy-4'-methoxyphenyl) 2-hydroxyethanoic acid (3-Hydroxy-4-methoxymandelic acid) (HO--,CH 3 O--C 6 H 3 )(H)C(OH)COOH
8. 2-(4'-Hydroxy-3'-methoxyphenyl) 2-hydroxyethanoic acid (4-Hydroxy-3-methoxymandelic acid) (HO--,CH 3 O--C 6 H 3 )(H)C(OH)COOH
9. 3-(2'-Hydroxyphenyl) 2-hydroxypropanoic acid 3-(2'-Hydroxyphenyl)lactic acid! HO--C 6 H 4 --CH 2 (H)C(OH)COOH
10. 3-(4'-Hydroxyphenyl) 2-hydroxypropanoic acid 3-(4'-Hydroxyphenyl)lactic acid! HO--C 6 H 4 --CH 2 (H)C(OH)COOH
11. 2-(3',4'-Dihydroxyphenyl) 2-hydroxyethanoic acid (3,4-Dihydroxymandelic acid) HO--,HO--C 6 H 3 (H)C(OH)COOH
(3) Polyhydroxy Alpha Hydroxyacids
1. 2,3-Dihydroxypropanoic acid (Glyceric acid) (HOCH 2 )(H)C(OH)COOH
2. 2,3,4-Trihydroxybutanoic acid (Isomers; erythronic acid, threonic acid) HOCH 2 (HO)CH 2 (H)C(OH)COOH
3. 2,3,4,5-Tetrahydroxypentanoic acid (Isomers; ribonic acid, arabinoic acid, xylonic acid, lyxonic acid) HOCH 2 (HO)CH 2 (HO)CH 2 (H)C(OH)COOH
4. 2,3,4,5,6-Pentahydroxyhexanoic acid (Isomers; allonic acid, altronic acid, gluconic acid, mannoic acid, gulonic acid, idonic acid, galactonic acid, talonic acid) HOCH 2 (HO)CH 2 (HO)CH 2 (HO)CH 2 (H)C(OH)COOH
5. 2,3,4,5,6,7-Hexahydroxyheptanoic acid (Isomers; glucoheptonic acid, galactoheptonic acid etc.) HOCH 2 (HO)CH 2 (HO)CH 2 (HO)CH 2 (HO)CH 2 (H)C(OH)COOH
(4) Polycarboxylic Alpha Hydroxyacids
1. 2-Hydroxypropane-1,3-dioic acid (Tartronic acid) HOOC(H)C(OH)COOH
2. 2-Hydroxybutane-1,4-dioic acid (Malic acid) HOOCCH 2 (H)C(OH)COOH
3. 2,3-Dihydroxybutane-1,4-dioic acid (Tartaric acid) HOOC(HO)CH(H)C(OH)COOH
4. 2-Hydroxy-2-carboxypentane-1,5-dioic acid (Citric acid) HOOCCH 2 C(OH)(COOH)CH 2 COOH
5. 2,3,4,5-Tetrahydroxyhexane-1,6-dioic acid (Isomers; saccharic acid, mucic acid etc.) HOOC(CHOH) 4 COOH
(5) Lactone Forms
The typical lactone forms are gluconolactone, galactonolactone, glucuronolactone, galacturonolactone, gulonolactone, ribonolactone, saccharic acid lactone, pantoyllactone, glucoheptonolactone, mannonolactone, and galactoheptonolactone.
The second group of compounds which may be incorporated into amphoteric or pseudoamphoteric compositions for cosmetic conditions and dermatologic disorders, is organic carboxylic acids in which the alpha carbon of the acids is in keto form. The generic structure of such alpha ketoacids may be represented as follows:
(Ra)COCOO(Rb)
wherein Ra and Rb are H, alkyl, aralkyl or aryl group of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 25 carbon atoms, and in addition Ra may carry F, Cl, Br, I, OH, CHO, COOH and alkoxy group having 1 to 9 carbon atoms. The alpha ketoacids may be present as a free acid or an ester form, or in a salt form with an organic base or an inorganic alkali. The typical alkyl, aralkyl and aryl groups for Ra and Rb include methyl, ethyl, propyl, isopropyl, butyl, pentyl, octyl, lauryl, stearyl, benzyl and phenyl, etc.
In contrast to alpha hydroxyacids the ester form of alpha ketoacids has been found to be therapeutically effective for cosmetic and dermatologic conditions and disorders. For example, while ethyl lactate has a minimal effect, ethyl pyruvate is therapeutically very effective. Although the real mechanism for such difference is not known, we have speculated that the ester form of an alpha ketoacid is chemically and/or biochemically very reactive, and a free acid form of the alpha ketoacid is released in the skin after the topical application.
The representative alpha ketoacids and their esters which may be useful in amphoteric or pseudoamphoteric compositions for cosmetic conditions and dermatologic disorders are listed below:
1. 2-Ketoethanoic acid (Glyoxylic acid) (H)COCOOH
2. Methyl 2-ketoethanoate (H)COCOOCH 3
3. 2-Ketopropanoic acid (Pyruvic acid) CH 3 COCOOH
4. Methyl 2-ketopropanoate (Methyl pyruvate) CH 3 COCOOCH 3
5. Ethyl 2-ketopropanoate (Ethyl pyruvate) CH 3 COCOOC 2 H 5
6. Propyl 2-ketopropanoate (Propyl pyruvate) CH 3 COCOOC 3 H 7
7. 2-Phenyl-2-ketoethanoic acid (Benzoylformic acid) C 6 H 5 COCOOH
8. Methyl 2-phenyl-2-ketoethanoate (Methyl benzoyl formate) C 6 H 5 COCOOCH 3
9. Ethyl 2-phenyl-2-ketoethanoate (Ethyl benzoylformate) C 6 H 5 COCOOC 2 H 5
10. 3-Phenyl-2-ketopropanoic acid (Phenylpyruvic acid) C 6 H 5 CH 2 COCOOH
11. Methyl 3-phenyl-2-ketopropanoate (Methyl phenylpyruvate) C 6 H 5 CH 2 COCOOCH 3
12. Ethyl 3-phenyl-2-ketopropanoate (Ethyl phenylpyruvate) C 6 H 5 CH 2 COCOOC 2 H 5
13. 2-Ketobutanoic acid C 2 H 5 COCOOH
14. 2-Ketopentanoic acid C 3 H 7 COCOOH
15. 2-Ketohexanoic acid C 4 H 9 COCOOH
16. 2-Ketoheptanoic acid C 5 H 11 COCOOH
17. 2-Ketooctanoic acid C 6 H 13 COCOOH
18. 2-Ketododecanoic acid C 10 H 21 COCOOH
19. Methyl 2-ketooctanoate C 6 H 13 COCOOCH 3
The third group of compounds which may be incorporated into amphoteric or pseudoamphoteric compositions for cosmetic and dermatologic conditions and disorders, is chemically related to alpha hydroxyacids or alpha ketoacids, and can be represented by their names instead of the above two generic structures. The third group of compounds include ascorbic acid, quinic acid, isocitric acid, tropic acid, trethocanic acid, 3-chlorolactic acid, cerebronic acid, citramalic acid, agaricic acid, 2-hydroxynervonic acid, aleuritic acid and pantoic acid.
II. Dimeric and Polymeric Forms of Hydroxyacids
When two or more molecules of hydroxycarboxylic acids either identical or non-identical compounds are reacted chemically to each other, dimeric or polymeric compounds will be formed. Such dimeric and polymeric compounds may be classified into three groups, namely (a) acyclic ester, (b) cyclic ester and (c) miscellaneous dimer and polymer.
(a) Acyclic ester. The acyclic ester of a hydroxycarboxylic acid may be a dimer or a polymer. The dimer is formed from two molecules of a hydroxycarboxylic acid by reacting the carboxyl group of one molecule with the hydroxy group of a second molecule. For example, glycolyl glycollate is formed from two molecules of glycolic acid by eliminating one mole of water molecule. Likewise, lactyl lactate is formed from two molecules of lactic acid. When two molecules of different hydroxycarboxylic acids are intermolecularly reacted, a different dimer is formed. For example, glycolyl lactate is formed by reacting the carboxyl group of lactic acid with the hydroxy group of glycolic acid. The polymer is formed in a similar manner but from more than two molecules of a hydroxycarboxylic acid. For example, glycoly glycoly glycollate is formed from three molecules of glycolic acid. Copolymer is formed from two or more than two different kinds of hydroxycarboxylic acids. For example, glycolyl lactyl glycollate is formed from two molecules of glycolic acid and one molecule of lactic acid.
The acyclic ester of dimeric and polymeric hydroxycarboxylic acids may be shown by the following chemical structure:
H --O--C(Ra)(Rb)--CO--!nOH
wherein Ra,Rb=H, alkyl, aralkyl ar aryl group of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 25 carbon atoms, and n=1 or any numerical number, with a preferred number of up to 200. Ra and Rb in monomer unit 2, 3, 4 and so on may be the same or the different groups from that in monomer unit 1. For example, Ra,Rb=H in monomer unit 1, and Ra=CH 3 ,Rb=H in monomer unit 2 when n=2 is a dimer called lactyl glycollate, because the first monomer is glycollate unit and the second monomer is lactic acid unit. The hydrogen atom in Ra and Rb may be substituted by a halogen atom or a radical such as a lower alkyl, aralkyl, aryl or alkoxy of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 9 carbon atoms. The dimer and polymer of a hydroxycarboxylic acid may be present as a free acid, ester or salt form with organic base or inorganic alkali.
The typical alkyl, aralkyl and aryl groups for Ra and Rb include methyl, ethyl, propyl, isopropyl, butyl, benzyl and phenyl. Representative acyclic esters of hydroxycarboxylic acids which may be useful for cosmetic conditions and dermatologic disorders are listed below:
1. Glycolyl glycollate (Glycolic acid glycollate) Ra,Rb=H in units 1 & 2, n=2
2. Lactyl lactate (Lactic acid lactate) Ra=CH 3 ,Rb=H in units 1&2, n=2
3. Mandelyl mandellate Ra=C 6 H 5 ,Rb=H in units 1 & 2, n=2
4. Atrolactyl atrolactate Ra=C 6 H 5 ,Rb=CH 3 in units 1 & 2, n=2
5. Phenyllactyl phenyllactate Ra=C 6 H 5 CH 2 , Rb=H, in units 1 & 2, n=2
6. Benzilyl benzillate Ra,Rb=C 6 H 5 in units 1 & 2, n=2
7. Glycolyl lactate Ra=CH 3 in unit 1, Ra=H in unit 2, Rb=H in units 1 & 2, n=2
8. Lactyl glycollate Ra=H in unit 1, Ra=CH 3 in unit 2, Rb=H in units 1 & 2, n=2
9. Glycolyl glycolyl glycollate Ra,Rb=H in units 1, 2 & 3, n=3
10. Lactyl lactyl lactate Ra=CH 3 , Rb=H in units 1, 2 & 3, n=3
11. Lactyl glycolyl lactate Ra=CH 3 in units 1 & 3, Ra=H in unit 2, Rb=H in units 1, 2 & 3, n=3
12. Glycolyl glycolyl glycolyl glycollate Ra,Rb=H in units 1, 2, 3 & 4, n=4
13. Lactyl lactyl lactyl lactate Ra=CH 3 , Rb=H in units 1, 2, 3 & 4, n=4
14. Glycolyl lactyl glycolyl lactyl glycollate Ra=H in units 1, 3 & 5, Ra=CH 3 in units 2 & 4, Rb=H in units 1, 2, 3, 4 & 5, n=5
15. Polyglycolic acid and polylactic acid
(b) Cyclic ester. The cyclic ester of a hydroxycarboxylic acid may also be a dimer or polymer, the most common type however, is a dimer form. The cyclic dimer may be formed from an identical monomer or different monomers. For example, glycolide is formed from two molecules of glycolic acid by removing two molecules of water, and lactide is formed from two molecules of lactic acid in the same manner. The cyclic ester of dimeric and polymeric hydroxycarboxylic acids may be shown by the following chemical structure:
--O--C(Ra)(Rb)--Co--!n
wherein Ra,Rb=H, alkyl, aralkyl or aryl group of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 25 carbon atoms, and n=1 or any numerical number, however with a preferred number of 2. Ra and Rb in units 1, 2, 3 and so on may be the same or the different groups. For example, in glycolide Ra and Rb are H in both units 1 & 2, but in lactoglycolide Ra is H in unit 1, CH 3 in unit 2 and Rb is H in both units 1 & 2. The hydrogen atom in Ra and Rb may be substituted by a halogen atom or a radical such as a lower alkyl, aralkyl, aryl or alkoxy of saturated or unsaturated, isomeric or non-isomeric, straight or branched chain or cyclic form, having 1 to 9 carbon atoms.
The typical alkyl, aralkyl and aryl groups for Ra and Rb include methyl, ethyl, propyl, isopropyl, butyl, benzyl and phenyl. Representative cyclic esters of hydroxycarboxylic acids which may be useful for cosmetic conditions and dermatologic disorders are listed below:
1. Glycolide Ra,Rb=H, n=2
2. Lactide Ra=CH 3 , Rb=H in units 1 & 2, n=2
3. Mandelide Ra=C 6 H 5 , Rb=H in units 1 & 2, n=2
4. Atrolactide Ra=C 6 H 5 , Rb=CH 3 in units 1 & 2, n=2
5. Phenyllactide Ra=C 6 H 5 CH 2 , Rb=H in units 1 & 2, n=2
6. Benzilide Ra,Rb=C 6 H 5 in units 1 & 2, n=2
7. Methyllactide Ra,Rb=CH 3 in units 1 & 2, n=2
8. Lactoglycolide Ra=H in unit 1, Ra=CH 3 in unit 2 Rb=H in units 1 & 2, n=2
9. Glycolactide Ra=CH 3 in unit 1, Ra=H in unit 2 Rb=H in units 1 & 2, n=2
(c) Miscellaneous dimer and polymer. This group includes all the dimeric and polymeric forms of hydroxycarboxylic acids, which can not be represented by any one of the above two generic structures, such as those formed from tropic acid, trethocanic acid and aleuritic acid. When a hydroxycarboxylic acid has more than one hydroxy or carboxy group in the molecule a complex polymer may be formed. Such complex polymer may consist of acyclic as well as cyclic structures.
The following hydroxycarboxylic acids have more than one hydroxy groups: glyceric acid, gluconic acid and gluconolactone, galactonic acid and galactonolactone, glucuronic acid and glucuronolactone, ribonic acid and ribonolactone, galacturonic acid and galacturonolactone, ascorbic acid, gulonic acid and gulonolactone, glucoheptonic acid and glucoheptonolactone. These polyhydroxycarboxylic acids can form complex polymers with themselves or with other simple monohydroxymonocarboxylic acids.
The following hydroxycarboxylic acids have more than one carboxyl groups: malic acid, citric acid, citramalic acid, tartronic acid, agaricic acid and isocitric acid. These monohydroxypolycarboxylic acids can also form complex polymers with themselves or with other simple hydroxycarboxylic acids.
The following hydroxycarboxylic acids have more than one hydroxy and more than one carboxyl groups: tartaric acid, mucic acid and saccharic acid. These polyhydroxypolycarboxylic acids can form even more complex polymers with themselves or with other hydroxycarboxylic acids.
III. Combination Compositions
Any cosmetic and pharmaceutical agents may be incorporated into amphoteric or pseudoamphoteric compositions, or into compositions containing dimeric or polymeric forms of hydroxyacids with or without amphoteric or pseudoamphoteric systems to enhance therapeutic effects of those cosmetic and pharmaceutical agents to improve cosmetic conditions or to alleviate the symptoms of dermatologic disorder. Cosmetic and pharmaceutical agents include those that improve or eradicate age spots, keratoses and wrinkles; analgesics; anesthetics; antiacne agents; antibacterials; antiyeast agents; antifungal agents; antiviral agents; antidandruff agents; antidermatitis agents; antipruritic agents; antiemetics; antimotion sickness agents; antiinflammatory agents; antihyperkeratolytic agents; antidryskin agents; antiperspirants; antipsoriatic agents; antiseborrheic agents; hair conditioners and hair treatment agents; antiaging and antiwrinkle agents; antiasthmatic agents and bronchodilators; sunscreen agents; antihistamine agents; skin lightening agents; depigmenting agents; vitamins; corticosteroids; tanning agents; hormones; retinoids; topical cardiovascular agents and other dermatologicals.
Some examples of cosmetic and pharmaceutical agents are clotrimazole, ketoconazole, miconazole, griseofulvin, hydroxyzine, diphenhydramine, pramoxine, lidocaine, procaine, mepivacaine, monobenzone, erythromycin, tetracycline, clindamycin, meclocycline, hydroquinone, minocycline, naproxen, ibuprofen, theophylline, cromolyn, albuterol, retinoic acid, 13-cis retinoic acid, hydrocortisone, hydrocortisone 21-acetate, hydrocortisone 17-valerate, hydrocortisone 17-butyrate, betamethasone valerate, betamethasone dipropionate, triamcinolone acetonide, fluocinonide, clobetasol propionate, benzoyl peroxide, crotamiton, propranolol, promethazine, vitamin A palmitate and vitamin E acetate.
IV. Specific Compositions For Skin Disorders
We have discovered that topical formulations or compositions containing specific alpha hydroxyacids or alpha ketoacids, or related compounds are therapeutically very effective for certain skin disorders without utilizing any amphoteric or pseudoamphoteric systems. The alpha hydroxyacids and the related compounds include 2-hydroxyethanoic acid, 2-hydroxypropanoic acid, 2-methyl 2-hydroxypropanoic acid, 2-phenyl 2-hydroxyethanoic acid, 2,2-diphenyl 2-hydroxyethanoic acid, 2-phenyl 2-methyl 2-hydroxyethanoic acid and 2-phenyl 3-hydroxypropanoic acid. The alpha ketoacids and their esters include 2-ketopropanoic acid, methyl 2-ketopropanoate and ethyl 2-ketopropanoate. The mentioned skin disorders include warts, keratoses, age spots, acne, nail infections, wrinkles and aging related skin changes.
In general, the concentration of the alpha hydroxyacid, the alpha ketoacid or the related compound used in the composition is a full strength to an intermediate strength, therefore the dispensing and the application require special handling and procedures.
If the alpha hydroxyacid, or the alpha ketoacid or the related compound at full strength (usually 95-100%) is a liquid form at room temperature such as 2-hydroxypropanoic acid, 2-ketopropanoic acid, methyl 2-ketopropanoate and ethyl 2-ketopropanoate, the liquid compound with or without a gelling agent is directly dispensed as 0.5 to 1 ml aliquots in small vials.
If the alpha hydroxyacid, or the alpha ketoacid or the related compound at full strength is a solid form at room temperature such as 2-hydroxyethanoic acid, 2-methyl 2-hydroxypropanoic acid, 2-phenyl 2-hydroxyethanoic acid, 2,2-diphenyl 2-hydroxyethanoic acid and 2-phenyl 3-hydroxypropanoic acid, the solid compound is first dissolved in a minimal amount of vehicle or vehicle system such as water, or ethanol and propylene glycol with or without a gelling agent. For example, 2-hydroxyethanoic acid 70 g is dissolved in water 30 g, and the 70% strength solution thus obtained is dispensed as 0.5 to 1 ml aliquots in small vials. If a gelling agent is used, 0.5 to 3% of for example, hydroxyethyl cellulose, methyl cellulose, hydroxypropyl cellulose or carbomer may be incorporated into the above solution.
To prepare an intermediate strength (usually 20-50%), the alpha hydroxyacid, alpha ketoacid or related compound either a liquid or solid form at room temperature is first dissolved in a vehicle or vehicle system such as water, acetone, ethanol, propylene glycol and butane 1,3-diol. For example, 2-hydroxyethanoic acid or 2-ketopropanoic acid 30 g is dissolved in ethanol 56 g and propylene glycol 14 g, and the 30% strength solution thus obtained is dispensed as 7 to 14 ml aliquots in dropper bottles.
For topical treatment of warts, keratoses, age spots, acne, nail infections, wrinkles or aging related skin changes, patients are advised to apply a small drop of the medication with a toothpick or a fine-caliber, commonly available artist's camel hair brush to affected lesions only and not surrounding skin. Prescribed applications have been 1 to 6 times daily for keratoses and ordinary warts of the hands, fingers, palms, and soles. For age spots, acne, nail infections, wrinkles and aging related skin changes topical applications have been 1 to 2 times daily.
Very often, frequency and duration of applications have been modified according to clinical responses and reactions of the lesions and the patient or responsible family member is instructed accordingly. For example, some clinical manifestations other than pain have been used as a signal to interrupt application. These manifestations include distinct blanching of the lesions or distinct peripheral erythema.
Alternatively, an office procedure may be adapted when a full strength of 2-ketopropanoic acid or 70% 2-hydroxyethanoic acid is used for topical treatment of age spots, keratoses, acne, warts or facial wrinkles.
We have found that the above mentioned alpha hydroxyacids, alpha ketoacids and related compounds are therapeutically effective for topical treatments of warts, keratoses, age spots, ache, nail infections, wrinkles and aging related skin changes.
Preparation of the Therapeutic Compositions
Amphoteric and pseudoamphoteric compositions of the instant invention may be formulated as solution, gel, lotion, cream, ointment, shampoo, spray, stick, powder or other cosmetic and pharmaceutical preparations.
To prepare an amphoteric or pseudoamphoteric composition in solution form at least one of the aforementioned amphoteric or pseudoamphoteric compounds and in combination at least one of the hydroxyacids or the related compounds are dissolved in a solution which may consist of ethanol, water, propylene glycol, acetone or other pharmaceutically acceptable vehicle. The concentration of the amphoteric or pseudoamphoteric compound may range from 0.01 to 10M, the preferred concentration ranges from 0.1 to 3M. The concentration of hydroxyacids or the related compounds may range from 0.02 to 12M, the preferred concentration ranges from 0.2 to 5M.
In the preparation of an amphoteric or pseudoamphoteric composition in lotion, cream or ointment form, at least one of the amphoteric or pseudoamphoteric compounds and one of the hydroxyacids or the related compounds are initially dissolved in a solvent such as water, ethanol and/or propylene glycol. The solution thus prepared is then mixed in a conventional manner with commonly available cream or ointment base such as hydrophilic ointment or petrolatum. The concentrations of amphoteric or pseudoamphoteric compounds and hydroxyacids used in the compositions are the same as described above.
Amphoteric and pseudoamphoteric compositions of the instant invention may also be formulated in a gel form. A typical gel composition of the instant invention utilizes at least one of the amphoteric or pseudoamphoteric compounds and one of the hydroxyacids or the related compounds are dissolved in a mixture of ethanol, water and propylene glycol in a volume ratio of 40:40:20, respectively. A gelling agent such as methyl cellulose, ethyl cellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, carbomer or ammoniated glycyrrhizinate is then added to the mixture with agitation. The preferred concentration of the gelling agent may range from 0.1 to 4 percent by weight of the total composition.
Since dimeric and polymeric forms of hydroxyacids are less stable in the presence of water or the like vehicle, cosmetic and pharmaceutical compositions should be prepared as anhydrous formulations. Typical vehicles suitable for such formulations include mineral oil, petrolatum, isopropyl myristate, isopropyl palmitate, diisopropyl adipate, occtyl palmitate, acetone, squalene, squalane, silicone oils, vegetable oils and the like. Therapeutic compositions containing dimeric or polymeric forms of hydroxyacids do not require any incorporation of an amphoteric or pseudoamphoteric compound. The concentration of the dimeric or polymeric form of a hydroxyacid used in the composition may range from 0.1 to 100%, the preferred concentration ranges from 1 to 40%. Therapeutic compositions may be formulated as anhydrous solution, lotion, ointment, spray, powder or the like.
To prepare a combination composition in a pharmaceutically acceptable vehicle, a cosmetic or pharmaceutical agent is incorporated into any one of the above composition by dissolving or mixing the agent into the formulation.
The following are illustrative examples of formulations and compositions according to this invention. Although the examples utilize only selected compounds and formulations, it should be understood that the following examples are illustrative and not limited. therefore, any of the aforementioned amphoteric or pseudoamphoteric compounds, hydroxyacids, dimeric or polymeric forms of hydroxyacids may be substituted according to the teachings of this invention in the following examples.
EXAMPLE 1
An amphoteric composition containing 1M 2-hydroxyethanoic acid and 0.5M L-arginine in solution form for dandruff or dry skin may be formulated as follows.
2-Hydroxyethanoic acid (glycolic acid) 7.6 g is dissolved in water 60 ml and propylene glycol 20 ml. L-Arginine 8.7 g is added to the solution with stirring until all the crystals are dissolved. Ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.0. An amphoteric composition formulated from 1M 2-hydroxyethanoic acid and 1M L-arginine has pH 6.3. The solution has pH 1.9 if no amphoteric compound is incorporated.
EXAMPLE 2
An amphoteric composition containing 1M 2-hydroxyethanoic acid and 0.5M L-lysine in a cream form for dry skin and other dermatologic and cosmetic conditions may be formulated as follows.
2-Hydroxyethanoic acid 7.6 g and L-lysine 7.3 g are dissolved in 30 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.3.
EXAMPLE 3
An amphoteric composition containing 1M 2-hydroxyethanoic acid and 0.5M 4-aminobutanoic acid in lotion form for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxyethanoic acid 7.6 g and 4-aminobutanoic acid 5.2 g are dissolved in water 30 ml, and the solution is mixed with 50 g of an oil-in-water emulsion. The lotion thus obtained is made up to 100 ml in volume with more oil-in-water emulsion. The amphoteric composition thus formulated has pH 3.1.
EXAMPLE 4
A pseudoamphoteric composition containing 1M 2-hydroxyethanoic acid and 0.5M creatinine in solution form for cosmetic conditions and dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 7.6 g is dissolved in water 70 ml and propylene glycol 10 ml. Creatinine 5.7 g is added to the solution with stirring until all the crystals are dissolved. More water is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 3.2. The composition has pH 4.0 when 1M instead of 0.5M creatinine is incorporated into the formulation.
EXAMPLE 5
An amphoteric composition containing 1M 2-hydroxyethanoic acid and 0.5M L-histidine in a cream form for dermatologic and cosmetic conditions may be formulated as follows.
2-Hydroxyethanoic acid 7.6 g and L-histidine 7.8 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.2.
EXAMPLE 6
An amphoteric composition containing 0.5M 2-hydroxyethanoic acid and 0.5M dipeptide of β-Ala-L-His for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and L-carnosine β-alanyl-L-histidine) 11.3 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 4.5.
EXAMPLE 7
An amphoteric composition containing 0.5M 2-hydroxyethanoic acid and 0.5M cycloleucine for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and 1-aminocyclopentane-1-carboxylic acid (cycloleucine) 6.5 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.2.
EXAMPLE 8
A pseudoamphoteric composition containing 0.5M 2-hydroxyethanoic acid and 0.25M 1,12-diaminododecane for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and 1.12-diaminododecane 5 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 9
An amphoteric composition containing 0.5M 2-hydroxyethanoic acid and 5% protamine for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and protamine 5 g, isolated and purified from salmon sperm are dissolved in water 25 ml. The solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.2.
EXAMPLE 10
An amphoteric composition containing 1M 2-hydroxypropanoic acid and 0.5M L-arginine in solution form for dandruff or dry skin may be formulated as follows.
2-Hydroxypropanoic acid (DL-lactic acid) USP grade 9.0 g is dissolved in water 60 ml and propylene glycol 20 ml. L-Arginine 8.7 g is added to the solution with stirring until all the crystals are dissolved. Ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.1. An amphoteric composition formulated from 1M 2-hydroxypropanoic acid and 1M L-arginine has pH 6.9. The solution has pH 1.9 if no amphoteric compound is incorporated.
EXAMPLE 11
An amphoteric composition containing 1M 2-hydroxypropanoic acid and 0.5M L-lysine in a cream form for dry skin and other dermatologic and cosmetic conditions may be formulated as follows.
2-Hydroxypropanoic acid 9.0 g and L-lysine 7.3 g are dissolved in 30 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.6. An amphoteric composition formulated from 1M 2-hydroxypropanoic acid and 1M L-lysine has pH 8.4
EXAMPLE 12
An amphoteric composition containing 1M 2-hydroxypropanoic acid and 0.5M 4-aminobutanoic acid in lotion form for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxypropanoic acid 9.0 g and 4-aminobutanoic acid 5.2 g are dissolved in water 30 ml, and the solution is mixed with 50 g of an oil-in-water emulsion. The lotion thus obtained is made up to 100 ml in volume with more oil-in-water emulsion. The amphoteric composition thus formulated has pH 3.0
EXAMPLE 13
A pseudoamphoteric composition containing 1M 2-hydroxypropanoic acid and 0.5M creatinine in solution form for cosmetic conditions and dermatologic disorders may be formulated as follows.
2-Hydroxypropanoic acid 9.0 g is dissolved in water 70 ml and propylene glycol 10 ml. Creatinine 5.7 g is added to the solution with stirring until all the crystals are dissolved. More water is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 3.3. The composition has pH 4.4 when 1M instead of 0.5M creatinine is incorporated into the formulation.
EXAMPLE 14
An amphoteric composition containing 1M 2-hydroxypropanoic acid and 1M L-histidine in a cream form for dermatologic and cosmetic conditions may be formulated as follows.
2-Hydroxypropanoic acid 9.0 g and L-histidine 15.5 g are dissolved in 35 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated as pH 4.9.
EXAMPLE 15
An amphoteric composition containing 1M 2-hydroxypropanoic acid and 1M dipeptide of Gly-Gly for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxypropanoic acid 9.0 g and glycylglycine 13.2 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.0.
EXAMPLE 16
An amphoteric composition containing 1M 2-methyl-2-hydroxypropanoic acid and 0.5M L-arginine in solution form for dandruff or dry skin may be formulated as follows.
2-Methyl-2-hydroxypropanoic acid (methyllactic acid) 10.4 g is dissolved in water 60 ml and propylene glycol 20 ml. L-Arginine 8.7 g is added to the solution with stirring until all the crystals are dissolved. Ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.3. An amphoteric composition formulated from 1M 2-methyl-2-hydroxypropanoic acid and 1M L-arginine has pH 6.5. The solution has pH 1.9 if no amphoteric compound is incorporated.
EXAMPLE 17
An amphoteric composition containing 1M 2-methyl-2-hydroxypropanoic acid and 0.5M 4-aminobutanoic acid in a cream form for dry skin and other dermatologic and cosmetic conditions may be formulated as follows.
2-Methyl-2-hydroxypropanoic acid 10.4 g and 4-aminobutanoic acid 5.2 g are dissolved in 30 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.2.
EXAMPLE 18
An amphoteric composition containing 1M 2-methyl-2-hydroxypropanoic acid and 1M dipeptide of Gly-Gly in lotion form for cosmetic and dermatologic conditions may be formulated as follows.
2-Methyl-2-hydroxypropanoic acid 10.4 g and glycylglycine 13.2 g are dissolved in water 30 ml, and the solution is mixed with 50 g of an oil-in-water emulsion. The lotion thus obtained is made up to 100 ml in volume with more oil-in-water emulsion. The amphoteric composition thus formulated has pH 3.0.
EXAMPLE 19
A pseudoamphoteric composition containing 1M 2-methyl-2-hydroxypropanoic acid and 0.5M creatinine in solution form for cosmetic conditions and dermatologic disorders may be formulated as follows.
2-Methyl-2-hydroxypropanoic acid 10.4 g is dissolved in water 70 ml and propylene glycol 10 ml. Creatinine 5.7 g is added to the solution with stirring until all the crystals are dissolved. More water is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 3.4. The composition has pH 4.4 when 1M instead of 0.5M creatinine is incorporated into the formulation.
EXAMPLE 20
An amphoteric composition containing 0.5M 2-phenyl-2-hydroxyethanoic acid and 0.5M L-histidine in a cream form for dermatologic and cosmetic conditions may be formulated as follows.
2-Phenyl 2-hydroxyethanoic acid (mandelic acid) 7.6 g and L-histidine 7.8 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 5.0. The composition has pH 2.2 if no amphoteric compound is incorporated.
EXAMPLE 21
An amphoteric composition containing 0.5M 2-phenyl-2-hydroxyethanoic acid and 0.5M L-lysine for cosmetic and dermatologic conditions may be formulated as follows.
2-Phenyl 2-hydroxyethanoic acid 7.6 g and L-lysine 7.3 g are dissolved in 25 ml of water. The solution thus obtained is mixed with an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated for pH 4.6.
EXAMPLE 22
A pseudoamphoteric composition containing 0.5M 2-phenyl 2-hydroxyethanoic acid and 0.5M creatinine for cosmetic and dermatologic conditions may be formulated as follows.
2-Phenyl 2-hydroxyethanoic acid 7.6 g and creatinine 5.7 g are dissolved in 30 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 4.6.
EXAMPLE 23
An amphoteric composition containing 0.5M 2-phenyl 2-hydroxyethanoic acid and 0.5M L-citrulline for cosmetic and dermatologic conditions may be formulated as follows.
2-Phenyl 2-hydroxyethanoic acid 7.6 g and L-citrulline 8.8 g are dissolved in water 30 ml, and the solution is mixed with 50 g of an oil-in-water emulsion. The lotion thus obtained is made up to 100 ml in volume with more oil-in-water emulsion. The amphoteric composition thus formulated has pH 3.0.
EXAMPLE 24
An amphoteric composition containing 1M citric acid and 1M L-arginine for cosmetic conditions and dermatologic disorders may be formulated as follows.
Citric acid 19.2 g is dissolved in water 50 ml and propylene glycol 10 ml. L-Arginine 17.4 g is added to the solution with stirring until all the crystals are dissolved. More water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.0. The composition has pH 1.8 if no amphoteric compound is incorporated.
EXAMPLE 25
A pseudoamphoteric composition containing 1M citric acid and 1M creatinine for dermatologic and cosmetic conditions may be formulated as follows.
Citric acid 19.2 g and creatinine 11.3 g are dissolved in 40 ml of water, and the solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.7.
EXAMPLE 26
An amphoteric composition containing 1M malic acid and 1M L-arginine for cosmetic and dermatologic conditions may be formulated as follows.
2-Hydroxybutanedioic acid (DL-malic acid) 13.4 g and L-arginine 17.4 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.3. The composition has pH 1.8 if no amphoteric compound is incorporated.
EXAMPLE 27
A pseudoamphoteric composition containing 1M malic acid and 0.5M creatinine for cosmetic and dermatologic conditions may be formulated as follows.
DL-Malic acid 13.4 g and creatinine 5.7 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of water is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 3.0. The composition has pH 3.8 when 1M instead of 0.5M creatinine is incorporated into the formulation.
EXAMPLE 28
An amphoteric composition containing 1M tartaric acid and 1M L-arginine for cosmetic and dermatologic conditions may be formulated as follows.
2,3-Dihydroxybutanedioic acid (DL-tartaric acid) 15.9 g and L-arginine 17.4 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.0. The composition has pH 1.7 if no amphoteric compound is incorporated.
EXAMPLE 29
A pseudoamphoteric composition containing 1M tartaric acid and 1M creatinine for cosmetic and dermatologic conditions may be formulated as follows.
DL-Tartaric acid 15.0 g and creatinine 11.3 g are dissolved in 35 ml of water. The solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 3.4.
EXAMPLE 30
An amphoteric composition containing 1M gluconolactone and 0.5M L-arginine for cosmetic and dermatologic conditions may be formulated as follows.
Gluconolactone 17.8 g and L-arginine 8.7 g are dissolved in water 60 ml and propylene glycol 10 ml. After all the crystals have been dissolved sufficient water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.1. The composition has pH 5.9 when 1M instead of 0.5M L-arginine is incorporated into the formulation. If no amphoteric compound is incorporated the pH of the composition is 1.8.
EXAMPLE 31
An amphoteric composition containing 1M gluconolactone and 0.5M 4-aminobutanoic acid for cosmetic and dermatologic conditions may be formulated as follows.
Gluconolactone 17.8 g and 4-aminobutanoic acid 5.2 g are dissolved in water 60 ml and propylene glycol 10 ml. After all the crystals ave been dissolved sufficient water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.2.
EXAMPLE 32
An amphoteric composition containing 1M gluconolactone and 1M dipeptide of Gly-Gly for cosmetic and dermatologic conditions may be formulated as follows.
Gluconolactone 17.8 g and glycylglycine 13.2 g are dissolved in water 50 ml and propylene glycol 5 ml. More water is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 3.1
EXAMPLE 33
A pseudoamphoteric composition containing 1M gluconolactone and 0.5M creatinine for cosmetic conditions and dermatologic disorders may be formulated as follows.
Gluconolactone 17.8 g and creatinine 5.7 g are dissolved in water 60 ml and propylene glycol 10 ml. More water is added to make a total volume of the solution to 100 ml. The pseudoamphoteric composition thus formulated has pH 3.2. The composition has pH 4.8 when 1M instead of 0.5M creatinine is incorporated into the formulation.
EXAMPLE 34
A pseudoamphoteric composition containing 1M pyruvic acid and 1M creatinine for dermatologic and cosmetic conditions may be formulated as follows.
2-Ketopropanoic acid (pyruvic acid) 8.8 g and creatinine 11.3 g are dissolved in water 25 ml. The solution thus obtained is mixed with sufficient amount of an oil-in-water emulsion to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 3.4.
EXAMPLE 35
An amphoteric composition containing 0.5M benzilic acid and 0.5M L-lysine for cosmetic and dermatologic conditions may be formulated as follows.
2,2-Diphenyl 2-hydroxyethanoic acid (benzilic acid) 11.4 g and L-lysine 7.3 g are dissolved in water 40 ml and propylene glycol 20 ml. After all the crystals have been dissolved sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 4.9. The composition has pH 2.7 if no amphoteric compound is incorporated.
EXAMPLE 36
An amphoteric composition containing 0.5M benzilic acid and 0.5M L-histidine for cosmetic and dermatologic conditions may be formulated as follows.
Benzilic acid 11.4 g and L-histidine 7.8 g are dissolved in water 40 ml and propylene glycol 20 ml. Ethyl cellulose 2 g is added with stirring, and sufficient amount of ethanol is added to make a total volume of the gel to 100 ml. The amphoteric gel composition thus formulated has pH 5.0.
EXAMPLE 37
A pseudoamphoteric composition containing 0.5M benzilic acid and 0.5M creatinine for cosmetic and dermatologic conditions may be formulated as follows.
Benzilic acid 11.4 g and creatinine 5.7 g are dissolved in water 40 ml and propylene glycol 20 ml. Sufficient amount of ethanol is added to make a total volume of the solution to 100 ml. The amphoteric composition thus formulated has pH 4.9.
EXAMPLE 38
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 0.05% betamethasone dipropionate in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. Betamethasone dipropionate 1% in ethanol solution 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 39
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 0.05% clobetasol propionate in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. Clobetasol propionate 1% in acetone solution 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 40
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 0.1% triamcinolone acetonide in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. Triamcinolone acetonide 2% solution of acetone:ethanol (50:50), 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 41
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 0.2% 5-fluorouracil in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g and creatinine 5.7 g are dissolved in 20 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. 5-Fluorouracil 2% solution of propylene glycol: water (95:5), 10 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 42
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxypropanoic acid and 0.05% betamethasone dipropionate in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxypropanoic acid 4.5 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of a oil-in-water emulsion. Betamethasone dipropionate 1% in ethanol solution 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 43
A pseudoamphoteric composition containing in combination 0.5M hydroxypropanoic acid and 0.05% clobetasol propionate in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxypropanoic acid 4.5 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. Clobetasol propionate 1% in acetone solution 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 44
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxypropanoic acid and 0.1% triamcinolone acetonide in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxypropanoic acid 4.5 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. Triamcinolone acetonide 2% solution of acetone:ethanol (50:50), 5 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 45
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxypropanoic acid and 0.2% 5-fluorouracil in a cream form for dermatologic disorders may be formulated as follows.
2-Hydroxypropanoic acid 4.5 g and creatinine 5.7 g are dissolved in 20 ml of water, and the solution thus obtained is mixed with 50 g of an oil-in-water emulsion. 5-Fluorouracil 2% solution of propylene glycol:water (95:5), 10 ml is added to the above mixture. More oil-in-water emulsion is added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 46
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 2% clotrimazole in a cream form for athlete's foot and other fungal infections may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g, clotimazole 2 g and creatinine 5.7 g are dissolved in water 20 ml and propylene glycol 5 ml, and the solution thus obtained is mixed with enough amount of an oil-in-water emulsion to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 47
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 2% erythromycin in solution form for acne may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g, erythromycin 2 g and creatinine 5.7 g are dissolved in water 25 ml, ethanol 40 ml and propylene glycol 15 ml. More water is then added to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 48
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 1% ketoconazole in a cream form for fungal infections may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g, ketoconazole 1 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with enough amount of an oil-in-water emulsion to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.2.
EXAMPLE 49
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxypropanoic acid and 2% clotrimazole in a cream form for fungal infections may be formulated as follows.
2-Hydroxypropanoic acid 3.8 g, clotrimazole 2 g and creatinine 5.7 g are dissolved in 25 ml of water, and the solution thus obtained is mixed with enough amount of an oil-in-water emulsion to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated has pH 4.1.
EXAMPLE 50
A pseudoamphoteric composition containing in combination 0.5M 2-hydroxyethanoic acid and 2% tetracycline in a gel form for dermatologic disorders may be formulated as follows.
2-Hydroxyethanoic acid 3.8 g, tetracycline 2 g, creatinine 5.7 g, xantham gum 0.2 g, carbomer-941 1 g, propylene glycol 5 ml, ethanol 20 ml and enough amount of water are homogenized to make a total volume of 100 ml. The pseudoamphoteric composition thus formulated for acne and oily skin has pH 4.2.
EXAMPLE 51
An amphoteric composition containing 0.2M aleuritic acid and 0.1M L-lysine in a solution form for cosmetic and dermatologic conditions may be formulated as follows.
Aleuritic acid 6.1 g and L-lysine 1.5 g are dissolved in sufficient amount of a solution from ethanol:propylene glycol 80:20 to make a total volume of 100 ml. The amphoteric composition thus formulated has pH 6.4.
EXAMPLE 52
A typical composition containing a dimeric form of alpha hydroxyacid in solution for acne, dandruff, and as a skin cleanser may be formulated as follows.
Glycolide powder 1.0 g is dissolved in ethanol 89 ml and propylene glycol 10 ml. The composition thus formulated has pH 4.0, and contains 1% active ingredient.
EXAMPLE 53
A typical composition containing a dimeric form of alpha hydroxyacid in ointment for dry skin, psoriasis, eczema, pruritus, wrinkles and other skin changes associated with aging may be formulated as follows.
Glycolide powder 2.0 g is mixed uniformly with petrolatum 66 g and mineral oil 32 g. The composition thus formulated contains 2% active ingredient.
EXAMPLE 54
A typical composition containing a full strength or a high concentration of an alpha hydroxyacid, alpha ketoacid or closely related compound for topical treatments of warts, keratoses, ache, age spots, nail infections, wrinkles and aging related skin changes may be prepared as follows.
If the alpha hydroxyacid, alpha ketoacid or closely related compound at full strength is a liquid form at room temperature such as 2-hydroxypropanoic acid, 2-ketopropanoic acid, methyl 2-ketopropanoate and ethyl 2-ketopropanoate, the compound is directly dispensed as 0.5 to 1 ml aliquots in small vials. If the compound is a solid form at room temperature such as 2-hydroxyethanoic acid and 2-methyl 2-hydroxypropanoic acid, it is first dissolved in minimal amount of an appropriate solvent or solvent system such as water or ethanol and propylene glycol with or without a gelling agent. For example, 2-hydroxyethanoic acid 70 g is dissolved in water 30 ml, and the 70% strength 2-hydroxyethanoic acid thus obtained is dispensed as 0.5 to 1 ml aliquots in small vials. If a gelling agent is used, methyl cellulose or hydroxyethyl cellulose 1 g may be added to the above solution.
EXAMPLE 55
A typical composition containing an intermediate strength of an alpha hydroxyacid, alpha ketoacid or closely related compound for topical treatment of warts, keratoses, acne, nail infections, age spots, wrinkles and aging related skin changes may be prepared as follows.
2-Hydroxyethanoic acid or 2-ketopropanoic acid 40 g is dissolved in ethanol 54 g and propylene glycol 6 g, and the 40% strength solution thus obtained is dispensed as 5 to 10 ml aliquots in dropper bottles.
TEST RESULTS
In order to determine whether amphoteric and pseudoamphoteric compositions of the instant invention were therapeutically effective for various cosmetic conditions and dermatologic disorders, a total of more than 90 volunteers and patients participated in these studies. Some participating subjects were given two preparations; an amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound, and a vehicle placebo. Others were given multiple preparations containing a known pharmaceutical agent such as a corticosteroid with or without incorporation of an amphoteric or pseudoamphoteric composition consisting of an alpha hydroxyacid or the related compound of the instant invention. The amphoteric and pseudoamphoteric compositions were formulated according to the Examples described in the previous section.
1. Common dry skin.
Human subjects having ordinary dry skin or with moderate degrees of dry skin as evidenced by dryness, flaking and cracking of the skin were instructed to apply topically the lotion, cream or ointment containing an alpha hydroxyacid or the related compound in amphoteric or pseudoamphoteric composition, on the affected area of the skin. Topical application, two to three times daily, was continued for two to four weeks.
In all the 28 subjects tested, the feeling of the skin dryness disappeared within a week of topical application. The rough and cracked skin became less pronounced and the skin appeared normal and felt smooth after several days of topical treatment. The alpha hydroxyacids and the related compounds which have been found to be therapeutically effective when incorporated into the amphoteric or pseudoamphoteric compositions for dry skin are as follows:
2-hydroxyethanoic acid (glycolic acid), 2-hydroxypropanoic acid (lactic acid), 2-methyl-2-hydroxypropanoic acid (methyllactic acid), phenyl 2-hydroxyethanoic acid (mandelic acid), phenyl 2-methyl-2-hydroxyethanoic acid (atrolactic acid), 3-phenyl-2-hydroxypropanoic acid (phenyllactic acid), diphenyl 2-hydroxyethanoic acid (benzilic acid), gluconolactone, tartaric acid, citric acid, saccharic acid, malic acid, tropic acid, glucuronic acid, galacturonic acid, gluconic acid, 3-hydroxybutanoic acid, quinic acid, ribonolactone, glucuronolactone, galactonolactone, pyruvic acid, methyl pyruvate, ethyl pyruvate, phenylpyruvic acid, benzoylformic acid and methyl benzoylformate.
The ordinary dry skin conditions, once restored to normal appearing skin, remained improved for some time until causes of dry skin, such as low humidity, cold weather, excessive contact pressure, detergents, soaps, solvents, chemicals, etc., again caused recurrence of the dry skin condition. On continued use it was also found that twice daily topical application of an amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound of the instant invention prevented the development of new dry skin lesions.
2. Severe dry skin.
In severe dry skin, the skin lesions are different from the ordinary dry skin. A main cause of severe dry skin is inherited genetic defects of the skin. The involved skin is hyperplastic, fissured and has thick adherent scales. The degree of thickening is such that lesions are palpably and visually elevated. The thickened adherent scales cause the surface of involved skin to be markedly rough and uneven. These two attributes of thickness and texture can be quantified to allow objective measurement of degree of improvement from topically applied test materials as follows:
______________________________________DEGREE OF IMPROVEMENTNone Mild Moderate Substantial Complete(0) (1+) (2+) (3+) (4+)______________________________________Thickness Highly Detectable Readily Barely Normal elevated reduction apparent elevated thickness reductionTexture Visibly Palpably Uneven but Slightly Visibly rough rough not rough uneven and palpably smooth______________________________________
By means of such parameters, degrees of change in lesions can be numerically recorded and comparisons made of one treated site to another.
In order to evaluate the amphoteric and pseudoamphoteric compositions of the instant invention, a total of 6 patients having severe dry skin conditions were treated with the compositions containing an alpha hydroxyacid or the related compound.
Tested areas were of a size convenient for topical applications, i.e., circles 5 cm in diameter demarcated with a plastic ring of that size inked on a stamp pad. The medicinal lotions or creams were topically applied by the patient in an amount sufficient to cover the treatment sites. Applications were made three times daily and without occlusive dressings. Applications were discontinued at any time when resolutions of the lesion on the treatment area was clinically judged to be complete.
The test results of amphoteric and pseudoamphoteric compositions containing the following alpha hydroxyacids or the related compounds on patients with severe dry skin are summarized as follows:
4+ Effectiveness; glycolic acid, lactic acid, methyllactic acid, mandelic acid, tropic acid, atrolactic acid and pyruvic acid.
3+ Effectiveness; benzilic acid, gluconolactone, malic acid, tartaric acid, citric acid, saccharic acid, methyl pyruvate, ethyl pyruvate, phenyllactic acid, phenylpyruvic acid, glucuronic acid and 3-hydroxybutanoic acid.
2+ Effectiveness; mucic acid, ribonolactone, 2-hydroxydodecanoic acid, quinic acid, benzoylformic acid and methyl benzoylformate.
3. Psoriasis.
The involved skin in psoriasis is hyperplastic (thickened), erythematous (red or inflamed), and has thick adherent scales. The degree of thickening is such that lesions are elevated up to 1 mm above the surface of adjacent normal skin; erythema is usually an intense red; the thickened adherent scales cause the surface of involved skin to be markedly rough and uneven. These three attributes of thickness, color and texture can be quantified to allow objective measurement of degree of improvement from topically applied test materials as follows.
______________________________________DEGREE OF IMPROVEMENTNone Mild Moderate Substantial Complete(0) (1+) (2+) (3+) (4+)______________________________________THICK- Highly Detectable Readily Barely NormalNESS elevated reduction apparent elevated thickness reductionTEXTURE Visibly Palpably Uneven Slightly Visibly rough rough but not uneven and rough palpably smoothCOLOR Intense Red Dark Pink Light Pink Normal Red Skin Color______________________________________
By means of such parameters, degree of improvement in psoriatic lesions can be numerically recorded and comparisons made of one treated site to another.
Patients having psoriasis participated in this study. Amphoteric and pseudoamphoteric compositions containing both an alpha hydroxyacid or the related compound and a corticosteroid were prepared according to the Examples. Compositions containing only a corticosteroid were also prepared and included in the comparison test. Test areas were kept to minimal size convenient for topical application, i.e., circles approximately 4 cm in diameter. The medicinal compositions were topically applied by the patient in an amount (usually about 0.1 milliliter) sufficient to cover the test site. Applications were made two to three times daily and without occlusive dressings. Test periods usually lasted for two to four weeks. The test results on patients having psoriasis are summarized on the following table.
______________________________________Topical Effects on Psoriasis ofAntipsoriatic Compositions TherapeuticCompositions* Effectiveness______________________________________Hydrocortisone 2.5% alone 1+With lactic acid 2+With glycolic acid 2+With ethyl pyruvate 2+With methyl pyruvate 2+With benzilic acid 2+With pyruvic acid 2+With methyllactic acid 2+Hydrocortisone 17-valerate 0.2% alone 2+With lactic acid 3+With glycolic acid 3+With benzilic acid 3+With ethyl pyruvate 3+With methyl pyruvate 3+With gluconolactone 3+With pyruvic acid 3+Betamethasone dipropionate 0.05% alone 3+With lactic acid 4+With glycolic acid 4+With ethyl pyruvate 4+With methyl pyruvate 4+With mandelic acid 4+With benzilic acid 4+Clobetasol propionate 0.05% alone 3+With lactic acid 4+With glycolic acid 4+With ethyl pyruvate 4+With methyl pyruvate 4+With methyllactic acid 4+With mandelic acid 4+With tropic acid 4+With benzilic acid 4+______________________________________ *Except the "alone" preparations, all others were amphoteric or pseudoamphoteric compositions containing 0.2 to 2M alpha hydroxyacids or related compounds.
We have also found that an amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound in combination with an antimetabolite agent such as 5-fluorouracil with or without additional incorporation of a corticosteroid is therapeutically effective for topical treatment of psoriasis.
4. Eczema.
In a topical treatment of eczema patients, hydrocortisone alone at 2.5% or hydrocortisone 17-valerate alone at 0.2% would achieve only 2+ improvement, and betamethasone dipropionate or clobetasol propionate alone at 0.05% would achieve only a 3+ improvement on all the eczema patients tested. Test results of amphoteric and pseudoamphoteric compositions containing both a corticosteroid and one of the following alpha hydroxyacids or the related compounds are shown as follows:
3+ Effectiveness; hydrocortisone 2.5% or hydrocortisone 17 -valerate 0.2% plus lactic acid, glycolic acid, mandelic acid, ethyl pyruvate, gluconolactone, benzilic acid or ribonolactone.
4+ Effectiveness; betamethasone dipropionate or clobetasol propionate 0.05% plus lactic acid, glycolic acid, mandelic acid, ethyl pyruvate, methyl pyruvate, benzilic acid, gluconolactone, citric acid, tartaric acid or methyllactic acid.
5. Oily Skin and Skin Cleanse.
Human subjects having oily skin or blemished skin as well as acne patients having extremely oily skin participated in this study. Amphoteric and pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds were formulated in solution or gel form.
Each participating subject received a solution or a gel preparation containing an alpha hydroxyacid or a related compound in an amphoteric or pseudoamphoteric composition. The participating subjects were instructed to apply topically the solution or gel medication on the affected areas of forehead or other part of the face. Three times daily applications were continued for 2 to 6 weeks.
The degree of improvement of oily skin as well as the rate of improvement of acne lesions were clinically evaluated. Most participants reported that oiliness of skin disappeared within one to two weeks of topical administration, and the skin so treated became smooth and soft. Many participating subjects preferred gel preparations than solution compositions. It was found that all the participants showed substantial improvements on oily skin and ache lesions by six weeks of topical administration of amphoteric or pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds of the instant invention.
Those alpha hydroxyacids and the related compounds which have been found to be therapeutically effective for oily skin and as skin cleansers include: benzilic acid, glycolic acid, lactic acid, methyllactic acid, mandelic acid, pyruvic acid, ethyl pyruvate, methyl pyruvate, tropic acid, malic acid, gluconolactone, 3-hydroxybutanoic acid, glycolide and polyglycolic acid. As a skin cleanser for oily skin or acne-prone skin, the amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound may also be incorporated with other dermatologic agents. For example, an amphoteric gel composition may consist of both an alpha hydroxyacid and erythromycin or tetracycline.
6. Acne
Amphoteric and pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds of the instant invention in a solution or gel form were provided to patients having comedongenic and/or papulopustular lesions of acne. Each participating patient was instructed to apply topically the composition on the involved areas of the skin such as forehead, face and chest. Three times daily administration was continued for 6 to 12 weeks.
The degree and rate of improvement on acne lesions were clinically evaluated. It was found that acne lesions consisting mainly of comedones improved substantially after 6 to 8 weeks of topical administration with the amphoteric or the pseudoamphoteric composition containing an alpha hydroxyacid or the related compound. The time for complete clearing of comedongenic acne treated with the amphoteric or pseudoamphoteric composition of the instant invention varied from 6 to 12 weeks.
As a topical treatment for papulopustular and/or pustular acne the amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound may incorporate in addition an antiache agent. The antiacne agents include antibiotics such as erythromycin, tetracycline, clindamycin, meclocycline and minocycline, and retinoids such as retinoic acid. Such combination compositions have been found to be therapeutically more effective for topical treatment of severe acne.
7. Age Spots
Many small and large discolored lesions, commonly called age spots on the face and the back of the hands are benign keratoses, if they are not variants of actinic keratoses. Very few of such age spots are true lentigines, therefore alpha hydroxyacids and the related compounds may be effective in eradicating most age spots without concurrent use of skin bleaching agents such as hydroquinone and monobenzone. However, additional beneficial effects have been found when a skin bleaching agent such as hydroquinone or monobenzone is also incorporated into the compositions of the instant invention for age spots involving pigmented lesions.
Amphoteric and pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds, with or without incorporation of hydroquinone were provided to volunteer subjects and patients having age spot keratoses, melasma, lentigines and/or other pigmented lesions. Each participating subject received two products, i.e., with or without the addition of 2% hydroquinone to the amphoteric or pseudoamphoteric composition containing an alpha hydroxyacid or the related compound.
The volunteer subjects and patients were instructed to apply topically one medication on one side of the body such as left side of the face or on the back of the left hand, and the other medication on the other side of the body such as on right side of the face or on the back of the right hand. Specific instructions were given to the participating subjects that the medications were applied three times daily to the lesions of age spot keratoses, melasmas, lentigines and/or other pigmented lesions. Clinical photos were taken of participating subjects before the initiation of the topical treatment and every 4 weeks during the course of treatment.
At the end of 4 to 8 weeks, improvement of age spot keratoses was clinically discernible. After 4 to 6 months of topical treatment, substantial improvement of age spot keratoses occurred in the majority of subjects tested. Complete eradication of age spot keratoses occurred after 6 to 9 months of topical administration with the amphoteric or pseudoamphoteric compositions of the instant inventions.
Amphoteric or pseudoamphoteric compositions containing both an alpha hydroxyacid or the related compound and hydroquinone were judged to be more effective in eradicating pigmented age spots, melasma, lentigines and other pigmented lesions.
The alpha hydroxyacids and the related compounds which have been found to be therapeutically effective for age spots with or without combination with hydroquinone include glycolic acid, lactic acid, methyllactic acid, mandelic acid, pyruvic acid, methyl pyruvate, ethyl pyruvate, benzilic acid, gluconolactone, malic acid, tartaric acid, citric acid and tropic acid. For flat or slightly elevated seborrheic keratoses on the face and/or the back of the body, amphoteric or pseudoamphoteric compositions containing higher concentrations of alpha hydroxyacids or the related compounds have been found to be effective in eradicating such lesions.
Actinic keratoses may be successfully treated with amphoteric or pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds in combination with an antimetabolite agent such as 5-fluorouracil.
8. Warts.
Eradications of common warts by topical application of amphoteric or pseudoamphoteric compositions require higher than usual concentrations of alpha hydroxyacids or the related compounds in the formulations. The amphoteric or pseudoamphoteric compositions were formulated as a liquid or light gel form, and dispensed usually as 0.5-1 ml aliquots in small vials.
Topical applications were made discreetly to wart lesions by adult patients or by responsible adult family members. For ordinary usual warts of hands, fingers, palms and soles topical applications were made 2 to 4 times daily, and were continued for 2 to 6 weeks. Generally, the overlying stratum corneum of the wart lesion change in appearance after several weeks topical application of the composition. In most cases, the wart lesion simply fell off. The skin then healed normally without forming any scars.
We have also found that when a dermatologic agent such as 5-fluorouracil is incorporated into the amphoteric or pseudoamphoteric compositions containing alpha hydroxyacids or the related compounds, the medications have been very effective for topical treatment of warts without using higher concentrations of alpha hydroxyacids or the related compounds.
The alpha hydroxyacids and the related compounds which have been found to be therapeutically effective for topical treatment of warts with or without incorporation of 5-fluorouracil include glycolic acid, lactic acid, pyruvic acid, ethyl pyruvate, methyl pyruvate and mandelic acid.
Topical formulations and compositions containing specific alpha hydroxyacids, alpha ketoacids or the related compounds at full strengths or high to intermediate concentrations prepared according to Examples 54 and 55, without utilizing amphoteric or pseudoamphoteric systems, have also been tested for ordinary warts of the hands, fingers, palms and soles. Participating patients have been advised to apply a small drop of the medication with a toothpick or a fine caliber brush to the center of a wart lesion only. Prescribed applications have been 3 to 6 times daily, and are continued until the patient feels pain.
For the more rough-surfaced wart, the duration of application has been as short as one or a few days. For lesions with more compact, less permeable stratum corneum, the time to experience gpain has been longer. Frequency and duration of applications have been modified according to other clinical responses and reactions of lesions, and the patient or responsible family member is instructed accordingly.
For example, some clinical manifestations other than pain have also been used as a signal to interrupt application. These manifestations have included distinct blanching of the lesions or distinct peripheral erythema. Very often, discomfort is the usual signal of clinical reactions.
Generally, the overlying stratum corneum of the wart lesions became loose, and the whole wart lesion simply fell off. The skin then healed normally without forming any scars.
9. Athlete's Foot and Nail Infections
Amphoteric and pseudoamphoteric compositions containing both an antifungal agent and one of the alpha hydroxyacids or the related compounds were provided to patients having frequent recurrence of fungal infections involving the foot. The antifungal agents include clotrimazole, miconazole, ketoconazole and griseofulvin. When both feet but not toe nails were involved in the infection, the patients were instructed to apply topically the compositions of the instant invention on the left foot, and a brand-name antifungal product on the right foot. Three times daily applications were continued for one to four weeks. The degree and rate of improvement on skin lesions were clinically evaluated, and comparison was made one side of the body against the other. It was found that the skin lesions improved much faster with the amphoteric or pseudoamphoteric compositions containing both the antifungal agent and the alpha hydroxyacid or the related compound. The alpha hydroxyacids or the related compounds seemed to enhance the efficacies of the antifungal agents, and also to eliminate the discomforts such as itching, tingling, burning and irritation due to fungal infections. When toe nails were not involved the infected skin generally healed within one to two weeks from topical application of the amphoteric or pseudoamphoteric composition containing both an antifungal agent and an alpha hydroxyacid or the related compound.
Fungal infections of the nails are very difficult to treat, because antifungal products to date are not therapeutically effective for topical treatment of nails. One of the reasons is that most antifungal drugs have not been formulated as bioavailable forms in the commercial products. When tow nails were involved in the infections, patients were provided with amphoteric or pseudoamphoteric compositions containing in combination an antifungal agent and an alpha hydroxyacid or an alpha ketoacid at higher concentrations ranging from 20 to 99%, dispensed as 1-2 ml aliquots in small vials. The patients were instructed to apply topically the compositions discreetly to the infected nail surface by means of a fine calibre paint brush. the technique was the same as for application of nail polish, that is careful avoidance of contact with lateral nail folds or any peri-ungual skin. Once or twice daily applications were continued for 2 to 8 weeks.
As mentioned above, while brand-name antifungal products are usually not effective against fungus infections within or underneath the nail, it was found that the amphoteric or pseudoamphoteric compositions containing an antifungal agent and an alpha hydroxyacid or alpha ketoacid were therapeutically effective in eradicating fungal infections of the nails. Such treatment may cause in some instances the treated nail plate to become loose and eventually fell off from the nail bed. This happened quite naturally without any feeling of pain nor bleeding, and the skin lesion healed quickly with normal growth of a new nail.
10. Wrinkles
Wrinkles of skin may be due to natural aging and/or sun damage. Most fine wrinkles on the face are due to natural or innate aging, while coarse wrinkles on the face are the consequence of actinic or sun damage. Although the real mechanism of wrinkles formation in the skin is still unknown, it has been shown that visible fine wrinkles are due to diminution in the number and diameter of elastic fibers in the papillary dermis, and also due to atrophy of dermis as well as reduction in subcutaneous adipose tissue. Histopathology and electron microscopy studies indicate that coarse wrinkles are due to excessive deposition of abnormal elastic materials in the upper dermis and thickening of the skin. At present there are no commercial products which have been found to be therapeutically effective for topical eradication of wrinkles, although retinoic acid (tretinoin) has been shown to be beneficial for sun damaged skin.
In order to determine whether the amphoteric or pseudoamphoteric composition containing the alpha hydroxyacids, alpha ketoacids or the related compounds are therapeutically effective for wrinkles, patients and volunteer subjects participated in this study. The participants were instructed to apply the formulations of the instant invention twice daily on areas of facial wrinkles for 4 to 12 months. All participants were told to avoid sun exposure, and to use sunscreen products if exposure to sunlight was unavoidable. Photographs of each side of the face for each participant were taken at the beginning of the study and repeated at one to three-month intervals. The participants were asked not to wear any facial make-up at the time of each office visit. Standardized photographic conditions were used including the use of same lot of photographic film, the same light source at two feet from the face, aimed at a locus on the frontal aspect of each cheek. Each time photographs were taken with camera aimed perpendicular to the cheek. At the end of study twenty two participants had been entered into the study for at least four months. Clinical evaluations and review of photographs have revealed substantial reductions in facial wrinkles of the temporal region and cheek area on at least one side of the face in eighteen cases. Degree of improvement and reduction in wrinkles has been evaluated and determined to be mild to moderate in six participants but very substantial in twelve participants.
The alpha hydroxyacids, alpha ketoacids and other related compounds including their lactone forms which may be incorporated into the amphoteric and pseudoamphoteric compositions for cosmetic conditions and dermatologic disorders such as dry skin, acne, age spots, keratoses, warts and skin wrinkles or in combination with other dermatologic agents to enhance therapeutic effects include the following:
(1) Alkyl Alpha Hydroxyacids
2-Hydroxyethanoic acid (Glycolic acid), 2-Hydroxypropanoic acid (Lactic acid), 2-Methyl 2-hydroxypropanoic acid (Methyllactic acid), 2-Hydroxybutanoic acid, 2-Hydroxypentanoic acid, 2-Hydroxyhexanoic acid, 2-Hydroxyheptanoic acid, 2-Hydroxyoctanoic acid, 2-Hydroxynonanoic acid, 2-Hydroxydecanoic acid, 2-Hydroxyundecanoic acid, 2-Hydroxydodecanoic acid (Alpha hydroxylauric acid), 2-Hydroxytetradecanoic acid (Alpha hydroxymyristic acid), 2-Hydroxyhexadecanoic acid (Alpha hydroxypalmitic acid), 2-Hydroxyoctadecanoic acid (Alpha hydroxystearic acid), 2-Hydroxyeicosanoic acid (Alpha hydroxyarachidonic acid).
(2) Aralkyl And Aryl Alpha Hydroxyacids
2-Phenyl 2-hydroxyethanoic acid (Mandelic acid), 2,2-Diphenyl 2-hydroxyethanoic acid (Benzilic acid), 3-Phenyl 2-hydroxypropanoic acid (Phenyllactic acid), 2-Phenyl 2-methyl 2-hydroxyethanoic acid (Atrolactic acid), 2-(4'-Hydroxyphenyl) 2-hydroxyethanoic acid, 2-(4'-Clorophenyl) 2-hydroxyethanoic acid, 2-(3'-Hydroxy-4'-methoxyphenyl) 2-hydroxyethanoic acid, 2-(4'-Hydroxy-3'-methoxyphenyl) 2-hydroxyethanoic acid, 3-(2'-Hydroxyphenyl) 2-hydroxypropanoic acid, 3-(4'-Hydroxyphenyl) 2-hydroxypropanoic acid, 2-(3',4'-Dihydroxyphenyl) 2-hydroxyethanoic acid.
(3) Polyhydroxy Alpha Hydroxyacids
2,3-Dihydroxypropanoic acid (Glyceric acid), 2,3,4-Trihydroxybutanoic acid (Isomers; erythronic acid, threonic acid), 2,3,4,5-Tetrahydroxypentanoic acid (Isomers; ribonic acid, arabinoic acid, xylonic acid, lyxonic acid), 2,3,4,5,6-Pentahydroxyhexanoic acid (Isomers; aldonic acid, altronic acid, gluconic acid, mannoic acid, gulonic acid, idonic acid, galactonic acid, talonic acid), 2,3,4,5,6,7-Hexahydroxyheptanoic acid (Isomers; glucoheptonic acid, galactoheptonic acid, etc.)
(4) Polycarboxylic Alpha Hydroxyacids
2-Hydroxypropane-1,3-dioic acid (Tartronic acid), 2-Hydroxybutane-1,4-dioic acid (Malic acid), 2,3-Dihydroxybutane-1,4-dioic acid (Tartaric acid), 2-Hydroxy-2-carboxypentane-1,5-dioic acid (Citric acid), 2,3,4,5-Tetrahydroxyhexane-1,6-dioic acid (Isomers; saccharic acid, mucic acid, etc.)
(5) Alpha Hydroxyacid Related Compounds
Ascorbic acid, quinic acid, isocitric acid, tropic acid, 3-chlorolactic acid, trethocanic acid, cerebronic acid, citramalic acid, agaricic acid, 2-hydroxynervonic acid and aleuritic acid.
(6) Alpha Ketoacids And Related Compounds
2-Ketoethanoic acid (Glyoxylic acid), Methyl 2-ketoethanoate, 2-Ketopropanoic acid (Pyruvic acid), Methyl 2-ketopropanoate (Methyl pyruvate), Ethyl, 2-ketopropanoate (Ethyl pyruvate), Propyl 2-ketopropanoate (Propyl pyruvate), 2-Phenyl-2-ketoethanoic acid (Benzoylformic acid), Methyl 2-phenyl-2-ketoethanoate (MEthyl benzoylformate), Ethyl 2-phenyl-2-ketoethanoate (Ethyl benzoylformate), 3-Phenyl-2-ketopropanoic acid (Phenylpyruvic acid), Methyl 3-phenyl-2-ketopropanoate (Ethyl phenylpyruvate), 2-Ketobutanoic acid, 2-Ketopentanoic acid, 2-Ketohexanoic acid, 2-Ketoheptanoic acid, 2-Ketooctanoic acid, 2-Ketododecanoic acid, Methyl 2-ketooctanoate
The amphoteric and pseudoamphoteric compounds which may be incorporated into the compositions of the instant invention for cosmetic and dermatologic conditions include amino acids, peptides, polypeptides, proteins and the like compounds such as creatinine and creatine.
The dimeric and polymeric forms of alpha hydroxyacids and the related compounds which may be incorporated into the compositions of the instant invention include acyclic esters and cyclic ester; for example, glycolyl glycollate, lactyl lactate, glycolide, lactide, polyglycolic acid and polylactic acid.
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 and all changes which come within the meaning and equivalency of the claims are therefore intended to be embraced therein. | Methods for improved topical delivery of lactic acid comprising forming a topically acceptable composition by admixing lactic acid and an amphoteric or pseudoamphoteric agent, and applying said topically acceptable composition to the skin. | 8 |
FIELD OF THE INVENTION
The present invention relates to an image scanner and more particularly to an image scanner using a line sensor as a light-receiving means.
BACKGROUND OF THE INVENTION
As an example of the conventional image scanner, a handy scanner 1 employing a condenser system is shown in FIG. 3. This scanner includes a lower casing 2 containing, in the order from right to left in the view, an LED 3 as light-emitting means, a condenser system 4 and a line sensor (PD) 5 as light-receiving means. Disposed close to one end of the lower casing 2 is a roller 7 as a sensor means for detecting the relative amount of movement between the reading position of the PD 5 and the image on a document 6.
The LED 3 is attached to the lower casing 2 with a holder 8 and the light emitted from the LED 3 passes through an aperture 9 formed in the lower casing 2 and is incident on the upper surface of the document 6. The reflected light from the document 6 is reflected by a mirror 10 secured to said holder 8 and guided to the condenser system 4 through a light path 11. The condenser system 4 is composed of a plurality of lenses 13 supported by a holder 12 which is rigidly secured to a first base plate 14 disposed in parallel with the lower casing 2.
The lower casing 2 is provided with a holder plate 15 making an angle of 90° therewith and a second base plate 17 and the PD 5 are fixedly secured to the holder plate 15 by means of a screw 16. The light guided through the light path 11 is focused on the PD 5, where it is converted to an electric signal by the photoelectric transducer, and the resulting signal is fed to a reader device not shown through a cable 18. Rotatably mounted on the underside of the lower casing 2 in the vicinity of PD 5 through a shaft 19 is an auxiliary roller 20.
On the other hand, a supporting shaft 21 for a sensor roller 7 is rotatably supported by a bearing 22 disposed on the lower casing 2 and a drive gear 23 is rigidly mounted in concentric relation with the roller 7. The lower casing 2 is further provided with an encoder 25 through a supporting member 24 and a driven gear 27 is concentrically mounted on a shaft 26 of the encoder 25. The driven gear 27 is driven by the drive gear 23 via the train of gears 28, 29 and 30 and as the scanner 1 is driven in pressure contact with the document 6, the encoder 25 detects the reading position.
Dismountably attached to the lower casing 2 by a screw 31 is an upper casing 32 which covers the various component parts mentioned above. Furthermore, the upper casing 32 is provided with a window 33, which can be freely opened and closed, at one end close to the LED 3. This window 33 is made of a light-transparent material so that the reading position can be ascertained from above.
In the scanner 1 having the above construction, entry of dust or other foreign matter may adversely affect its electrical system to cause a trouble or failure. Moreover, deposition of dust on the mirror 10, condenser system 4 or PD 5 would cause local darkening to interfere with proper image reading. Therefore, the lower casing 2 and the upper casing 32 are hermetically sealed together and a transparent member 34 is tightly fitted across an aperture 9 through which the reading light from the LED 3 is projected on the document 6.
However, the conventional image scanner described above has the following disadvantages. Thus, since the transparent member 34 is located close to the document 6, the entry of dust in the scanner 1 may result in deposition of the dust on the inner surface of the transparent member 34. If the deposit of dust occurs within the depth of field of the lens 13, the resulting shadow of the dust interferes with correct image reading. Moreover, since this deposit of dust occurs in a position closer to the document as compared with the deposit of dust on the other members disposed in the light path, such as the mirror 10, condenser system 4 and PD 5, it exerts a well-magnified influence.
The image scanner of the present invention has been developed to overcome the above disadvantages.
It is an object of the invention to provide an image scanner which insures accurate reading of an image without interferences of dust that may deposit on the transparent member.
Other objects and advantages of the invention will become apparent from the following description and accompanying drawings.
SUMMARY OF THE INVENTION
The present invention is, therefore, directed to an image scanner comprising a light-emitting means for projecting light on a document, a light-receiving means for receiving reflected light from said document to read an image thereon, an optical system for focusing said reflected light on said light-receiving means, a sensor means for detecting a relative amount of movement between the reading position of said light receiving means and the position of the image on said document and a housing accommodating said respective means, wherein said housing is provided with a transparent member for guiding said reflected light to said light-receiving means, said transparent member being disposed sufficiently apart from the surface of said document in such a manner that at least its area transmitting the reflected light is located outside of the depth of field.
In accordance with the invention, wherein the transparent member is located away from the depth of field, dust which may deposit on the transparent member will not cast a large shadow on the image-receiving means so that the dimming of the projected image on the light-receiving means is precluded, thus insuring correct image reading.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal section view showing the cardinal part of an image scanner embodying the principles of the invention;
FIG. 2 is an elementary view illustrating the optical system in a conventional image scanner; and
FIG. 3 is a longitudinal section view of a conventional scanner.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1 which illustrates an image scanner embodying the principles of the invention, all the parts like the corresponding parts of the prior art scanner shown in FIG. 3 are indicated by the like reference numerals and no further description is made.
This embodiment is characterized by the configuration of the transparent member 34 disposed across the aperture 9 of the lower casing 2 and the remainder of the construction is similar to that of the prior art device of FIG. 3. As illustrated in FIG. 1, the transparent member 34 is markedly curved inwardly (upwardly as illustrated) and has a first surface 34a facing the LED 3, a second surface 34b for passage of reflected light from the document 6, and a third surface 34c contiguous to the two surfaces 34a, 34b. Both ends, 34d and 34e, of the transparent member 34 are held in close contact with the lower casing 2, with the end 34e being continual to the second surface 34b through a fourth surface 34f. The third surface 34c and the fourth surface 34f each makes an angle of about 80 degrees with the bottom surface of the lower casing 2, while the second surface 34b is far displaced from the bottom surface (the surface of document 6) out of the depth of field of a lens system 13.
The effects of this embodiment are now explained with reference to FIG. 2.
The optical system of the conventional scanner 1 is illustrated in FIG. 2. In the view, the reading light from the LED 3 passes through a surface 34a of said transparent member 34 which is substantially normal to the axis of incidence and is projected on the document 6 and the reflected light from the document 6 passes through surfaces 34b, 34b' of the transparent member 34 and is incident on the mirror 10. The reflected light from the mirror 10 passes along the light path 11 and is focused by the condenser system 4 on the PD 5.
The positions liable to pickup dust in the above optical system are the inner surface 34b' and outer surface 34b of the transparent member 34, the mirror 10, the lenses 13a, 13b of the condenser system 4, and the PD 5. The size corresponding to one picture element at the PD 5 in each of said various members may for example be as follows.
______________________________________Position Size per picture element (mm)______________________________________Transparent member 34b' 0.283Transparent member 34b 0.245Mirror 10 1.07Lenses 13a, 13b 3.98-2.62Line sensor (PD) 5 0.557______________________________________
It will be apparent from the above table that the size corresponding to one sensor picture element is smallest for the transparent member 34. Therefore, dust deposited on the surface of the transparent member 34 is imaged large on the PD 5. This is because the transparent member is located close to the document (within the depth of field).
However, in the above embodiment of the invention wherein the second surface 34b of the transparent member 34 for passage of reflected light is located far away (distance L) from the document (outside of the depth of field of the lens 13), the size corresponding to one sensor picture element on this surface is very large. As a result, the dust deposited on the surface will not form a large shadow on the PD 5 so that dimming of the image on the PD 5 is prevented and, hence, accurate image reading is insured.
In accordance with this embodiment, dust control in the production and assembly process can be less exacting and the cost of production be as much decreased. Moreover, since the image output has no streaks due to dust, an attractive image can be insured. Furthermore, since there is no remarkable influence of dust on image density data, shading correction can be properly carried out and an image true to the original can be reproduced. In addition, the convenience in use is improved because the surface of the transparent member facing the document need not be wiped clean after each scanning.
The constructions of the respective component parts of the above embodiment are not limited to those described but may be different constructions within the scope of the invention which is only defined by the appended claim.
It should also be understood that while the present invention has been described with reference to the handy scanner 1, the same result can be obtained by applying the invention to other kinds of image scanners. | An image scanner for a document incorporates a transparent member on a lower surface for passing reading and reflecting light while preventing entry of dust and foreign matter into the scanner housing. The transparent member is disposed so that at least the area which passes reflected light is located outside of the depth of field of the scanner optical system. | 7 |
CLAIM OF PRIORITY
This application claims priority to U.S. Provisional Application No. 60/573,204 entitled “Independent Portlet Rendering” filed May 21, 2004.
FIELD OF THE INVENTION
The present invention is directed to portal technology.
BACKGROUND
Portals can provide access to information networks and/or sets of services through the World Wide Web and other computer networks. Portals can provide a single point of access to data and applications, making them valuable to developers, businesses, and consumers alike. A portal can present a unified and personalized view of enterprise information to employees, customers, and business partners. In many implementations, portal applications can include web application views designed as a portal.
Portals are capable of presenting multiple web application views within a single web interface. In addition to regular web content that can appear in a portal, portals provide the ability to display portlets (self-contained applications or content) in a single web interface. Portals can also support multiple pages with menu-based or custom navigation for accessing the individualized content and portlets for each page.
A working portal can be defined by a portal configuration. The portal configuration can include a portal definition such as a file including Extensible Markup Language (XML); portlet definition files for any portlets associated with the portal; java server pages (JSPs); web application descriptors; images such as graphics interchange format files (GIFs); deployment descriptors, configuration files, the java archive (JAR) files that contain the logic and formatting instructions for the portal application; and any other files necessary for the desired portal application.
BRIEF DESCRIPTION OF THE FIGURES
FIGS. 1A-1C are diagrams that illustrate the display of a portal page of one embodiment of the present invention.
FIG. 2 illustrates a system of one embodiment of the present invention.
FIG. 3 is a flowchart of a method of the present invention.
FIG. 4 illustrates interactions of a server and a browser client of one embodiment of the present invention.
FIG. 5 is a flowchart of a method of the present invention.
DETAILED DESCRIPTION
Portals can provide access to information networks and/or sets of services through the World Wide Web (WWW) or other computer networks. These networks can range from broad interconnections of computing systems such as the Internet to localized area networks including a few computers located in close geographic proximity such as a home or office. Portal applications can include web application views designed as a portal.
Portlets can be implemented as java server pages (JSPs) referenced by XML-based metadata of the portal descriptor. Portlets can utilize various types of display code to display highly focused information directed to a specific user or user group, having a portal as its container. Portlets can be comprised of portlet components which include portlet attributes (i.e. whether the portlet is editable, floatable, minimizable, maximizable, helpable, mandatory, has defaults minimized, or whether login is required) and portlet layout elements or components (i.e. banner, header, content, and footer sections). In one embodiment, a portlet is defined by a file that contains a portlet's XML-based metadata, which is created and edited by an integrated design environment or administration tool. Portlets can also be associated with portlet resource files including skeleton JSPs (one for each portlet layout element) and image files saved to a local file system by portal designer of integrated design environment.
In one embodiment, the portlets can be rendered in their own threads. A “forkable” portlet is one whose execution takes place on the thread that is separate from the main servlet thread (This thread can allocated from a separate thread pool and can be configured in the config.xml file). This can increase the efficiency as the total time to execute the page is no longer the sum of all portlet execution times but is now limiting by the longest running portlet. However, all portlets on a portal page must finish execution before the page can be rendered as a single Hypertext Markup Language (HTML) document. Therefore, the slowest portlet, and more generally the slowest-executing portion of a portal page still act as the governing entity with regard to actual portal response time. That is to say, the “longest link” in the processing chain can still have a significant effect on portal response time.
The present invention concerns ways to speed up the presentation of a portal page to a user. One embodiment of the present invention concerns providing a portal page display with only the fast rendering portlets at first and then later providing the slow rendering portlet information to update the display. This can enhance the user experience since the display does not wait for slow rendering but potentially inessential portlets.
Another embodiment concerns the use of a timeout property for portlets. If the portlet rendering exceeds the timeout period, the rendering of the portlet can stop. An error message can be displayed to the user.
FIGS. 1A-1C are diagrams that illustrate one embodiment of the present invention. In one embodiment, a portal page is constructed using portlets. As shown in FIG. 1A , the display 102 of the portal page does not wait for at least one slow rendering portlet but at least one fast rendering portlet 104 is displayed to the user before the at least one slow rendering portlet. As shown in FIG. 1B , the display can be updated with the at least one slow rendering portlet 108 after it renders.
Looking again at FIG. 1A , temporary content 110 can be displayed for a slow rendering portlet. A fast content (temporary content) Uniform Resource Indicator (URI) can be used to obtain the temporary content 110 if the portlet is slow to render. The portlets can have a ‘fast content URI’ property to indicate the URI of the temporary content. ‘Fast content URI’ is an optional URI that the system can render if the portlet is in ‘render independently’ mode. The fast content could display a simple message like “retrieving flight information.” while the system is working on the real portlet content, and upon completion would replace the ‘fast content’ in the portal.
The independent rendering functions of the portlets can be activated or inactivated based on stored information for each portlet. This allows essential portlets to always be rendered with the first display of the portal page.
A ‘supports rendering independently’ property of the portlet marks the portlet as supporting this feature. This property can be set in the IDE as it is determined by the developer. The developer can decide if the portlet will not be adversely affected if the portlets rendering phase is out of sync with other portlets. A case where a portlet's functionality could be affected is were the developer inserts request or session attributes during the render phase and other portlets are relying on these attributes.
‘A render independently’ property of the portlet can actually turn on the independent rendering function for the portlet. The portal framework would not wait for the portlet to finish rendering before sending its HTML to the browser. When the portlet completes the rendering phase, the portlet's contents can get injected into the main page.
In one embodiment, the portlet execution can be timed out if the portlet rendering exceeds a predetermined period of time. FIG. 1C shows an error message 112 that is displayed to the user after a portlet times out. In this case, an error message 112 can replace the temporary content 114 . A ‘timeout’ attribute of the portlet can inform the framework to kill the processing of the portlet if the execution of the portlet exceeds that of the timeout value. This can insure that one portlet cannot bring down the entire portal. Upon a portlet timeout, an error message can be displayed in the portlet's content indicating a timeout has occurred and the user may wish to try again.
The server 202 can be used to produce the portal for display at the browser client 204 . In one embodiment, the server 202 produces portal display information in response to a request from the browser client 204 . The portal can be configured for different users and different group of users, where different portlets can be displayed based upon a user's group or role. The server 202 can use a portlet configuration 210 . The portlet configurations including a portal definition 212 which can be an XML file pointing to portal elements 214 . In one embodiment, the portal elements can include a portlet definition 216 . The properties of the portlet can include the “support rendering independently”, “fast content URI” and “timeout”. These properties can be stored in the portlet definition. The portal elements 214 can also include other portals elements 218 , such as images, look and feel elements JSPs and the like. The server 202 can use the properties stored in the portlet definition to determine the information provided to the browser client 204 . The server 202 can be software that can be run on one or more server machines. In one embodiment, the server 202 is the WebLogic Server™ available BEA Systems Inc., of San Jose, Calif.
The browser client 204 can produce a display 220 of the portal pages and other information from the Internet. In one embodiment, the Document Object Model (DOM) standard is supported by the client as well as the current browser client supporting javascript. The DOM/javascript 224 can be used for updating the portal page displays with the information provided by the server as discussed below.
A portal product 230 can be Integrated Designed Environment (IDE) for producing the portal. In one embodiment, the IDE includes a portal designer 232 for the design of the portal, portlets and other portal elements. The administration tools 234 and visitor tools 236 are used for producing versions of the portal. In one embodiment, different version use the portal configuration 210 and stores it in a database where changes to the portal configuration can be done. Portals can be produced from the database or directly from the portal configuration.
FIG. 3 illustrates a flow chart of one embodiment in the present invention. In step 302 , the rendering of the portlets or the portal page has begun. If the “support rendering independently” property is not set, as determined in step 304 , or the “rendering independently property” is not set as determined in step 306 , then, in step 308 , the portlet is rendered without independent portlet rendering.
If a portet is ready to render in step 310 , then the independent display of the portlet can be done in step 312 . If not, if there is a fast URI as determined in step 314 , independent display of the fast URI content can be can be done in step 316 . If the portlet times out as determined in step 318 , an independently displayed error message can be produced in step 320 . Steps 304 - 320 can be done independently for each portlet, each portlet in its own thread.
FIG. 4 illustrates the operation of one embodiment of the present invention. The browser client 402 sends a request, in step A, for a portal page to the server 404 . In step B, the server begins rendering the portlets for the portal page. In step C, the preparation of the fast rendering portlets is finished. In one embodiment, the fast rendering portlets are determined after certain period of time or after certain number of portlets are finished. In step D, an HTML connection with the browser client is opened. HTML for the fast running portlets is set along with temporary messages for and associated IDs for the slow rendering portlets to the browser/client 402 . In step E, browser client 402 can display the portlet page. This can correspond to the display of FIG. 1A . In step F, the preparing of a slow rendering portlet is finished and an HTML for a slow rendering portlet along with the ID of the portlet is set to the browser/client 402 , in step G. In step H, javascript can be used to update the display of the portal rendering page with the slow rendering portlet. This can correspond with the display of FIG. 1B .
In step I, a portlet times out. In step J an error message can be sent for a timed out portlet along with the portlet ID. In step K, the browser/client 402 use javascript to update the display of the portlet page with error message. This can correspond with the display of FIG. 1C . In step L, the HTML connection can be closed.
Delayed rendering can use ordinary HTTP request response type mechanisms to achieve its goal. A portlet that is delayed will not output its content into the HPPT response but instead can output a div tag with a special id/name. This marks a place in the DOM were javascript at the browser can update the contents at a later time. The HPPT response is held open unitl the delayed portlets are finished or timeout. This gives the illusion that the portlet's content is being pushed to the browser.
The response is not held open any longer than if we did not do delayed rendering. In one embodiment, the benefit comes with the HTML filing the screen a lot faster with portlest that have already finished their execution.
In one embodiment, a timeout property of a portlet is checked. If the timeout property value is exceeded by the rendering time of the portlet, the rendering of the portlet is ended. This can be done as part of the delayed rendering system of FIG. 3 as discussed above.
FIG. 5 shows an alternate embodiment where the display waits until all portlets render or the timeout property value is exceeded for all portlets. In step 502 , rendering begins. After step 504 determines that all of the portlets are either ready to displayed or timeout, the display of the whole page with any error messages for timed out potlets is done in step 506 .
One embodiment may be implemented using a conventional general purpose or a specialized digital computer or microprocessor(s) programmed according to the teachings of the present disclosure, as will be apparent to those skilled in the computer art. Appropriate software coding can readily be prepared by skilled programmers based on the teachings of the present disclosure, as will be apparent to those skilled in the software art. The invention may also be implemented by the preparation of integrated circuits or by interconnecting an appropriate network of conventional component circuits, as will be readily apparent to those skilled in the art.
One embodiment includes a computer program product which is a storage medium (media) having instructions stored thereon/in which can be used to program a computer to perform any of the features presented herein. The storage medium can include, but is not limited to, any type of disk including floppy disks, optical discs, DVD, CD-ROMs, micro drive, and magneto-optical disks, ROMs, Rams, EPROM's, EPROM's, Drams, Rams, flash memory devices, magnetic or optical cards, Nan systems (including molecular memory ICs), or any type of media or device suitable for storing instructions and/or data.
Stored on any one of the computer readable medium (media), the present invention includes software for controlling both the hardware of the general purpose/specialized computer or microprocessor, and for enabling the computer or microprocessor to interact with a human user or other mechanism utilizing the results of the present invention. Such software may include, but is not limited to, device drivers, operating systems, execution environments/containers, and user applications.
The foregoing description of preferred embodiments of the present invention has been provided for the purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise forms disclosed. Many modifications and variations will be apparent to one of ordinary skill in the relevant arts. For example, steps performed in the embodiments of the invention disclosed can be performed in alternate orders, certain steps can be omitted, and additional steps can be added. The embodiments were chosen and described in order to best explain the principles of the invention and its practical application, thereby enabling others skilled in the art to understand the invention for various embodiments and with various modifications that are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents. | The rendering of portal pages on can be sped up by allowing individual portlets to be displayed while other portlets of the page are still waiting to finish rendering. Temporary messages can be displayed for the portlets that are still rendering. This temporary content can be replaced by the finished portal rendering for the slow rendering portlets. Additionally, a timeout feature for the portlets can be used. The timeout feature allows the rendering of the portlet to be stopped after a certain period of time. | 6 |
BACKGROUND OF THE INVENTION
The present invention relates to the field of organic chemistry and more specifically to the preparation of methyl N-methylanthranilate.
At least two processes for the preparation of the subject compound are known in the prior art. In one such process anthranilic acid is used as the starting compound and reacted with formaldehyde and hydrogen as described in J. Soc. Org. Synthetic Chem. (Japan) 11,434 (1953), Chem. Abst. 49, 955a (1955), to produce N-methylanthranilic acid. This resulting intermediate is thereafter reacted with thionyl chloride and methanol to produce the desired methyl N-methylanthranilate. This step is described in Aust. J. Chem. 27, 537 (1974). The disadvantages of this process lie in the use of a relatively expensive starting material and the relatively poor yields of final product. Typical reported reaction yields based on the starting compound amount to about 36% overall for the two steps.
In another prior art process, described in J. Org. Chem. 24,1214 (1959), the starting compound is N-methylisatoic anhydride, again a costly starting material which is more expensive than anthranilic acid.
Methyl N-methylanthranilate has found use in the preparation of artificial food flavorings. The compound has been disclosed to be offensive to birds and has "very excellent repellent action for prolonged periods in very small concentrations" according to U.S. Pat. No. 2,967,128 which issued on Jan. 3, 1961.
It is an object of this invention to provide a process for the preparation of methyl N-methylanthranilate which is feasible towards producing the compound in commercial quantities, in high purity and good yield.
SUMMARY OF THE INVENTION
The present application discloses a process for the preparation of methyl N-methylanthranilate (DMA) comprising the use as starting material of methyl anthranilate. In accordance with the invention, the process involves forming a mixture of methyl anthranilate dissolved in a water-miscible solvent such as, for example, isopropanol or methanol, with an aqueous or alcoholic solution of formaldehyde. The resulting honogeneous mixture (solution) is reduced in a hydrogen atmosphere in the presence of a hydrogenation catalyst at moderate temperatures and pressures. The resultant product is recovered from the reaction mixture by fractional vacuum distillation.
The process may be illustrated by the following equation: ##STR1##
The reductive methylation produces water as a by-product. The feature of the process lies in the reductive methylation of the amino group in the presence of what is normally considered to be a water-sensitive hydrolyzable ester group which unexpectedly survives the methylation conditions.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preparation of the methyl N-methylanthranilate in accordance with the invention is carried out employing a process involving reactive methylation.
The preparation is started by first providing a mixture of methyl anthranilate and formaldehyde in a suitable pressure reactor, i.e. a vessel which is able to withstand superatmospheric pressures. To provide a fluid medium for reaction, the methyl anthranilate is generally dissolved in water-miscible solvent such as a lower alkanol. Suitable water-miscible solvents include alkanols, cyclic and acyclic ethers and mixtures thereof. Typical useful solvents include methanol, isopropanol and p-dioxane. Isopropanol and methanol are preferred solvents with isopropanol being most preferred. Use of methanol leads to a twophase system during the recovery of the product while use of isopropanol maintains a one-phase system. The proportion of starting compound to solvent is not critical and can vary over a wide range, but a preferable proportion is from about 1:1 to 1:8, and most preferable is from about 1:2 to 1:4.
The formaldehyde needed in the reaction mixture is used as an aqueous or alcoholic solution. Most conveniently, it is used as a 37% aqueous solution or 55% methanolic solution, both as commercially supplied. The methyl anthranilate and formaldehyde are used on a mole to mole ratio but a slight excess (up to about 10 mole percent) of either reactant is permissible. An equimolar ratio is preferred.
The catalyst useful in carrying out the reducing reaction is not critical and may be any of the common hydrogenation catalysts known in the art. Most useful, however, are Raney nickel and noble metal catalysts such as palladium on charcoal. As is known, palladium on charcoal permits the hydrogenation to proceed at lower operating pressures than Raney nickel. The catalyst is added to the reaction mixture in amounts known in the art of hydrogenation. Ordinarily, the amounts used in the present reaction will range from about 1 to 10% by weight based on the participating reactants.
In carrying out a reaction according to the present invention, the reaction vessel head space and the reaction mixture of methyl anthranilate, formaldehyde and catalyst are purged with hydrogen to be free of air, and the mixture is gently heated to about 30° to 40° C. The system is pressurized with additional hydrogen to a pressure of about 150 to 1,000 pounds per square inch (psi). Typical operating pressures will be in the range of 150 to 750 psi depending on the desired reaction rates and the specific catalyst employed. Moderate heating is continued to reach an operating temperature of about 35° to 75° C. Preferred temperatures will be in the range of about 35°-55° C. The reaction is allowed to proceed with periodic repressurization as necesssary until no further decrease in hydrogen pressure (due to reaction) is observed, usually a period of from about 2-12 hours, preferably about 2-8 hours.
When the reaction is completed, the vessel is cooled to room temperature and the reaction mixture is filtered to remove the catalyst. The bulk of the solvent is removed by vacuum distillation, usually at pressures of about 100-300 mm Hg. and temperatures of 25°-90° C.
Depending on the solvent used in the reaction mixture, phase separation may or may not occur. Where phase separation occurs, the aqueous (non-product) phase is decanted. The remaining phase contains the product and is subjected to vacuum distillation to recover the product as a colorless liquid having a boiling point in the range of 138°-143° C. at 21 mm Hg. or 104°-108° C. at 0.5 mm Hg. As is known, the boiling point range is dependent on the specific vacuum applied to the system.
Where phase separation does not occur after stripping, the product is further purified by direct vacuum distillation.
This invention is further illustrated in connection with the following examples. In these examples, all parts are given by weight unless otherwise noted.
EXAMPLE I
Preparation of Methyl N-Methylanthranilate
A two liter high pressure reactor equipped with a mechancial stirrer is charged with the following:
a. Methyl anthranilate--226.8 grams (1.50 moles)
b. Methanol--1270. ml
c. Aqueous formaldehyde (37%)--121.6 grams (1.50 moles)
d. Raney nickel (W-2 grade)--13.2 grams
The mixture is stirred to achieve a homogeneous slurry. The slurry and head space are purged free of air using hydrogen, and the system is heated to 36° C. The system is then pressurized to about 600 psi and allowed to consume hydrogen while gradual heating is applied. The hydrogenation is allowed to proceed in the 36°-72° C. range with repressurization to 700 psi until no further hydrogen is consumed in the reaction, about 2 hours. The reactor is cooled to room temperature and the catalyst is removed by filtration. The bulk of the solvent is stripped off while raising the temperature to 90° C. at 40 mm Hg. vacuum resulting in a layering of the product.
The two-phase system is treated with 600 ml of toluene and 300 ml of water with mechanical agitation at room temperature. The aqueous phase is decanted and the toluene layer vacuum distilled using a six-inch Vigereaux column collecting the fraction boiling at 138°-143° C. at 21 mm Hg. The yield is 171 grams of 98.7% pure methyl N-methylanthranilate which calculates to be 69% of theory.
EXAMPLE II
The procedure of Example I was repeated substantially as described with slight variations as noted to obtain seven additional preparations of the subject compound.
______________________________________ Dis- Sol- Reaction tilledBatch No. vent Formaldehyde Period Yield Purity______________________________________4707- MeOH Aqueous (37%) 5.0 hours 69.0% 97.1%64BB4707-79B MeOH Aqueous (37%) 4.0 hours 86.6% 93.8%4707-82 i-PrOH Aqueous (37%) 3.5 hours 97.0%* 88.7%4707-133 i-PrOH Alcoholic (55%) 3.0 hours 92.0% 92.0%4707-86B i-PrOH Aqueous (37%)** <8.0 91.6% -- hours4707-89B i-PrOH Aqueous (37%)** 5.0 hours 74.5% --4707-91B MeOH Aqueous (37%)** <8.0 91.4% 94.3% hours______________________________________ *undistilled **10 mole percent excess
EXAMPLE III
In a manner similar to the procedure of Example I, a preparation of the subject compound was made employing palladium on charcoal (5% by weight based on reactants) as the hydrogenation catalyst. Alcoholic formaldehyde was used. The system was pressurized to about 150 psi and the reaction was allowed to proceed in a temperature range of 38°-50° C. The reaction was terminated prior to completion resulting in a yield of methyl N-methylanthranilate of 13% of theory.
In summary the invention provides a process for the preparation of methyl N-methylanthranilate employing methyl anthranilate as the starting material, which process yields the compound in high purity and good yield.
Now that the preferred embodiments of the present invention have been described in detail, various modifications and improvements thereon will become readily apparent to those skilled in the art. Accordingly, the spirit and scope of the invention are to be limited only by the following claims and not by the foregoing specification. | A mixture of methyl anthranilate, dissolved in a water-miscible solvent, with a solution of formaldehyde is reduced in a hydrogen atmosphere in the presence of a hyrogenation catalyst at moderate temperatures and pressures to yield methyl N-methylanthranilate. The invention provides a process which is feasible towards producing the compound in commercial quantities in high purity and good yield. | 2 |
[0001] The present application claims priority to Chinese Patent Application No. 201110193333.7, filed with the State Intellectual Property Office of PRC on Jul. 11, 2011 and entitled “Data communication method and apparatus in carrier aggregation system”, the contents of which are hereby incorporated by reference in their entirety.
FIELD
[0002] The present invention relates to the field of communications and particularly to a data communication method and apparatus in a carrier aggregation system.
BACKGROUND
[0003] Inter-band carrier aggregation is performed in a Release 11 (Rel-11) Long Term Evolution (LTE) system, and in order to avoid interference with an adjacent carrier Time Division Duplex (TDD) system in a different band, an LTE cell in the different band may perform Carrier Aggregation (CA) using a different TDD uplink and downlink sub-frame configuration. For a TDD CA User Equipment (UE) with a low capability, its simultaneous uplink and downlink operation over different carriers, for example, simultaneous reception of downlink data over a Component Carrier (CC) 1 and transmission of uplink data over a CC 2 in the same sub-frame, can not be supported.
[0004] The technology of carrier aggregation will be introduced below.
[0005] In wireless communication systems of the LTE and earlier, there is only one carrier in a cell, and there is a maximum bandwidth of 20 MHz in the LTE system, as illustrated in FIG. 1 .
[0006] In a Long Term Evolution-Advanced (LTE-A) system, there are required peak rates of the system up to downlink 1 Gbps and uplink 500 Mbps significantly improved over the LTE system. The required peak rates can not be achieved by only a carrier with a maximum bandwidth of 20 MHz. Thus the LTE-A system has to extend the bandwidth available to the user equipment, and in view of this, the technology of carrier aggregation has been introduced where a plurality of consecutive or inconsecutive carriers under the same evolved NodeB (eNB) are aggregated together to serve the UE simultaneously and provide the required rates. These aggregated carries are also referred to as component carriers. Each cell may be a component carrier, and cells (member carriers) under different eNBs can not be aggregated. In order to ensure the UE of the LTE to be capable of operating over each aggregated carrier, the maximum bandwidth of each carrier is no more than 20 MHz. The CA technology of the LTE-A is as illustrated in FIG. 2 where there are four carriers that can be aggregated under an LTE-A eNB, and the eNB can communicate data with the UE simultaneously over the four carriers to improve the throughout of the system.
[0007] In the LTE system, there is a radio frame of 10 ms and a sub-frame of 1 ms in both FDD and TDD schemes. For each TDD radio frame, seven TDD uplink and downlink sub-frame configurations are defined as depicted in Table 1:
[0000]
TABLE 1
Uplink and downlink
sub-frame
Sub-frame number
configuration
0
1
2
3
4
5
6
7
8
9
0
D
S
U
U
U
D
S
U
U
U
1
D
S
U
U
D
D
S
U
U
D
2
D
S
U
D
D
D
S
U
D
D
3
D
S
U
U
U
D
D
D
D
D
4
D
S
U
U
D
D
D
D
D
D
5
D
S
U
D
D
D
D
D
D
D
6
D
S
U
U
U
D
S
U
U
D
[0008] Where D represents a downlink (DL) sub-frame, U represents an uplink (UL) sub-frame, and S represents a special sub-frame of the TDD system, for example, the sub-frames are configured as DSUUDDSUUD in the case of the configuration 1.
[0009] For the LTE TDD system, the UE may feed back, in an uplink sub-frame, acknowledgement (ACK) or non-acknowledgement (NACK) information corresponding to a plurality of downlink sub-frames, that is, after demodulating and decoding data in a downlink sub-frame n−k, the UE feeds back in an uplink sub-frame n, to the eNB, signaling (that is, ACK/NACK information) of whether to retransmit the data in the downlink sub-frame, kεK, K: {k 0 , k 1 , . . . k M−1 }, where the values of the set K depend upon an uplink and downlink configuration of the system and a particular sub-frame number as depicted in Table 2:
[0000]
TABLE 2
Uplink and downlink
Sub-frame number (n)
sub-frame configuration
0
1
2
3
4
5
6
7
8
9
0
—
—
6
—
4
—
—
6
—
4
1
—
—
7, 6
4
—
—
—
7, 6
4
—
2
—
—
8, 7, 4, 6
—
—
—
—
8, 7,
—
—
4, 6
3
—
—
7, 6, 11
6, 5
5, 4
—
—
—
—
—
4
—
—
12, 8, 7, 11
6, 5,
—
—
—
—
—
—
4, 7
5
—
—
13, 12, 9, 8, 7,
—
—
—
—
—
—
—
5, 4, 11, 6
6
—
—
7
7
5
—
—
7
7
—
[0010] Here a plurality of radio frames are arranged sequentially, that is, if the last sub-frame in a radio frame a is k, then the first sub-frame in a radio frame a+1 is k+1, and Table 2 depicts K corresponding to each uplink sub-frame by way of an example with only one radio frame, where n−k<0 represents a downlink sub-frame in a preceding radio frame.
[0011] In the existing carrier aggregation system, the UE feeds back UL ACK/NACK at the foregoing timing in each aggregated cell, and the corresponding feedback is performed in a primary cell (PCell).
[0012] For transmission of uplink data, the eNB needs to transmit in the downlink an ACK/NACK feedback, which is carried over a Physical Hybrid Automatic Repeat Request (HARQ) Indicator Channel (PHICH). For a Frequency Division Duplex (FDD) system, uplink and downlink sub-frames coexist, that is, there is a PHICH resource per sub-frame, so there is a relatively fixed timing relationship between the downlink ACK/NACK feedback and the corresponding uplink data, where ACK/NACK feedback information corresponding to uplink data in the n-th sub-frame is transmitted in the (n+4)-th downlink sub-frame. For a TDD system, there are different numbers of uplink and downlink sub-frames in different TDD sub-frame configurations, such a case may arise that ACK/NACK feedback information of a plurality of uplink sub-frames are transmitted in the same downlink sub-frame, where ACK/NACK feedback information corresponding to uplink data in the n-th sub-frame is transmitted in the (n+k)-th downlink sub-frame, and the value of k is as depicted in Table 3:
[0000]
TABLE 3
TDD uplink
and downlink sub-frame
Uplink sub-frame number (n)
configuration
0
1
2
3
4
5
6
7
8
9
0
4
7
6
4
7
6
1
4
6
4
6
2
6
6
3
6
6
6
4
6
6
5
6
6
4
6
6
4
7
[0013] In existing carrier aggregation, the UE receives DL ACK/NACK information at the foregoing timing in each aggregated cell, and the corresponding feedback is received over the PHICH channel in the cell in which a UL grant scheduling a Physical Uplink Shared Channel (PUSCH) is transmitted.
[0014] In the system of the LTE Rel-11 or later, in order to avoid interference with another TDD system, there is such network deployment that different TDD uplink and downlink sub-frame configurations may be used in a plurality of LTE cells in different bands as illustrated in FIG. 3 where a carrier 1 is in a band A, and a carrier 2 is in a band B, and a cell 1 and a cell 2 are cells respectively over the carrier 1 and the carrier 2. A TDD uplink and downlink sub-frame configuration of the cell 1 is the configuration 0, and a TDD uplink and downlink sub-frame configuration of the cell 2 is the configuration 1 different from that of the cell 1. If the UE intends to perform carrier aggregation for these two cells, then such a case may arise that there are different TDD uplink and downlink configurations of the aggregated cells for the UE as illustrated in FIG. 4 , and this network deployment scheme using different TDD configurations may result in inconsistent transmission directions of different cells in the same sub-frame, for example, the sub-frame 4 and the sub-frame 9 illustrated in FIG. 4 are uplink sub-frames in the cell 1 and downlink sub-frames in the cell 2. For some UE with a low capability, a capability to operate simultaneously in a plurality of cells may be absent in such sub-frames.
[0015] In summary, there has been no solution so far in the prior art to how the UE incapable of supporting simultaneous uplink and downlink transmission communicates data in the carrier aggregation system using different TDD uplink and downlink configurations.
SUMMARY
[0016] Embodiments of the invention provide a data communication method and apparatus in a carrier aggregation system so as to enable a UE incapable of supporting simultaneous uplink and downlink transmission to communicate data in the carrier aggregation system using different TDD uplink and downlink configurations.
[0017] An embodiment of the invention provides a data communication method in a carrier aggregation system, including:
[0018] an eNB communicating data with a specific User Equipment, UE, over component carriers in the carrier aggregation system using a Time Division Duplex, TDD, uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system,
[0019] wherein the specific UE is a TDD UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0020] An embodiment of the invention provides another data communication method in a carrier aggregation system, including:
[0021] a User Equipment, UE, communicating data with an eNB over component carriers in the carrier aggregation system using a Time Division Duplex. TDD, uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system,
[0022] wherein the specific UE is a TDD UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0023] An embodiment of the invention provides a data communication apparatus in a carrier aggregation system, including:
[0024] a sub-frame configuration determining component configured to determine a Time Division Duplex, TDD, uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system; and
[0025] a data communication processing component configured to communicate data with a specific User Equipment, UE, over component carriers in the carrier aggregation system using the Time Division Duplex, TDD, uplink and downlink sub-frame configuration adopted for the specific component carrier in the carrier aggregation system;
[0026] wherein the specific UE is a UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0027] An embodiment of the invention provides another data communication apparatus in a carrier aggregation system, including:
[0028] a sub-frame configuration determining component configured to determine a Time Division Duplex, TDD, uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system; and
[0029] a data communication processing component configured to communicate data with an eNB over component carriers in the carrier aggregation system using the Time Division Duplex, TDD, uplink and downlink sub-frame configuration adopted for the specific component carrier in the carrier aggregation system;
[0030] wherein the specific UE is a UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0031] In the embodiments of the invention, an eNB communicates with a specific User Equipment (UE) over component carriers in the carrier aggregation system using a Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system, where the specific UE is a TDD UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame, thereby enabling the UE incapable of supporting simultaneous uplink and downlink transmission to communicate data over a plurality of carriers in the carrier aggregation system using different TDD uplink and downlink configurations.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] FIG. 1 is a schematic diagram of carrier distribution in an LTE cell;
[0033] FIG. 2 is a schematic diagram of CA in the LTE-A;
[0034] FIG. 3 is a schematic diagram of different TDD uplink and downlink sub-frame configurations in different bands aggregated for an LTE-A CA UE;
[0035] FIG. 4 is a schematic diagram of two cells aggregated in the TDD configuration 0 and the TDD configuration 1;
[0036] FIG. 5 is a data communication method in a carrier aggregation system according to an embodiment of the invention;
[0037] FIG. 6 is a schematic diagram of a UE selecting a sub-frame transmission direction when the cell 1 is a Pcell using the TDD uplink and downlink configuration 0 and the cell 2 is an Scell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0038] FIG. 7 is a schematic diagram of a UE selecting a sub-frame transmission direction when the cell 1 is an Scell using the TDD uplink and downlink configuration 0 and the cell 2 is a Pcell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0039] FIG. 8 is a schematic diagram of a UE feeding back UL ACK/NACK when the cell 1 is an Scell using the TDD uplink and downlink configuration 0 and the cell 2 is a Pcell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0040] FIG. 9 is a schematic diagram of a UE feeding back UL ACK/NACK when the cell 1 is a Pcell using the TDD uplink and downlink configuration 0 and the cell 2 is an Scell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0041] FIG. 10 is a schematic diagram of a UE receiving a PHICH in non-cross-carrier scheduling when the cell 1 is a Pcell using the TDD uplink and downlink configuration 0 and the cell 2 is an Scell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0042] FIG. 11 is a schematic diagram of a UE receiving a PHICH in non-cross-carrier scheduling when the cell 1 is an Scell using the TDD uplink and downlink configuration 0 and the cell 2 is a Pcell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0043] FIG. 12 is a schematic diagram of a UE receiving a PHICH in cross-carrier scheduling when the cell 1 is a Pcell using the TDD uplink and downlink configuration 0 and the cell 2 is an Scell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0044] FIG. 13 is a schematic diagram of a UE receiving a PHICH in cross-carrier scheduling when the cell 1 is an Scell using the TDD uplink and downlink configuration 0 and the cell 2 is a Pcell using the TDD uplink and downlink configuration 1 according to an embodiment of the invention;
[0045] FIG. 14 is a schematic structural diagram of a data communication apparatus in a carrier aggregation system according to an embodiment of the invention; and
[0046] FIG. 15 is a schematic structural diagram of another data communication apparatus in a carrier aggregation system according to an embodiment of the invention.
DETAILED DESCRIPTION
[0047] Embodiments of the invention provide a data communication method and apparatus in a carrier aggregation system so as to enable a UE incapable of supporting simultaneous uplink and downlink transmission to communicate data in the carrier aggregation system using different TDD uplink and downlink configurations, that is, a technical solution according to the embodiments of the invention enables the UE incapable of supporting simultaneous uplink and downlink transmission to communicate with carrier aggregation in a carrier aggregation scenario using different TDD uplink and downlink configurations across bands.
[0048] The embodiments of the invention propose such solutions that a TDD UE incapable of supporting simultaneous uplink and downlink transmission performs communication and a feedback with aggregation when the UE accesses a multi-carrier network using different TDD uplink and downlink configurations. The following description will be given with reference to the drawings.
[0049] Referring to FIG. 5 , a data communication method in a carrier aggregation system at the eNB side according to an embodiment of the invention includes the following steps:
[0050] S 101 . An eNB determines a UE needing to communicate data as a specific UE, where the specific UE is a TDD UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0051] Preferably the method further includes:
[0052] The eNB receives capability information reported from the UE and obtains therefrom an indicator of whether the UE is the specific UE, and determines from the indicator the UE as the specific UE in the step 101 .
[0053] S 102 . The eNB communicates data with the specific UE over component carriers in the carrier aggregation system using a Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system.
[0054] Preferably in the step S 102 , for the specific component carrier, the eNB communicates data with the specific UE over the specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier; and
[0055] For a non-specific component carrier, the eNB communicates data with the specific UE over the non-specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier as follows:
[0056] The eNB judges whether the non-specific component carrier has the same transmission direction as the specific component carrier in the same sub-frame, and if so, then the eNB determines the sub-frame as an available sub-frame to the non-specific component carrier, otherwise, the eNB determines the sub-frame as an unavailable sub-frame to the non-specific component carrier;
[0057] The eNB schedules for the UE an uplink transmission resource corresponding to an uplink available sub-frame and receives data transmitted from the UE over the scheduled uplink transmission resource; and
[0058] The eNB transmits downlink data to the UE in a downlink available sub-frame.
[0059] For example, the UE is configured with carrier aggregation and assigned with a Pcell, and as prescribed, the UE refers to transmission directions of respective sub-frames over a component carrier corresponding to the Pcell, and if the transmission direction of the same sub-frame in a secondary cell (Scell) is different from the Pcell, then the sub-frame in the Scell is ignored for corresponding processing.
[0060] Referring to FIG. 6 , if the cell 1 is a Pcell and the cell 2 is an Scell, then the UE operates in the Pcell in the sub-frames 4 and 9 which are uplink sub-frames, and ignores reception and processing in the Scell in corresponding downlink sub-frames (including corresponding blind detection of a DL grant and reception of a downlink signal being ignored).
[0061] Preferably after the eNB transmits the data to the UE, the method further includes:
[0062] The eNB receives uplink (UL) acknowledgement (ACK)/non-acknowledgement (NACK) information transmitted from the UE in an uplink sub-frame of the specific component carrier according to a timing correspondence relationship between data reception over a Physical Downlink Shared Channel (PDSCH) and the UL ACK/NACK information feedback of the specific component carrier.
[0063] Preferably the UL ACK/NACK information transmitted from the UE does not include UL ACK/NACK information corresponding to a downlink unavailable sub-frame to the non-specific component carrier.
[0064] Still taking FIG. 6 as an example, the UE feeds back UL ACK/NACK by precluding from the size of an ACK/NACK codebook the downlink sub-frame ignored for processing and not feeding back UL ACK/NACK for the downlink sub-frame.
[0065] On the contrary, referring to FIG. 7 , if the cell 1 is an Scell and the cell 2 is a Pcell, then the UE receives and processes in the Pcell in the sub-frames 4 and 9 which are downlink sub-frames and ignores transmission and processing in the Scell in the corresponding uplink sub-frames (including corresponding blind detection of a UL grant and reception of an uplink signal being ignored).
[0066] Downlink and uplink data transmission of the Scell here may be scheduled by a DL grant and a UL grant of the Scell itself or be scheduled across the carriers by a DL grant and a UL grant of the PCell.
[0067] For example, the specific component carrier is a Pcell carrier, and the UE communicates data over the component carrier in the carrier aggregation system using a TDD uplink and downlink sub-frame configuration of the Pcell. Upon reception of data over a Physical Downlink Shared Channel (PDSCH) in the corresponding downlink sub-frames of the Pcell and the Scell, the UE feeds back corresponding PDSCH ACK/NACK information of the Pcell and the Scell in a corresponding uplink sub-frame in the Pcell according to a timing relationship between the PDSCH and UL ACK/NACK in the Pcell, that is, the UE feeds back corresponding PDSCH ACK/NACK information of the Pcell and the Scell in a corresponding uplink sub-frame over the specific carrier according to UL ACK/NACK timing of the specific carrier.
[0068] Referring to FIG. 8 and FIG. 9 illustrating feedback correspondence relationships respectively when the Pcell is configured differently, an arrow represents a PDSCH reception sub-frame pointing to an UL ACK/NACK feedback sub-frame. The PDSCH to UL ACK/NACK timing here is the same as the LTE Rel-8, that is, the timing relationship corresponding to the Pcell may be retrieved in Table 2, where for a forked downlink sub-frame, the UE does not receive and process it and does not feed back corresponding UL ACK/NACK.
[0069] Downlink data transmission of the Scell as described in the embodiment of the invention may be scheduled by a DL grant of the Scell itself or may be scheduled across the carriers by a DL grant of the Pcell.
[0070] Preferably after the eNB receives the data transmitted from the UE over the scheduled uplink transmission resource, the method further includes:
[0071] The eNB transmits downlink (DL) acknowledgement (ACK) or non-acknowledgement (NACK) information to the UE over a Physical Hybrid Automatic Repeat Request (HARQ) Indicator Channel (PHICH) according to a timing correspondence relationship between data transmission over a Physical Uplink Shared Channel (PUSCH) and reception of the DL ACK/NACK information over the PHICH.
[0072] Preferably in the case that the secondary cell Scell is not configured with cross-carrier scheduling, the eNB transmits the DL ACK/NACK information to the UE over the PHICH according to the timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH as follows:
[0073] The eNB transmits the DL ACK/NACK information to the UE over the PHICH in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier; and
[0074] The eNB transmits the DL ACK/NACK information to the UE over the PHICH in a downlink available sub-frame of the non-specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the non-specific component carrier.
[0075] Preferably in the case that the secondary cell Scell is configured with cross-carrier scheduling, the eNB transmits the DL ACK/NACK information to the UE over the PHICH according to the timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH as follows:
[0076] The eNB transmits the DL ACK/NACK information to the UE over the PHICH only in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier.
[0077] For example the UE receives the DL ACK/NACK feedback over the corresponding PHICH according to the following timing relationship after transmitting the PUSCH in the corresponding uplink sub-frames of the Pcell and the Scell.
[0078] In a first case, if the Scell is not configured with cross-carrier scheduling, that is, PUSCH transmission in the Scell is scheduled by a UL grant of the Scell itself, then the UE receives respective DL ACK/NACK feedbacks of the Pcell and the Scell in the Pcell and the Scell at their respective separate PUSCH to PHICH timings.
[0079] As illustrated in FIG. 10 , the direction of an arrow represents a PUSCH transmission sub-frame corresponding to a PHICH feedback sub-frame. The PUSCH to PHICH timing relationship is the same as the LTE Rel-8, that is, the respective timing relationships corresponding to the Pcell and the Scell may be retrieved respectively in Table 3.
[0080] It shall be noted that the UE can not receive the PHICH data in the Scell in a downlink sub-frame ignored for processing due to a different transmission direction from the Pcell (e.g., a downlink sub-frame forked in FIG. 10 ), so transmission of an uplink PUSCH procedure associated therewith may also be influenced, and the eNB may not schedule the PUSCH in these sub-frames; and moreover the eNB may alternatively schedule the PUSCH in these sub-frames but not feed back DL ACK/NACK for these sub-frames.
[0081] As illustrated in FIG. 10 , the eNB may schedule the PUSCH in the sub-frame 3 of the Scell, and the UE transmits data in the sub-frame 3 of the Scell, but a DL ACK/NACK feedback sub-frame corresponding to the sub-frame 3 of the Scell is the sub-frame 9 of the Scell, and the UE does not process the sub-frame 9 of the Scell, so the eNB does not feed back DL ACK/NACK for the sub-frame 3 of the Scell. Moreover the eNB may alternatively not schedule the PUSCH in the sub-frame 3 of the Scell so that the UE does not transmit data in the sub-frame 3 of the Scell. The same applies to the sub-frame 8 of the Scell and the sub-frame 3 of the Scell.
[0082] Moreover the UE does not transmit the PUSCH data in the Scell in an uplink sub-frame ignored for processing due to a different transmission direction from the Pcell (e.g., an uplink sub-frame forked in FIG. 11 ), so the UE does not receive the PHICH data in a corresponding downlink feedback sub-frame either.
[0083] In a second case, if the Scell is configured with cross-carrier scheduling, that is, PUSCH transmission in the Scell is scheduled by a UL grant of the Pcell, then the UE receives PUSCH DL ACK/NACK feedbacks for the Pcell and the Scell over the PHICH of the downlink sub-frame of the carrier (i.e., the Pcell) transmitting the UL grant according to the PUSCH to PHICH timing in the Pcell.
[0084] As illustrated in FIG. 12 and FIG. 13 , the direction of an arrow represents a PUSCH transmission sub-frame corresponding to a PHICH feedback sub-frame. The PUSCH to PHICH timing relationship here is the same as the LTE Rel-8, that is, the timing relationship corresponding to the Pcell may be retrieved in Table 3.
[0085] It shall be noted that the UE does not transmit the PUSCH data in the Scell in an uplink sub-frame ignored for processing due to a different transmission direction from the Pcell (e.g., an uplink sub-frame forked in FIG. 13 ), so the UE does not receive the PHICH data in a corresponding downlink feedback sub-frame either.
[0086] Preferably the method further includes:
[0087] The eNB transmits an indicator of the specific component carrier to the UE.
[0088] Preferably the specific component carrier is a component carrier adopted for the primary cell Pcell.
[0089] In the embodiment of the invention, the Pcell is preferably referred to, but another component carrier may alternatively be taken as a specific component carrier, that is, a Scell may be referred to, and the sequence number of the reference Scell (or the sequence number of the specific component carrier) may be notified by the eNB to the UE. That is, the UE may receive the indicator of the specific component carrier and determine the specific component carrier from the indicator.
[0090] In the foregoing embodiment of the invention, the solution to data communication referring to the Pcell is proposed, but another specific cell can be referred to, and the sequence number of the reference cell can be notified by the eNB to the UE. Moreover in the embodiment of the invention, there is an operating scheme in which the Pcell and the Scell are configured with different TDD uplink and downlink sub-frame configurations, but the technical solution according to the embodiment of the invention can be equally applicable to the case that a plurality of Scells are configured with different TDD uplink and downlink sub-frame configurations and the case that cross-carrier scheduling is configured across Scclls.
[0091] Correspondingly at the UE side, a data communication method in a carrier aggregation system according to an embodiment of the invention includes:
[0092] A User Equipment (UE) communicates data with an eNB over component carriers in the carrier aggregation system using a Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system;
[0093] Where the specific UE is a TDD UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0094] Preferably for the specific component carrier, the UE communicates data with the eNB over the specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier; and
[0095] For a non-specific component carrier, the UE communicates data with the eNB over the non-specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier in the carrier aggregation system as follows:
[0096] The UE obtains an uplink transmission resource corresponding to an uplink available sub-frame scheduled by the eNB and transmits data to the eNB over the uplink transmission resource; and
[0097] The UE receives data transmitted from the eNB in a downlink available sub-frame;
[0098] Where the available sub-frame refers to a sub-frame in which the non-specific component carrier has the same transmission direction with the specific component carrier.
[0099] Preferably after the UE receives the data transmitted from the eNB, the method further includes:
[0100] The UE transmits uplink (UL) acknowledgement (ACK)/non-acknowledgement (NACK) information to the eNB in an uplink sub-frame of the specific component carrier according to a timing correspondence relationship between data reception over a Physical Downlink Shared Channel (PDSCH) and the UL ACK/NACK information feedback of the specific component carrier.
[0101] Preferably the UL ACK/NACK information transmitted from the UE does not include UL ACK/NACK information corresponding to a downlink unavailable sub-frame of the non-specific component carrier;
[0102] Where the unavailable sub-frame refers to a sub-frame in which the non-specific component carrier has a different transmission direction from the specific component carrier.
[0103] Preferably after the UE transmits the data to the eNB over the uplink transmission resource scheduled by the eNB, the method further includes:
[0104] The UE receives downlink (DL) acknowledgement (ACK) or non-acknowledgement (NACK) transmitted from the eNB over a Physical Hybrid Automatic Repeat Request (HARQ) Indicator Channel (PHICH) according to a timing correspondence relationship between data transmission over a Physical Uplink Shared Channel (PUSCH) and reception of the DL ACK/NACK information over the PHICH.
[0105] Preferably in the case that a secondary cell Scell is not configured with cross-carrier scheduling, the UE receives the DL ACK/NACK transmitted from the eNB over the PHICH according to the timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH as follows:
[0106] The UE receives the DL ACK/NACK information over the PHICH in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH over the specific component carrier; and
[0107] The UE receives the DL ACK/NACK information over the PHICH in a downlink available sub-frame of the non-specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the non-specific component carrier.
[0108] Preferably in the case that a secondary cell Scell is configured with cross-carrier scheduling, the UE receives the DL ACK/NACK information transmitted from the eNB over the PHICH according to the timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH as follows:
[0109] The UE receives the DL ACK/NACK information over the PHICH only in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier.
[0110] Preferably the method further includes:
[0111] The UE receives an indicator of the specific component carrier transmitted from the eNB and determines the specific component carrier from the indicator.
[0112] Preferably the specific component carrier is a component carrier adopted for a primary cell Pcell.
[0113] Preferably the method further includes:
[0114] The UE reports capability information of the UE to the eNB, where the capability information includes an indicator of whether the UE is a specific UE.
[0115] Referring to FIG. 14 , a data communication apparatus in a carrier aggregation system at the eNB side includes:
[0116] A sub-frame configuration determining component 11 configured to determine a Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system; and
[0117] A data communication processing component 12 configured to communicate data with a specific User Equipment (UE) over component carriers in the carrier aggregation system using the Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for the specific component carrier in the carrier aggregation system;
[0118] Where the specific UE is a UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0119] Preferably,
[0120] For the specific component carrier, the data communication processing component 12 communicates data with the specific UE over the specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier; and
[0121] For a non-specific component carrier, the data communication processing component 12 judges whether the non-specific component carrier has the same transmission direction as the specific component carrier in the same sub-frame, and if so, then it determines the sub-frame as an available sub-frame to the non-specific component carrier, otherwise, it determines the sub-frame as an unavailable sub-frame to the non-specific component carrier; schedules for the UE an uplink transmission resource corresponding to an uplink available sub-frame and receives data transmitted from the UE over the scheduled uplink transmission resource; and transmits downlink data to the UE in a downlink available sub-frame.
[0122] Preferably the apparatus further includes:
[0123] An uplink feedback processing component 13 configured to receive uplink (UL) acknowledgement (ACK)/non-acknowledgement (NACK) information transmitted from the UE in an uplink sub-frame of the specific component carrier according to a timing correspondence relationship between data reception over a Physical Downlink Shared Channel (PDSCH) and the UL ACK/NACK information feedback of the specific component carrier after the data communication processing component 12 transmits the data to the UE.
[0124] Preferably the UL ACK/NACK information, received by the uplink feedback processing component 13 , transmitted from the UE does not include UL ACK/NACK information corresponding to a downlink unavailable sub-frame to the non-specific component carrier.
[0125] Preferably the apparatus further includes:
[0126] A downlink feedback processing component 14 configured to transmit downlink (DL) acknowledgement (ACK) or non-acknowledgement (NACK) information to the UE over a Physical Hybrid Automatic Repeat Request (HARQ) Indicator Channel (PHICH) according to a timing correspondence relationship between data transmission over a Physical Uplink Shared Channel (PUSCH) and reception of the DL ACK/NACK information over the PHICH after the data communication processing component 12 receives the data transmitted from the UE over the scheduled uplink transmission resource.
[0127] Preferably in the case that a secondary cell Scell is not configured with cross-carrier scheduling, the downlink feedback processing component 14 transmits the DL ACK/NACK information to the UE over the PHICH in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier; and transmits the DL ACK/NACK information to the UE over the PHICH in a downlink available sub-frame of the non-specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the non-specific component carrier.
[0128] Preferably in the case that a secondary cell Scell is configured with cross-carrier scheduling, the downlink feedback processing component 14 transmits the DL ACK/NACK information to the UE over the PHICH only in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier.
[0129] Preferably the apparatus further includes:
[0130] A specific component carrier indicating component 15 configured to transmit an indicator of the specific component carrier to the UE.
[0131] Preferably the specific component carrier is a component carrier adopted for a primary cell Pcell.
[0132] Preferably the apparatus further includes:
[0133] A specific UE determining component 16 configured to receive capability information reported from the UE, to obtain therefrom an indicator of whether the UE is a specific UE and to determine from the indicator the UE as a specific UE.
[0134] Referring to FIG. 15 , a data communication apparatus in a carrier aggregation system at the UE side includes:
[0135] A sub-frame configuration determining component 21 configured to determine a Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for a specific component carrier in the carrier aggregation system; and
[0136] A data communication processing component 22 configured to communicate data with an eNB over component carriers in the carrier aggregation system using the Time Division Duplex (TDD) uplink and downlink sub-frame configuration adopted for the specific component carrier in the carrier aggregation system;
[0137] Where the specific UE is a UE incapable of supporting simultaneous uplink data transmission and downlink data transmission in the same sub-frame.
[0138] Preferably,
[0139] For the specific component carrier, the data communication processing component 22 communicates data with the eNB over the specific component carrier in the carrier aggregation system using the TDD uplink and downlink sub-frame configuration adopted for the specific component carrier; and
[0140] For a non-specific component carrier, the data communication processing component 22 obtains an uplink transmission resource corresponding to an uplink available sub-frame scheduled by the eNB and transmits data to the eNB over the uplink transmission resource; and receives data transmitted from the eNB in a downlink available sub-frame;
[0141] Where the available sub-frame refers to a sub-frame in which the non-specific component carrier has the same transmission direction as the specific component carrier.
[0142] Preferably the apparatus further includes:
[0143] An uplink feedback processing component 23 configured to transmit uplink (UL) acknowledgement (ACK)/non-acknowledgement (NACK) information to the eNB in an uplink sub-frame of the specific component carrier according to a timing correspondence relationship between data reception over a Physical Downlink Shared Channel (PDSCH) and the UL ACK/NACK information feedback of the specific component carrier after the data communication processing component receives the data transmitted from the eNB.
[0144] Preferably the UL ACK/NACK information transmitted from the uplink feedback processing component 23 does not include UL ACK/NACK information corresponding to a downlink unavailable sub-frame of the non-specific component carrier;
[0145] Where the unavailable sub-frame refers to a sub-frame in which the non-specific component carrier has a different transmission direction from the specific component carrier.
[0146] Preferably the apparatus further includes:
[0147] A downlink feedback processing component 24 configured to receive downlink (DL) acknowledgement (ACK) or non-acknowledgement (NACK) information transmitted from the eNB over a Physical Hybrid Automatic Repeat Request (HARQ) Indicator Channel (PHICH) according to a timing correspondence relationship between data transmission over a Physical Uplink Shared Channel (PUSCH) and reception of the DL ACK/NACK information over the PHICH after the data communication processing component 22 transmits the data to the eNB over the uplink transmission resource scheduled by the eNB.
[0148] Preferably in the case that a secondary cell Scell is not configured with cross-carrier scheduling, the downlink feedback processing component 24 receives the DL ACK/NACK information over the PHICH in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier; and receives the DL ACK/NACK information over the PHICH in a downlink available sub-frame of the non-specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the non-specific component carrier.
[0149] Preferably in the case that a secondary cell Scell is configured with cross-carrier scheduling, the downlink feedback processing component 24 receives the DL ACK/NACK information over the PHICH only in a downlink sub-frame of the specific component carrier according to a timing correspondence relationship between data transmission over the PUSCH and reception of the DL ACK/NACK information over the PHICH of the specific component carrier.
[0150] Preferably the apparatus further includes:
[0151] A specific component carrier determining component 25 configured to receive an indicator of the specific component carrier transmitted from the eNB and to determine the specific component carrier from the indicator.
[0152] Preferably the specific component carrier is a component carrier adopted for a primary cell Pcell.
[0153] Preferably the apparatus further includes:
[0154] A capability information reporting component 26 configured to report capability information of the UE to the eNB, where the capability information includes an indicator of whether the UE is a specific UE.
[0155] In summary, in the embodiments of the invention, the UE decides the use of the uplink and downlink sub-frames of the respective component carriers according to the transmission direction of the specific component carrier; the UE decides UL ACK/NACK feedbacks over the respective component carriers according to a timing relationship between the PDSCH and the UL ACK/NACK of the specific component carrier; and the UE decides a scheme to receive a PHICH over the respective component carriers according to a timing relationship between the PDSCH and the UL ACK/NACK of the specific component carrier. The solution to transmission of uplink and downlink data with carrier aggregation and the corresponding feedback solution are proposed for a TDD UE incapable of supporting simultaneous uplink and downlink transmission when the UE accesses a multi-carrier network using different TDD uplink and downlink configurations.
[0156] Those skilled in the art shall appreciate that the embodiments of the invention can be embodied as a method, a system or a computer program product. Therefore the invention can be embodied in the form of an all-hardware embodiment, an all-software embodiment or an embodiment of software and hardware in combination. Furthermore the invention can be embodied in the form of a computer program product embodied in one or more computer useable storage mediums (including but not limited to a disk memory, an optical memory, etc.) in which computer useable program codes are contained.
[0157] The invention has been described in a flow chart and/or a block diagram of the method, the device (system) and the computer program product according to the embodiments of the invention. It shall be appreciated that respective flows and/or blocks in the flow chart and/or the block diagram and combinations of the flows and/or the blocks in the flow chart and/or the block diagram can be embodied in computer program instructions. These computer program instructions can be loaded onto a general-purpose computer, a specific-purpose computer, an embedded processor or a processor of another programmable data processing device to produce a machine so that the instructions executed on the computer or the processor of the other programmable data processing device create means for performing the functions specified in the flow(s) of the flow chart and/or the block(s) of the block diagram.
[0158] These computer program instructions can also be stored into a computer readable memory capable of directing the computer or the other programmable data processing device to operate in a specific manner so that the instructions stored in the computer readable memory create an article of manufacture including instruction means which perform the functions specified in the flow(s) of the flow chart and/or the block(s) of the block diagram.
[0159] These computer program instructions can also be loaded onto the computer or the other programmable data processing device so that a series of operational steps are performed on the computer or the other programmable data processing device to create a computer implemented process so that the instructions executed on the computer or the other programmable device provide steps for performing the functions specified in the flow(s) of the flow chart and/or the block(s) of the block diagram.
[0160] Evidently those skilled in the art can make various modifications and variations to the invention without departing from the scope of the invention. Thus the invention is also intended to encompass these modifications and variations thereto so long as the modifications and variations come into the scope of the claims appended to the invention and their equivalents. | Disclosed are a data transmission method and device in a carrier aggregation system, used for realizing the data transmission of UE which does not support uplink and downlink transmission simultaneously in a carrier aggregation system which uses different TDD uplink and downlink configurations. The data transmission method in a carrier aggregation system provided in the present application includes: an eNB performing data transmission with specific user equipment (UE) according to the time division duplex (TDD) uplink and downlink sub-frame configuration employed by a specific component carrier in a carrier aggregation system by means of a component carrier in the carrier aggregation system, wherein said specific UE is TDDUE which does not support simultaneously performing uplink data transmission and downlink data transmission in an identical sub-frame. | 7 |
This is a continuation of application Ser. No. 675,424 lfiled Nov. 27, 1984, now U.S. Pat. No. 4,718,023.
BACKGROUND OF THE INVENTION
This invention relates generally to robot devices, and, more particularly, to apparatus for positioning a movable part of a robot in relation to a surface.
Robots are mechanical devices which can perform tasks in a manner that simulates human activity. One type of robot, the industrial robot, is finding widespread acceptance in manufacturing and other industrial operations, and promises many benefits in the automation of repetitive industrial operations. A typical industrial robot includes a stationary portion, usually referred to as the body, and a movable portion, usually referred to as the arm, wrist or hand, with the movable portion adapted for performing an operation on a workpiece. By way of example, robot arms can assemble components, join components as by welding, and finish components as by cleaning and painting.
In most industrial operations, a critical aspect of the operation of robot devices is the precise positioning of the movable robot arm with respect to the workpiece. In the simplest robots, each workpiece must be positioned at an exact location and orientation with respect to the robot arm, so that no separate sensing device is necessary to orient the robot arm with respect to each successive workpiece. For the robot arm to perform operations which require it to move over the surface of a workpiece, usually referred to as a continuous path operation, as in the painting of a part, a coordinate map of the surface of the workpiece must be coded into the memory of a computer which controls the trajectory of the moving robot. In such simple robots, failure to orient a workpiece in its exactly proper position can result in a failure of the operation to be performed by the robot. Further, such robots must be dedicated in the sense that a large amount of information concerning each particular type of workpiece must be coded into the control computer, and changes in the workpiece require reprogramming.
A more complex type of control utilizes some form of sensor to gather information about the workpiece and transmit this information to the robot, thereby providing a control input to the robot. As an example, a tactile or proximity sensor incorporated in the hand of the robot may be used to indicate the presence of a workpiece, and may also give some basic information about its orientation. Multiple tactile sensors can also be used to advantage. In a somewhat similar approach, light sources and photo cells may be used in combination to provide light beams which are broken when a workpiece is moved into position. However, both these approaches have not proved sufficiently versatile for use in many applications, especially where the robot arm is not in contact with, or in the close proximity of, the workpiece.
More recently, solid state video imaging systems have been developed for controlling robot devices. Such video imaging systems typically operate in a manner similar to television, wherein a visual field is scanned by a solid state camera to produce a sequential electronic signal having the visual image encoded thereupon. The digital signal is used to reconstruct an image on a television viewer or, for the purposes of controlling a robot, may be analyzed by existing pattern recognition techniques to provide information to the robot about the position, shape, and orientation of the workpiece, and the spacing of the robot arm from the workpiece. While robots having electronic video imaging systems represent an advance over the more primitive robots, such systems have severe disadvantages that limit their utilization in many applications. In many adverse working environments it is impossible to provide enough light to the camera. Image enhancement techniques are known, but in adverse environments the image may be insufficient for their use. More significantly, however, in all working environments such video imaging systems require a complex system utilizing extensive hardware components, including solid state cameras, a monitor and a computer, and complex programming and algorithms to recognize the patterns. The information from such video imaging systems is provided to a controlling computer which follows the encoded coordinate maps to guide the robot to take each successive step. Once the robot moves to its next step, the entire process of detecting the robot position and guiding it further must be repeated. In addition, the information transmission between interfaced devices is inherently slow, so that the system can communicate at a rate no greater than about 10-50 functions per second, thus limiting the speed and performance of the robot.
Robots equipped with video imaging systems must be controlled and their movement integrated by a central controller computer. This computer must necessarily be large and complex to provide the robot controller with a high degree of versatility, since it is often necessary to perform major computer reprogramming if the design of the workpiece is changed. For example, the computer may be programmed with a mathematical model of the surface of the workpiece for use in the pattern recognition function, and this mathematical model must be changed when the robot is to operate upon a different or modified workpiece. To some extent, such computers are therefore dedicated to use with a single type of workpiece, although the dedication may be changed by reprogramming.
There has been a need for a more versatile, non-dedicated apparatus to enable robots to sense the positioning of their movable arms with respect to the surface of a workpiece. Desirably, such an apparatus would be operable in adverse environments and would permit more rapid signal processing with less complex, less costly hardware and software. Such apparatus should be operable to allow the movable part of the robot to be positioned in a controllable manner adjacent the workpiece, with little or no preprogramming required for adapting the robot to operation in a continuous path on different workpieces. The present invention fulfills this need, and further provides related advantages.
SUMMARY OF THE INVENTION
The present invention resides in apparatus for sensing the presence and orientation of a surface, and then positioning a movable part of a robot, such as a robot arm, wrist, or hand, with respect to the surface, as on a workpiece to be processed by the robot. The apparatus utilizes parallel processing of signals to provide very high analysis cycle rates, typically on the order of 40,000-200,000 functions per second. The apparatus is operable in a wide range of liquid and gaseous environments, and its operation is largely unaffected by transient environments, such as those having vibrations, humidity or sparks, and environments having low or high light levels. The apparatus requires relatively simple hardware and no software to perform the basic positioning functions, so that the robot command control functions may be separated, with the control function remotely positioned in the movable arm. The control circuitry may be significantly reduced and simplified, thereby reducing the cost and complexity of the robot and eliminating most programming costs, while at the same time greatly increasing its versatility for operating upon a wide variety of types of workpieces.
In accordance with the invention, the apparatus for positioning a movable portion of a robot device with respect to a surface includes a precision positioning subsystem, an approximate positioning subsystem, or, preferably, both subsystems. The precision positioning subsystem comprises means for emitting an emitted signal toward the surface; means for receiving a response signal originating at the surface as a result of the emitting signal striking the surface, the means for receiving being mounted on the movable portion of the robot device and including at least two signal receivers; means for cmparing the time of flight of the signals received by the signal receivers on a pair-wise basis to create a comparison signal; and means for adjusting the movable portion of the robot device to maintain a predetermined value of the comparison signal on a pair-wise basis. The precision positioning subsystem may also include means for calculating the distance of the movable portion of the robot from the surface, from the time of flight of the signal received by at least one of the signal receivers, and means for comparing this calculated distance with a distance command signal so that the spacing of the movable portion of the robot may be adjusted to maintain the calculated distance equal to the distance command signal. Thus, the orientation of the movable part of the robot with respect to the surface may be determined and controlled through comparison of the time of flight of the signals received by the receivers, and the distance may be determined and controlled by the absolute value of the time of flight.
The approximate positioning subsystem comprises means for emitting at least two non-colinear emitted signals; means for receiving the respective response signals, if any, resulting from the striking of the respective emitted signals on a surface, said means for receiving being mounted on the moveable portion of the robot device; means for detecting the presence of a received signal; and means for adjusting the moveable portion of the robot device into an approximate facing relationship to the detected received signal. The approximate positioning subsystem is used to locate the surface and to approximately orient the precision positioning subsystem for precise robot control, but does not itself adjust the ranging of the moveable portion.
In a presently preferred embodiment, four pairs of emitting and receiving transducers of the approximate positioning subsystem are mounted peripherally on side lips of a sensor head and angularly directed outwardly and upwardly so as to sense the presence of a surface over a broad viewing area. The precision positioning subsystem transducers are mounted centrally among the approximate-positioning transmitters and receivers and have a relatively narrow field of view. The apparatus can thus seek out and locate a surface with the approximate positioning subsystem, rotating the moveable portion so that the precision positioning subsystem transducers approximately face the surface. Precise positioning and distance control are achieved by the precision positioning subsystem.
In this preferred embodiment the apparatus is responsive to one or more of four location incrementing command signals, three angular positioning command signals and one distance (range) positioning command signal. Mounted on the robot arm, the transmitters and receivers are arranged in a manner to provide a spatial field of view of about 135°-140°. The four pairs of wide beam transmitters and receivers of the approximate positioning subsystem view in four orthogonal directions within the field of view, while one narrow beam transmitter and three receivers of the precision positioning subsystem are mounted to view in the direction along the common axis of the four orthogonal directions. The electronic circuitry includes a signal generator to trigger the transmitters; a switching logic to provide the orientation control signal; two comparators, each of which receives the signal from one pair of the acoustic receivers and compares the signals to produce an output positioning control signal proportional to the difference in the time of flight of the signals received by each respective pair of acoustic receivers; a distance calculator which calculates a distance based on the time between emission of the acoustic signal and its receipt; and a controller for adjusting the position of the robot arm so that the two orientation command signals are respectively equal to the two orientation control signals, and the distance command signal to equal to the distance control signal.
The use of acoustic frequencies is preferred, since acoustic transmitters and receivers are readily available, and the signal propagation times are sufficiently rapid to allow high functional repetition rates, but sufficiently slow to allow the use of conventional comparators and time of flight measurement circuitry. The acoustic transmitters and receivers are preferably mounted on a square, flat sensor head having angled side lips at preferably 60° upward inclination on each of the four sides of the head, which in turn is mounted on the hand of the robot arm. One narrow beam acoustic transmitter is located centrally within the pattern formed by the three narrow beam acoustic receivers on the flat face of the sensor head, preferably spaced 120° apart on the square. One pair each of the broad band acoustic transmitter and receiver are mounted to the lip face such that the field of view is about 135°-140°. Orientation control is achieved when the switching logic identifies which pair of the broad beam acoustic receivers mounted on the side lips is receiving a response signal after reflection from an obliquely oriented reference surface in its field of view. The switching logic sends an orientation control signal to the robot motor controls and moves the robot hand in the direction from which the response signal was first received. The movement is continued until the response signal is no longer received by any of the side mounted broad beam acoustic receivers. At this time the robot hand is approximately in a facing relation with the flat face of the sensor head parallel to the reference surface. Precise position control is then achieved by measuring the difference between the time of flight of the acoustic signal to the different precision positioning subsystem acoustic receivers. For example, the sensor head is oriented parallel to the surface when the three time of flight signals are equal. Total distance from the surface of the workpiece to the robot hand is proportional to the time of flight of the acoustic signal. The controller drives positioning motors which can reorient the hand of the robot arm and also change its distance from the surface, thereby achieving complete positioning control of the arm in relation to the workpiece, without the need for a complex pattern recognition function or pre-mapping of the surface of the workpiece.
It will be appreciated from the foregoing that the present apparatus represents an important and significant advance in the field of controlling robot devices. The apparatus allows functional separation of the command and control operations so that the control function is accomplished remotely at the movable portion of the robot rather than requiring transmission of signals to a central command computer. Control is accomplished by parallel rather than serial processing to enable use of a high functional control rate, and the control function is achieved utilizing relatively simple hardware rather than a combination of complex hardware and complex software. Reprogramming costs are therefore significantly reduced as compared with prior devices. The apparatus is operable in a very wide range of operating environments without the need for readjustment or recalibration, including all light levels, dirty environments, and transient environments, such as clouds of opaque particles. Other features and advantages of the present invention will become apparent from the more detailed description, taken in conjunction with the accompanying drawings, which illustrate, by way of example, the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a robot arm employing an apparatus in accordance with a preferred embodiment of the invention, for orienting the arm with respect to a surface;
FIG. 2 is a block functional diagram of a prior approach to positioning of a robot arm using a video camera;
FIG. 3 is a block functional diagram of one embodiment of the present approach to orienting a robot arm;
FIG. 4 is a perspective view of a multiple-sensor array used in approximate position control;
FIG. 5 is a perspective view of a presently preferred sensor head;
FIG. 6 is a side view of the sensor head of FIG. 5;
FIG. 7 is a block circuit diagram of the approximate positioning subsystem used in orienting a robot arm;
FIG. 8 is a circuit diagram of the precision positioning subsystem used in orienting a robotm arm; and
FIG. 9 is an examplary schematic signal timing diagram for the precision positioning subsystem.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
As is shown in the drawings with reference to a preferred embodiment, the present invention is concerned with apparatus 10 for controlling the movable portion on arm 12 of a robot device 14. The robot 14 comprises a stationary base 16 and the movable arm 12. Robots may have a variety of physical arrangements for attaining movement in three dimensions, and the robot 14 of FIG. 1 illustrates just one such possibility. In the robot 14, the movable arm 12 achieves vertical movement by a vertical movement motor 18. Rotational movement about two axes in a horizontal plane is accomplished by a first rotational motor 20 and a second rotational motor 22. The first rotational motor 20 causes rotation of an outer arm 24 in relation to an inner arm 26, about a first rotational axis 28. The second rotational motor 22 accomplishes rotation of a sensor head 30 in a yoke 32 of the outer arm 24, about a second rotational axis 34 which is perpendicular to the first rotational axis 28. Complete three-dimensional movement of the sensor head 30 is accomplished by coordinated operation of the motors 18, 20, and 22.
The present invention relates to apparatus 10 for controlling the movement of the motors 18, 20, and 22. By way of contrasting the operation of the apparatus 10 with prior apparatus which also achieves control of the motors, FIGS. 2 and 3 present block functional diagrams of the prior approach and the present approach, respectively. As illustrated in FIG. 2, in the prior approach, a camera 36 is focused on a surface 38 to create a scanned image of the surface 38. The scanned image is fed in a serial manner to a digitizer 40, whose output is presented to a pattern recognizer 42. The pattern recognizer 42 analyzes key features of the digitized serial representation of the image and compares it with a digital map provided in the memory of a computer 44 controlling the robot 14. An analysis of the position of the movable arm 12 with respect to the surface 38 is made by the computer 44, which compares the present position with a command signal. A repositioning signal is then provided to a controller 46 by the computer 44. The controller 46 generates a control signal which is provided to the motors 18, 20, and 22 which in turn drive the movable arm 12 to a relative position whereat the computer 44 recognizes the position relative to the surface 38 to be the same as that commanded. The speed of such recognition, as well as the overall system speed, is limited by the complex pattern recognition algorithms utilized in the pattern recognizer 42, and the electronic interfaces used for communication between the pattern recognizer 42, the computer 44, and the controller 46. Because of this complexity, the position of the movable arm 12 with respect to the surface 38 can typically be updated at a rate of only about 10-50 times per second. For many applications, this update rate for the adjustment of the position is far too slow.
The slowness and complexity of the prior approaches based on video scanning are believed to stem essentially from the fact that such approaches provide far more information and analysis than required for the operation and control of typical industrial robots by requiring complex pattern matching and analysis. In a typical solution, such detail is not required. Instead, it is desired to maintain the sensor head 30 of the robot 14 in a specified angular orientation with respect to the surface of a workpiece, and at a specified distance from the surface of the workpiece. For many operations, it is not necessary to obtain a complete analysis of the viewable portion of the workpiece, but rather it is necessary only to maintain the specified orientation and distance, and then to move to another location on the surface. That is, the control of orientation and distance is desirably accomplished automatically, independently, and separately, apart from the incremental movement of the sensor head 30 to another location. For example, in many applications it is desirable to retain the same relative orientation and distance of the sensor head 30 from the workpiece surface 38 at all relative positionings as where the robot is operating to weld two workpieces together, or to pain, clean, spray or treat a curved workpiece surface. In such situations and in many others, it is far more efficient to place the relative angular and distance positioning function remotely in the movable arm 12, while providing a separate location incrementing command to the motors 18, 20 and 22, which increments the location of the robot arm with respect to the workpiece surface.
FIG. 3 illustrates the functional approach embodied in the present invention. The movement of the sensor head 30 in relation to a surface 38 is viewed as comprising three components, an orientation control component, a location incrementing control component and a positioning control component. The orientation component is the approximate relation of the sensor head 30 to the surface 38. It is determined by the approxiamte positioning subsystem in a manner to be described below in relation to FIG. 8. The positioning component includes the precise angular orientation of the sensor head 30 to the surface 38, and the precise vertical distance of the sensor head 30 from the surface 38. The location incrementing control component reflects the coordinate position of the sensor head 30 with respect to the surface 38, in the sense that the surface 38 may be viewed as having a set of coordinates defining each point or location on the surface 38. Its value is set externally in a manner to be described in relation to FIG. 8. As indicated, in many operations the positioning component remains constant or follows some simply defined pattern, as for example maintaining the sensor head 30 parallel to the surface 38 and at some fixed distance from the surface 38. The angular and distance commands are provided to a controller 50, which compares the commands to the actual relationship between the sensor head 30 and the surface 38, as determined by the electronic circuitry of the precision positioning subsystem. Utilizing the approach to be described, this comparison can proceed very rapidly and in a parallel processing manner, without the need for pattern recognition of the surface 38. Any deviation from a desired positioning command can be corrected with a positioning control signal provided to the motors 52, and originating in the precision positioning subsystem included in electronic circuitry 48. With the relative positioning of the sensor head 30 thus determined and controlled, the coordinate location may be directly controlled by providing a location control signal to the same motors 18, 20 and 22. It is not necessary to reevaluate location in order to maintain control of distance and angular position, nor need distance and angular position be considered explicitly when incrementing location.
In accordance with the invention, precision positioning of the sensor head with respect to the surface is accomplished by means of absolute and relative time of flight measurements for signals propagated from an emitter toward the surface 38, and return signals received from the surface 38 for at least two signal receivers located on the movable arm 12. The use of two signal receivers allows the determination of distance and relative orientation along a single axis, but the use of three receivers mounted in a non-colinear fashion is preferred, as this approach allows relative determination of angular orientations in two axes, and also the determination of distance. The following description is directed to the use of three receivers, although the principles are equally applicable to the use of two receivers, or more than three receivers.
As illustrated in FIGS. 4-6, the apparatus 10 includes the sensor head 30 and associated electronic signal processing circuitry. The signal head 30 comprises a flat square mounting plate 55 having attached thereto a downwardly facing narrow beam transmitter 56 and three non-colinear narrow beam receivers, a first receiver 58, a second receiver 60, and a third receiver 62, which may be mounted in radial slots to allow radial adjustment. In the illustrated preferred embodiment, the receivers 58, 60, and 62 are located in a triangular arrangement, with the three receivers regularly spaced 120° apart from each other. The transmitter 56 is located generally in the center of the triangle formed by the three receivers 58, 60, and 62, so that the transmitter 56 is located at approximately the average height when the receivers 58, 60, and 62 are positioned at different heights from the surface of the workpiece.
Also in accordance with the invention, sensing of the approximate positioning of the sensor head 30 with respect to the surface 38 is accomplished by the use of four pairs of transmitters and receivers mounted on four lips 100 angularly attached to the mounting plate 55. As illustrated in FIGS. 5 and 6, each of the lips 100 is a rectangular flat plate rigidly joined to the mounting plate 55 at an upward and outard inclination, preferably oriented at about 60° from the plane of the mounting plate 55. One lip is so joined to each side of the square mounting plate 55. A broad beam transmitter 102 and a broad beam receiver 104 are attached flush to the surface of each lip 100. This arrangement provides a forward spherical field of view for the approximate positioning subsystem of about 135°-140° when the transducers 102 and the receivers 104 have a beam angle of about 25°.
Another preferred arrangement of the transducers and receivers in the approximate positioning subsystem is illustrated as a sensor array 106 in FIG. 4. This sensor array 106 comprises an array of transceivers 108, each of which is capable of sending and receiving signals. The transceivers 108 are angularly arrayed so that the entire forward field of view is included within the beams of the transceivers 108 taken collectively. In fact, by extending the array, a greater spherical viewing area is possible, extending to a 360° view if necessary. A multiplexer 110 individually addresses the transceivers either sequentially or randomly, so that a single set of signal generator and analysis logic, to be described subsequently, may be utilized.
All of the transmitters and the receivers described herein are adapted for use of the same general type and frequency of energy, preferably from about 20,000 to about 200,000 cycles per second. Although in theory, any frequency of energy may be utilized, in practicing the invention with the presently available electronic components, it is preferably to utilize energy transmitted in waves travelling at a relatively low velocity, such as acoustic radiation. In the most preferred embodiment, a narrow beam ultrasonic transducer may be utilized for both the transmitter and receiver functions for the forward facing precision positioning subsystem (i.e., the transmitter 56 and the receivers 58, 60, and 62). One acceptable and preferred transducer is the model E-188 transducer available from Massa Products Corporation, Hingham, Mass. This transducer may be driven by a signal generator 64, such as model MP215, available from Metrotech, Inc., Richland, Wash. to emit acoustic waves, or can operate as a receiver to receive acoustic waves. The most preferred transducer for use as the side facing transducers 102 and 104 in the approximate positioning subsystem is a broad beam transducer having a beam angle of about 25°. Two acceptable and preferred transducers are the models V189 and A189R, available from Panametrics, Waltham, Mass.
In the following description of the apparatus and its operation, the components of the approximate positioning subsystem and the precision positioning subsystem are presently separately to maintain clarity. The approximate positioning subsystem provides the orientation component to the drive motors 18, 20, and 22, to bring the sensor head 30 into an approximate facing relation to the surface 38. The approximate positioning subsystem includes the side facing transmitters 102 and receivers 104, and electronic processing components such as illustrated in FIG. 7. The precision positioning subsystem provides the positioning component to the drive motors 18, 20, and 22, to establish precise positioning once the approximate facing relationship has been reached. The pecision positioning subsystem includes the forward facing transmitter 56 and receivers 58, 60 and 62, and electronic processing components such as illustrated in FIG. 8.
In a typical operation to be performed by a robot 14, it is known that a surface 38 will be presented to the robot 14 at some time, but the position and orientation of the surface 38 at the time of presentation are not known with certainty. In particular, it cannot be known whether the surface 38 will be presented so as to be within the field of view of the precision positioning subsystem transducers 56, 58, 60 and 62. The approximate positioning subsystem is therefore provided to sense the presence and general or approximate position of the presented surface 38, and to move the sensor head 30 into an approximate facing relationship with the surface 38, a "facing relationship" being an orientation of the sensor head 30 wherein the surface 38 is within the field of view of the transmitter 56 and the receivers 58, 60 and 62. FIG. 5 illustrates the operation of the transducers 102 and 104 in locating a surface 38 that is outside the field of view of the transducers 56, 58, 60 and 62 of the precision positioning subsystem.
Turning first to the approximate positioning subsystem illustrated in FIG. 7, the orientation of the surface 38 is sensed by determining the side direction form which a response signal is first received. This determination is achieved by using the four broad beam acoustic transmitters 102 mounted on the side lips 100 of the sensor head 30, which continuously transmit acoustic signals under excitation of the signal generator 64, in all directions within their collective spherical 135°-140° field of view. The broad beam acoustic receivers are mounted on the lips 100 in a pairwise fashion, with the receivers 104 used to sense the direction of a responsive signal, if any is found. As illustrated in FIG. 7, a switching logic 120 identifies which receiver is sensing the response signal, if any, thus determining the approximtae orientation of the surface 38 in respect to the sensor head 30. The switching logic 120 then commands a controller 122 to send orientation control signals to motors 18, 20, or 22 to rotate the sensor head 30 in the direction toward which the responsive signal was received The rotation of the sensor head 30 is continued by operating motors 20 or 22 until the signal from the receivers 104 disappears. In this position the sensor head 30, and the movable arm upon which it is mounted, is approximately in a facing relationship to the surface 38, and none of the four receivers 104 on the side lips 100 of the sensor head 30 receive any response signal. Operation of the precision positioning subsystem follows this initial step of bringing the sensor head 30 approximately to a facing relation to the surface 38.
Referring to the precision positioning subsystem illustrated in FIG. 8, the output signals from the receivers 58, 60, and 62 are provided in pair-wise fashion to two comparators 66 and 68. The first comparator 66 determines the difference in the time of flight between the signals produced by the first receiver 58 and the third receiver 62, while the second comparator 68 determines the difference in the time of flight between the signals of the first receiver 58 and the second receiver 60. The output signal of the first comparator 66 is therefore an indication of the difference in the distance from the surface of the workpiece of the first receiver 58 and the third receiver 62, which in turn is an indication of the angular orientation of the axis defined by the first receiver 58 and the third receiver 62.
FIG. 9 represents an exemplary schematic illustration of the interrelationship of some acoustic pulses transmitted to a surface and received by the embodiment illustrated in FIG. 8. It is hypothesized, for the purposes of the illustration presented in FIG. 9, that the emitted signal is received back by the first receiver 58 and the second receiver 60 at the same time, while there is a delay in receipt of the return signal by the third receiver 62. The output signal of the first comparator 66 is proportional to the difference in the time of receipt by the first receiver 58 and the third receiver 62, a value indicated in FIG. 9 as DEL13. While DEL13 is a time value, the corresponding distance may be determined by multiplying this value by the velocity of the acoustic wave in the medium, about 1100 feet per second for acoustic waves in air. From the known length of the baseline between the first receiver 58 and the third receiver 62, and the difference in distance from the surface of the first receiver 58 and the third receiver 62, the angular orientation of the axis defined by the first receiver 58 and the third receiver 62 may be readily calculated. Of course, in most cases an actual calculation is niot required, as the desired time difference values, if any, may be used directly to control the motors.
In a similar fashion, the signals from the first receiver 58 and the second receiver 60 are provided to the second comparator 68, wherein the difference in propagation time of the signal, the difference in distance between the surface and the two receivers 58 and 60, and the angular orientation of the axis defined by the first receiver 58 and the second receiver 60 may be determined in the fashion described above. In the illustration of FIG. 9, it has been postulated that the first receiver 58 and the second receiver 60 are at the same distance from the surface, and therefore there is no difference in the time of receipt of the signals. It is not necessary that a third comparator be provided, inasmuch as the orientation of the sensor head 30 in respect to the surface 38 may be defined fully by the angular displacement of two axes. However, if desired, a third comparator (not illustrated) may be provided as a check against the results determined by the comparators 66 and 68. In other embodiments, only two receivers and a single comparator could be provided if it were desired only to know the angular misorientation along a single axis, such as, for example, where the workpiece is highly elongated and essentially one-dimensional, and the robot has no freedom of movement perpendicular to the workpiece. More than three receivers, and more than two comparators, could also be provided for redundancy and to cross-check the determinations of the primary receivers, or for special applications, wherein the simultaneous orientation with respect to two or more surfaces is desired. Other applications of this approach of time-of-flight triangulation of acoustic signals are also operable, as where the transmitter 56 and receivers 58, 60 and 62 are replaced by three or more transceivers which both send and receive signals. Other non-colinear physical arrangements of the transmitters and receivers may be appropriate for specific applications.
The distance of spacing of the sensor head 30 from the surface 38 may be determined by computing the time of flight of the return signal from the surface 48 to the receivers 58, 60, and 62. If only an approximation is needed, the time of flight from the surface to any one of the receivers may be utilized. If a more precise figure is desired, the following preferred approach may be utilized.
As the signal generator 64 sends a signal to the transmitter 56, the signal is also transmitted to a time delay unit 70, as an indication of the time at which the emitted acoustic signal leaves the sensor head 30. When the return signal is received by the receivers 58, 60, and 62, this signal is provided to an averager 72, which provides an average time of receipt of the return signal to the time delay 70. If the plane containing the receivers 58, 60, and 62 is parallel to the surface, the average value will be identical to each of the individual values. However, if theplane is not parallel to the surface, then the return signals are received at different times. In the hypothetical example of FIG. 9, the first receiver 58 and the second receiver 60 at the same distance from the surface, and their respective times of flight T1 and T2 are identical. The third receiver 62 is at a greater distance, and the time of flight of the acoustic signal is greater. The averaging unit 72 approximates the distance of the center of the triangle defined by the three receivers 58, 60, and 62 from the surface.
The time delay 70 calculates the difference between the average time of receipt of the return signal and the emission time of the acoustic emitted signal. The distance of the sensor head 30 from the surface 48 is then calculated as one-half of the product of the time of flight multipled by the velocity of wave propagation in the medium. Where the transceivers are used both to send and receive the acoustic signals, this ranging logic must be altered slightly. In this case, the averager 72 is placed logically after the time delay 70, to determine an average time of flight for the three signals, this being a measure of the distance of the center of the sensor head 30 to the surface 38.
The output signals from the comparators 66 and 68, and the time delay 70, provide information as to the actual positioning of the sensor head 30 in relation to the surface 38. It is next necessary to compare these actual signals with the desired signals, illustrated as the "Positioning Commands" in FIGS. 3 and 8. Three positioning commands are required, the angular orientation of the axis defined by the first receiver 58 and the third receiver 62, herein termed ANG13, the angular orientation of the axis defined by the first receiver 58 and the second receiver 60, herein termed ANG12, and the average distance of the sensor head 30 from the surface 48, herein termed DIST. These signals are input to a controller 74, which also receives the output signals from the first comparator 66, the second comparator 68, and the time delay unit 70.
The controller 74 comprises three control comparators. A C13 control comparator 76 compares the signal received from the first comparator 66 with the ANG13 positioning command, with the output of the C13 control comparator 76 being a positioning control signal provided to the first rotational motor 20, which rotates the sensor head 30 about the axis 28. Preferably, as illustrated in FIG. 3, the location control signal may be superimposed upon the positioning control signal and the orientation control signal to provide the total command signal to the first rotational motor 20. Similarly, the C12 control comparator 78 compares the signal received from the second comparator 68 with the ANG12 positioning command, and provides a positioning control signal to the second rotational motor 22. A DIST control comparator 80 compares the signal received from the time delay unit 70 with the DIST positioning command, and sends a positioning control signal to the vertical movement motor 18, thereby controlling the spacing or distance of the sensor head 30 from the workpiece surface 38. Location and orientation control signals are also superimposed on the signals from the C12 control comparator 78 and the DIST control comparator 80. The logic of the comparators compensates for simple geometrical effects such as angular misorientations between the rotational axis and the receiver axis.
The switching logic 120 used in controlling the orientation of the robot arm 12 to approximately parallel to the surface 38 is a conventionally used logic module, for example Model No. 54/7400 or 54LS/74LS00 made by Fairchild Corp. Mountain View, Calif. The comparators 76, 78 and 80 are conventional, such as Model Nos. LM139, LM239, LM2901, and LM3302 all of which are made by National Semiconductor Corp. The averager 72 is a Model No. DM502 and the time delay 70 is a Model No. DD501, both made by Tektronix, Inc. Beaverton, Oreg. The controllers 48, 52, and 74 are standard analog voltage regulators consisting of a pulse generator, amplifiers, filters and comparators. The associated electronics incorporates conventionally used circuitry for simplicity and ease of operation; these include amplifier Model Nos. 7B10 or 7B15, function generator Model No. PR505, a digital latch Model No. DL502, signal recognizer Model No. WR501, time mark generator Model No. TG501 and digital counters Model No. DC501, all made by Tektronix, Inc.
The preferred apparatus 10, has the important advantages of the present invention. The electronic hardware components are reliable, commercially available electronic hardware components which do not require any programming or software. All of the electronic components may be placed on a single circuit board. It is therefore possible, and in fact preferable, to locate the orientation and positioning control logic remotely from the main programming controller of the robot 14, as within the sensor head 30 or the movable arm 12. Output of the controller 74 is directly connected to the motors 18, 20, and 22, and does not require any interface to the central controller 82. The presence of such an interface would slow operation of the apparatus 10 significantly. In a sense, the apparatus 10 acts in a manner comparable with that of the human reflex system, wherein it is not required that control signals for reflexive actions pass through the central brain, but such reflexive actions may be superimposed on volational commands to congtrol the muscles. In the present apparatus 10, the orientation and positioning control signals are remotely generated, apart from the location control signals. Updating of the positioning control signal is therefore not dependent upon the cycle time and software structure of the central robot controller 82, and the interface thereto, and therefore can proceed much more rapidly than could prior devices. The rate of updating the positioning control signals is instead determined by the pulse frequency of the signal generator 64 and by the frequency response of the sensors, which is about 20,000 to 200,000 cycles per second.
In a typical robot function, the location control signals are generated by the central controller 82, to move the movable arm 12 to a new coordinate location relative to the workpiece surface 38. At the new location, it may be desired to maintain the sensor head 30 at the same relative angular and spacing positions with respect to the workpiece surface 38, and in this circumstance the positioning commands ANG13, ANG12, and DIST are unchanged. As the movable arm 12 moves to its new commanded coordinate location, the sensor head 30 is automatically repositioned with respect to the surface 38 to maintain the same relative angular and spacing position with respect to the new coordinate location on the surface 38.
If the shape of the surface 38 is regular and varies slowly, the precision positioning subsystem is sufficient to follow the surface and maintain the precise relative position of the sensor head 38. In this instance no orientation control signal is generated by the approximate positioning subsystem. On the other hand, if the surface 38 is irregular and rapidly varying, the approximate positioning subsystem may come into play. The latter is not ordinarily the case, since the short adjustment time of the precision positioning system allows it to follow the surface directly. The approximate positioning subsystem ordinarily comes into operation only when a new surface is presented and the apparatus 10 must locate the surface and establish an approximate facing relation.
The positioning commands may be simply changed by the central controller 82 as the movable arm 12 traverses the surface 38. Significantly, the central controller 82 need not incorporate complex pattern recognition functions as required by prior devices, but instead is concerned only with outputting three location control signals and three positioning commands, and in many cases the three positioning commands remain unchanged. For example, if a workpiece is to be spray painted, the position (i.e., angular relation and distance) of the sensor head 30 (and paint gun, not shown) remain the same, and it is only necessary that the paint gun traverses over the entire surface in this position. It is also possible to automatically map an unknown surface profile with the present apparatus, simply by traversing the movable arm 12 in a controlled fashion, with the positioning control signals set to some constant value, and then automatically recording the positionings of the motors 18, 20, and 22.
It will now be appreciated that the present invention presents a significant advance in the field of robot systems, and particularly in the field of the control of intelligent robots. The present invention allows remote positioning of the movable part of the robot, without prior knowledge or mapping of the surface, thereby significantly simplifying the control functions required of the central robot controller. The robot need not be dedicated to use with a specific part in the sense that a complex pattern recognition program must be written for each new application, but instead it is necessary only to develop traversing command programs to accommodate any of a variety of workpieces. As an example, if the robot is to sandblast a number of different metal castings, it is necessary only to input a command program which ensures that the movable arm traverses over the entire surface of a casting presented for sandblasting. It is not necessary to specify the geometry of the workpiece, as the traversing program can record and recognize when the movable arm has previously traversed the region, and can keep track of the areas traversed until the entire surface has been traversed. During this traversing operation, the present apparatus will maintain the correct positioning of the sandblasting gun at a desired angular inclination and distance for all traversed positions. The acoustic approach of the present apparatus allows the control function to continue, even though visual images might be blurred by the sandblasting process. These principles are equally applicable to many other robot applications, and the scope of the present invention is not to be limited by specific applications discussed herein. Thus, although a particular embodiment of the invention has been described in detail for purposes of illustration, various modifications may be made without departing from the spirit and scope of the invention. Accordingly, the invention is not to be limited except as by the appended claims. | A robot positioning apparatus for use with robot devices having a movable portion, wherein the movable portion may be spatially oriented to, and controllably spaced from, a reference surface. Initial locating of the reference surface is accomplished by an approximate positioning subsystem using multiple, angularly oriented units which send and receive acoustic orientation positioning signals in search of the reference surface. Once a return signal is received, switching logic indentifies the necessary reorienting of the movable portion to achieve approximately the proper facing relationship of the movable portion to the surface. For precise positioning and ranging after the facing relation is established, a precision positioning subsystem emits an acoustic signal toward the surface, and a response signal is received back from the surface by at least two, and preferably three, receivers mounted upon the movable portion of the robot device. A comparator compares the times of flight of the signals received by the receivers on a pair-wise basis, thereby determining the relative distance of the pair of receivers from the surface, which in turn is a direct indication of the spatial orientation of the compared receivers in relation to the reference surface. The signal time of flight from the surface to the receivers is measured as an indicator of the distance of the receivers from the surface. The movable portion of the robot device is adjusted to maintain some predetermined distance and spatial orientation for the signal receivers mounted on the movable portion, thereby orienting the movable portion with respect to the surface in three dimensions. | 1 |
REFERENCE TO RELATED APPLICATION
[0001] This application is related to U.S. Provisional Patent Application Ser. No. 60/749,863 filed Dec. 13, 2005 entitled “Automation Of Testing, Recording, And Determination Of Acceptable Status Utilizing A Dynamic Cone Penetrometer (DCP)”, the entirety of which is incorporated as if set forth in its entirety herein.
BACKGROUND OF THE INVENTION
[0002] Penetrometers and related devices have been used for a variety of geotechnical engineering purposes over the years. Among the well-known types of penetrometers is the utility dynamic cone penetrometer (“DCP”) which is commonly used by utility companies to determine the adequacy and degree of soil compaction in restorations of openings made in roadways or other land features for the purpose of installing or maintaining underground facilities. Other types of DCPs are also presently known to be used in evaluating parameters in addition to soil compaction, including for example resistance to penetration or shear strength.
[0003] Generally, DCPs consist of an elongated shaft having a first and second flange spaced a standardized distance apart with a standardized drop weight conveyed freely there-between on the shaft. The DCP further has a conically shaped tip that is driven into the soil by means of the drop weight being lifted to the height of the first flange and then dropped onto the anvil, or second flange, attached to the shaft. Typically, the drop weight of most DCPs has a standardized mass and a standardized range of movement along the shaft, and thus the driving energy caused by the drop weight striking the anvil is also standardized. In common usage, the operator of the DCP will position the tip of the penetrometer on a soil to be evaluated and with one hand will raise the weight up to the first flange, which is located below a handle provided for steadying the device with the other hand. The weight is then released and permitted to fall freely by gravity. The driving energy generated by the weight hitting the anvil causes the tip of the DCP to move in a downward direction into the soil. Generally, the process of raising and releasing the weight to strike the anvil will be repeated until a standard depth of penetration is established. At that time a record is made of the number of times the anvil has been raised and dropped, as an indication of the relative compactness of the soil. If the required blowcount is reached before the standard penetration is reached, this automatically means a passing condition, and further blows are unnecessary, and not usually pursued.
[0004] The utility DCP is usually used in a go/no-go fashion, in which the number of blows by the drop weight to the anvil to achieve a standard depth of penetration is compared with a predetermined standard: if the number of blows equals or exceeds the standard, the compaction of the soil is deemed adequate. If the number of blows, however, does not meet or exceed the predetermined standard, additional compaction of the soil is performed until the standard is met. Certain soils may require a different criterion; one such is poorly-graded sand, for which the blow-count is determined for a greater depth of penetration, and thus one or more additional gradation lines can be provided on the shaft near the tip to assist in determining appropriate compaction.
[0005] DCPs are generally manual testing devices, relying exclusively on the ability of the user to record test results. Automation approaches by others in the field of soil testing, involve the use of some electronic measuring assemblies attached to the DCP. One such implementation involves a linear variable differential transformer sensor (e.g., an LVDT sensor) that extends from the DCP to the soil. Another implementation, by Applied Research Associates, Inc. (“ARA”) (marketed by Vertek as a Data Acquisition System (“DAS”)), features a portable DAS that utilizes a string potentiometer attached to a hook on the DCP rod anvil in such a way as to monitor the DCP penetration. These presently known automated approaches however are generally cumbersome and fragile and further lack the ability to readily transmit data collected by the DCP to remote data-logging and display devices, such as portable computers or personal digital assistants (“PDAs”) for secure logging and retention of data. Existing automated approaches are also generally unable to effectively display the collected data in real-time or transmit the data by means of wireless transmitters.
[0006] Accordingly, there is a need for an automated device and method to relieve a user of a DCP from the arduous task of keeping track of data manually. It would thus be advantageous to have a device to alleviate the need for the user to manually measure the distance that the DCP has moved during a particular evaluation, and further that would free the user from having to manually count the number of times that the drop weight strikes the anvil. It would additionally be advantageous if such an innovation could determine whether the drop weight of the DCP has been raised to an appropriate position before being released in order to generate the standardized driving force. Such an innovation would ensure that the evaluation being carried out by the DCP is proper and would alert the user when certain drops of the weight were invalid and require repetition of the test. Use of such an automated device and method in connection with a DCP would lessen the likelihood of user error and thus provide a more accurate and reliable assessment of the compaction of soil being evaluated. An automated device and method of collecting data generated by a DCP would further provide a more permanent, secure and tamper-proof record for test data, including, but not limited to, data concerning site location, soil description, lift thickness, and blowcount and depth of penetration patterns.
[0007] Another difficulty in determining soil compaction (and/or other soil properties) is posed by the smaller openings, such as keyhole openings, that have begun to be used by utility companies, and others, in operations that require installation or repair of underground equipment or settings. Keyhole openings are typically smaller than 18-inches in diameter (when circular) or on a side (when rectangular). These openings have become feasible due to the development of tools allowing work to be performed on underground facilities from the surface through tight or enclosed spaces. As operators cannot physically enter such openings, compaction and verification of soil at the bottom of the opening must be performed from the surface above and outside of the so called “keyhole”. The DCPs of the prior art as presently configured cannot be used for this purpose as readings are almost impossible to be made with any accuracy due to the limited sight lines available.
[0008] Accordingly, it would also be desirable to have a device and method to enable use of a DCP in a keyhole or in other applications in which a DCP is to be used to evaluate soil at the bottom of a small opening. It would be further advantageous for such a device and method to be automated in order to simplify the collection, recordation, monitoring and transmission of compaction data generated by the DCP so that it can be evaluated in real-time by the user and others from a remote location, and so that the data can be transferred to and stored at a centralized database for comprehensive record keeping, or transmission to others for analysis.
SUMMARY OF THE INVENTION
[0009] In one embodiment of the present invention, an automated device for processing soil compaction data generated by a dynamic cone penetrometer (“DCP”) is provided. The automated device features a sensor assembly having a distance sensing means, data acquisition means, and a transmitter. The device further includes a display device, a recording device, and a receiver for receiving data from the transmitter. A processing device in communication with the receiver is further provided for processing the data communicated to the receiver and to communicate the processed data to the recording device and the display device.
[0010] In this embodiment, the distance sensing means can be an optical or ultrasonic distance sensor and the processing device can be a handheld computer, a laptop computer, a cell phone or a personal digital assistant (PDA). Further, the transmitter of the automated device can be a radio frequency transmitter, an infrared light transmitter, a Bluetooth signal transmitter or other short range telemetry protocol transmitter.
[0011] Another embodiment of the present invention is directed to a DCP for automated evaluation of soil compaction. In this embodiment, the DCP features an elongated shaft having a first end with a flange and a handle adjacent to the flange and a second end comprising a tip. The elongated shaft may further feature a graduated area having one or more horizontal markings positioned in generally vertical alignment to one another along the length of the shaft near the tip. The flange of the DCP extends in a direction perpendicular to the elongated shaft and an anvil is fixedly mounted between the first and second ends of the elongated shaft. The DCP also features a drop weight slideably mounted to the elongated shaft such that the weight is moveable along the shaft between the flange and the anvil. In this embodiment, an automated device for collecting and processing compaction data from the DCP is also featured. Like the previously described embodiment, the automated device can comprise a sensor assembly having a distance sensing means, data acquisition means, and a transmitter. The device further includes a display device, a recording device, and a receiver for receiving data from the transmitter. A processing device in communication with the receiver is further provided for processing the data communicated to the receiver and to communicate the processed data to the recording device and the display device.
[0012] The DCP of this embodiment can further include an automated system for detecting when the drop weight has been raised into an upper position above the anvil. This system features a weight detection assembly positioned between the first end of the DCP and the anvil and a remote operator assembly having a receiver and an electronic processing device. The detection assembly of the system can further have a detector and transmission element tuned to receive and process compaction data. When the drop weight of the DCP is raised into the upper position, the detector is actuated in a manner which generates a signal that is broadcast by the transmission element to the receiver of the remote operator assembly. The receiver can be adapted to receive the signal broadcast from the transmission element and to transfer the signal to the electronic processing device for processing, display or recording.
[0013] In this embodiment, the detector of the weight detection assembly comprises a switch that is actuated when the drop weight is raised into the upper position. The switch can be an optical distance sensor, an ultrasonic proximity switch or a physically or electrically actuated sensor. Alternatively, if the drop weight of the DCP comprises a magnetic field, the detection assembly can be an inductive sensor that detects when the weight is in the upper position by detecting the magnetic field.
[0014] Another embodiment of the present invention is directed to a DCP for automated evaluation of soil compaction through a keyhole type opening. In this embodiment, a DCP is provided having general features consistent with the DCP of the previous embodiment. The DCP of this embodiment further includes an adjustable collar adapted to fasten around the elongated shaft. The collar is movable on the shaft between the anvil and tip and can have cooperative graduations of comparable dimension to the height of the tip and also the markings of the graduated area on the elongated shaft near the tip. The cooperative graduations of the adjustable collar enable an operator to manually determine how deep the DCP has moved into the soil from outside the keyhole opening by enabling the operator to visually read the graduations against an apparatus placed horizontally across the top of the keyhole opening.
[0015] The DCP of this embodiment can also include at least one elongated shaft extension unit having a first and second ends that are both capable of fastening to the second end of the elongated shaft, the tip, or the first or second ends of another extension unit. The DCP of this embodiment can further be used in connection with a surcharge weight having a top and bottom surface with centrally located openings forming a central cavity that permits the tip and elongated shaft or a shaft extension unit to extend through the weight. An automated device for collecting and processing compaction data from the DCP can further be included in this embodiment, as can an automated system for detecting when the drop weight has been raised into an upper position above the anvil.
[0016] An automated method to collect, record and monitor compaction data generated by a DCP is further provided by one embodiment of the present invention. This method features placing a sensor assembly having an optical distance sensor and transmitter at a fixed position on a soil surface to be evaluated by the DCP. The DCP having a sensor target mounted to the elongated shaft is positioned such that the target is aligned with the assembly in a vertical plane. The distance between the sensor and the target is then detected and streamed as an electronic signal from the transmitter to a receiver mounted to a remote electronic processing device. The streamed signal from the transmitter can then be monitored as a value in real-time at the remote processing device such that the value remains constant where the distance between the sensor and the target does not change. The drop weight affixed to the penetrometer is then raised from a first position adjacent to the anvil to a predetermined second position above the anvil and then is released and permitted to fall under the force of gravity in a direction towards the anvil until the weight contacts the anvil. The contact generated by the weight striking the anvil generates a force that causes the penetrometer to move in a downward direction into the ground surface to be evaluated such that the distance between the target and sensor decreases. When this occurs, the value monitored by the remote processing device changes such that a new value is constantly displayed which corresponds to the new distance between the sensor and the target. The number of times that the value changes is then registered as the number of times that the weight strikes the anvil. The distance that the penetrometer moves after each blow by the anvil is recorded, as is the cumulative distance that the penetrometer has moved during the evaluation. This distance data provides a permanent record which can be viewed by the user or others so that the success or failure of the compaction evaluation can be determined.
[0017] In another embodiment of the present invention, an automated method is provided for detecting when the drop weight has been raised to an appropriate position along the shaft of the DCP. In this method the drop weight of the DCP is raised from a first position adjacent to the anvil to a predetermined second position above the anvil, such that when raised into the second position, the drop weight is in closer proximity to the top flange of the penetrometer. The presence of the drop weight in the second position is detected by a weight detection assembly and an electronic signal indicating that the weight is present in the predetermined second position is generated. The electronic signal is transmitted to a reception element of a remote electronic processing device where a signal, such as for example an audible tone, can be generated in order to alert the user that the weight has been lifted into the second position. The drop weight is then released from the second position above the anvil and permitted to fall under the force of gravity in a direction towards the anvil. The absence of the drop weight in the second position is detected and an electronic signal is generated and transmitted upon release of the weight from the second position.
[0018] Another embodiment of the present invention is directed to a method of using a DCP to evaluate the compaction of soil through a keyhole type opening having an open top. In this method an apparatus having a top and bottom surface is placed across the open top of the keyhole opening. An adjustable collar is affixed to the elongated shaft in a position between the anvil and the tip. The DCP, possibly having one or more shaft extension units to match the height of device to the depth of the keyhole, is then positioned in the keyhole such that the tip of the DCP is resting on the soil surface at the bottom of the keyhole or is buried in the soil to a predetermined initial depth. The collar is then adjusted along the elongated shaft such that its cooperative graduated area can be read against the top surface of the apparatus spanning the opening of the keyhole. The drop weight affixed to the penetrometer is then raised from a first position adjacent to the anvil to a predetermined second position above the anvil and then released and permitted to fall under the force of gravity in a direction towards the anvil. A measurement is then taken to determine how much the DCP moved into the soil.
[0019] While the device and methods of the present invention are ordinary used in connection with evaluations for determining the compaction of various types of soil, persons having ordinary skill in the art will understand that each of the embodiments described herein may be used for alternative purposes, including for example evaluating resistance to penetration or shear strength, without departing from the novel scope of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] FIG. 1 is an elevational view of a Dynamic Cone Penetrometer (“DCP”) of the prior art.
[0021] FIG. 2 is an elevational view of one embodiment of a device made in accordance with the teachings of the present invention, including a sensor assembly for automatically collecting, transferring and monitoring data generated by a DCP.
[0022] FIG. 2A is a top perspective view of one type of sensor assembly of a type shown in FIG. 2 .
[0023] FIG. 2B is an elevational view of an alternative embodiment of a device made in accordance with the teachings of the present invention.
[0024] FIG. 3 is an elevational view of another embodiment of a device made in accordance with the teachings of the present invention; showing the use of a DCP in a “keyhole” application.
[0025] FIG. 4 is an elevational view of a further embodiment of a device made in accordance with the teachings of the present invention showing a device and method for placing and retrieving a surcharge weight and/or sensor assembly from the bottom of a keyhole when the device is used in connection with the embodiment demonstrated in FIG. 3 .
[0026] FIG. 5 is an elevational view of a further embodiment of a device made in accordance with the teachings of the present invention, showing a DCP used in a keyhole application together with an automated device and method where a sensor assembly is placed outside a keyhole opening.
[0027] FIG. 6 is an elevational view of a further embodiment of a device made in accordance with the teachings of the present invention featuring the use of a DCP in a keyhole application together with an automated sensor assembly located within a keyhole opening.
[0028] FIG. 7 is an elevational view of another embodiment of a device made in accordance with the teachings of the present invention featuring the use of a DCP in a keyhole application together with an automated sensor assembly.
[0029] FIG. 7A is a close-up broken elevational view of an insert for placing or retrieving the sensor assembly and/or surcharge weight form a keyhole opening.
[0030] FIG. 8 is a cut-away elevational view showing an automated weight-position detection assembly of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0031] While the present invention is susceptible of embodiment in various forms, there is shown in the drawings a number of presently preferred embodiments that are discussed in greater detail hereafter. It should be understood that the present disclosure is to be considered as an exemplification of the present invention, and is not intended to limit the invention to the specific embodiments illustrated. It should be further understood that the title of this section of this application (“Detailed Description of the Invention”) relates to a requirement of the United States Patent Office, and should not be found to limit the subject matter disclosed herein.
[0032] FIG. 1 shows a dynamic cone penetrometer (“DCP”) 1 having general characteristics in accordance with the teachings of the prior art. Persons having ordinary skill in the art will understand the basic operations of such a device; however, briefly, the tip 2 of the device is generally placed onto the surface of soil “S” whose compaction is to be tested. A weight 3 is raised from the flange, or anvil, 4 on which it rests, up to an upper flange 5 and allowed to drop to its first at rest position. The dropping of the weight causes the cone 2 to penetrate the surface of the soil S. This operation is repeated until the tip 2 , and attached shaft 6 , penetrate the soil to a marked level (such as, for example, as graduated 7 or 8 on the shaft depending on the type of soil being evaluated). The number of drops of the weight to reach this level is recorded and serves as an indication of the compactness of the soil.
[0033] In FIG. 2 , an embodiment of the present invention designed to automatically collect, transfer and monitor the data generated by a DCP 10 is provided. As shown in FIG. 2 , the DCP 10 features an elongated shaft 20 with a handle 21 and flange 22 at one end, and a conically shaped tip 23 at the other end. It will be understood by persons having ordinary skill in the art that while the various parts shown have been described and illustrated as having certain shapes, the actual shapes of the parts, such as “conical”, are merely given for ease of understanding, and that various shapes, sizes and proportions can be interchanged without departing from the novel scope of the present invention. For example, the tip of the device can have any shape that advantageously permits the end of the DCP to penetrate the soil while working, such shapes as generally triangular and others can be substituted therefore.
[0034] The handle 21 , in the illustrative embodiment, is located adjacent to a flange 22 and extends generally perpendicularly about shaft 20 . The DCP 10 also has an anvil 24 and drop weight 25 , having a standardized mass, mounted so that it can ride freely along shaft 20 . The drop weight 25 is slideably mounted to the elongated shaft 20 in a manner that allows the weight 25 to be manually or mechanically raised from a lower position adjacent to the anvil 24 to an upper position proximate to the handle 21 .
[0035] In the present embodiment, the elongated shaft 20 may also have a graduated area 26 to permit the measurement of the depth-of-penetration that is achieved once the tip 23 is driven into the ground surface “S” to be evaluated. The graduated area 26 can feature one or more horizontal markings 27 positioned in generally vertical alignment along the length of the shaft 20 proximate to the conically shaped tip 23 . In normal “go/no go” operation of the DCP, the user is generally interested in determining whether a standard depth of penetration can be achieved by at least a required number of blows by the drop weight. The markings 27 of the graduated area 26 correspond to standard penetration depths of various soil types and are thus provided along the shaft in order to assist the user in determining when a standard depth of penetration has been achieved.
[0036] In use, the DCP 10 of the present embodiment is positioned such that the tip 23 is placed on the ground surface S to be evaluated. Often the initial position of the tip 23 for evaluation is such that the end of the tip adjacent to the shaft 20 is flush with the soil S. This position is usually achieved by initially tapping the weight 25 against the anvil 24 until the tip 23 is sufficiently buried in the soil S. After being raised to the desired upper position, drop weight 25 is released and permitted to fall onto anvil 24 . As will be understood by persons having ordinary skill in the art, the contact between the drop weight 25 and the anvil 24 generates a standardized force that causes DCP 10 to move in a downward direction into the ground surface S to be evaluated. In the present embodiment however, the DCP 10 also features an automated method and device for recording and collecting data generated by this action. As shown in FIGS. 2 and 2 a , the device of the present invention includes a sensor target 30 mounted to the elongated shaft 20 between the anvil 24 and the conically shaped tip 23 , a remote operator assembly 40 , and a sensor assembly 31 mounted within a housing 32 , having a centrally located opening 33 to enable the tip 23 of the DCP 10 to pass through the housing 32 and contact the soil surface S. The present embodiment can additionally feature a surcharge weight 55 that can be incorporated in housing 32 or be a separate item with an opening in approximate vertical alignment with the opening 33 of the housing 32 .
[0037] In the operation of the device of the present embodiment, a weight 25 is raised and dropped onto the anvil 24 of the penetrometer as described above, with respect to the prior art. The sensor 34 records the distance that the DCP 10 is driven into the ground surface S each time the drop weight 25 contacts the anvil 24 , and also measures the cumulative distance that the DCP 10 travels into the ground surface S, during a particular evaluation. The automated data collection method and device of the present invention includes means to collect the distance measurements as well as the number of times the weight 25 strikes the anvil 24 , and also features means to broadcast the data collected to a desired receptor. In operation, therefore, as the penetrometer is used, the sensor 34 collects the measurements as data and then broadcasts the data as an electronic signal to the remote operator assembly 40 for information presentation and results recording.
[0038] It will be seen that the device of the present invention automates the process of independently documenting the number of blows to travel a known distance (instead of relying on the memory of the user). The device further provides additional important and useful information to the user which has previously been unavailable, such as the actual distance traveled per blow (review of which may help to identify uniformity of soil compaction, for example). The device can provide information that can help to independently identify whether a particular soil spot has been compacted to an acceptable level (passes) or not (fails the test). Use of the device can automate the recording of the details of tests providing specific detailed information for an entire construction site or over any operational area covered by a utility or its contractors, for example. Since the data collected by the present invention can be transmitted to a remote display device and can be uploaded, immediately or later, to a computer in a central facility for recording in a database, the results of soil evaluations conducted by the DCP can be made available to more people in less time. Thus personnel working a particular project will be more informed about the condition of soil being evaluated and will be able to make quicker and more informed decisions as to how work on the project should proceed.
[0039] In embodiments of the device of the present invention, an independent time/date stamp for each test can be provided. Further, to insure accuracy, embodiments of the device can be made such that the operator has a limited ability to interfere with or modify test results. The device of these embodiments can therefore limit the interaction of the operator with data collected to thereby better insure that the test details cannot be modified, either purposely or incidentally. In addition, the present embodiment can measure the time that it takes for the drop weight 25 to fall from the raised position to contact the anvil 24 in order to verify that the weight was raised to an appropriate height and that the fall of the weight 25 was unimpeded.
[0040] In some embodiments, the sensor 34 can measure the distance that the tip of the DCP travels into the soil, without being in physical contact with the DCP during operation. Such a system can advantageously protect the sensor device from exposure to the elements, and also the particularly the harsh conditions at a test or construction site. Previous attempts at independent or alternative measurement techniques, in the prior art, have involved equipment requiring actual physical connection or attachment to the DCP. Such prior art devices, as will be understood, are often subjected to harsh conditions permitting devices to bend, break or be otherwise damaged, causing diminution in accuracy or delay in completion of tests.
[0041] As shown in FIG. 2 , the sensor assembly 31 features a transmitter that can relay data and other information about the test to a cooperative unit, such as a receiving unit 40 which is capable of interaction and/or communication with the operator or a computer. In a preferred embodiment, such communication or interaction is accomplished without using wires or other physical communication means that are prone to breakage and are often difficult to use without entanglement.
[0042] It will be understood by persons having ordinary skill in the art that the utilization of a non-contact device and method for incremental and overall distance measurement can eliminate the problems occurring due to having equipment exposed to the impacts and vibrations inherent in the dropping of a weight and its jarring contact with the anvil. The added benefits of automatic recordation of the details of tests, without operator access, provides a more independent verification of the performance of the test and its results.
[0043] The illustrated embodiments also have many benefits over prior systems including: electronic recordation of the cumulative penetration depth and the depth of the DCP after each blow by the drop weight 25 ; systematic recordation of the number of blows by the drop weight; time-stamping of data records; independent verification of data through software algorithms of associated handheld computing devices; and isolation of recordation devices to protect them from vibrations resulting from the drop weight of the DCP.
[0044] It will be seen in FIG. 2 that there are primarily three main components to the automated device of the present embodiment. The first component, as shown in FIG. 2A , is the sensor assembly 31 which consists of: an optical distance sensor 34 having a light source 38 and sensing means 39 ; data acquisition circuitry 35 ; a wireless transmitter 36 and a power supply 37 . The sensor assembly 31 is mounted in a housing 32 that has a centrally located opening 33 to permit the shaft 20 and tip 23 of the DCP 10 to pass through the housing 32 and contact the soil S. As shown in FIG. 2 , the housing 32 is placed directly on the soil to be evaluated.
[0045] The second main component of the automated device is a remote operator assembly 40 . The remote operator assembly 40 consists of a wireless receiver 41 and an electronic processing device 42 , such as a handheld computer or personal data assistant (“PDA”). It will be understood by persons having ordinary skill in the art that any manner of data collection and possessing device can be used here, without departing from the novel scope of the present invention. The wireless receiver 41 , as illustrated, can record the incremental blowcount and distance information transmitted to it from the wireless transmitter 36 of the sensor assembly 31 and forward the information to a processing device 42 . The processing device 42 can include means to present some or all information to the user of the device, such that the efficacy of the test can be determined periodically such that necessary changes or adjustments to the test can be made. The processing device 42 further serves as a data recorder for storing information for observation and reporting purposes. Alternative processing devices such as laptops computers or smart phones having electronic processors, storage units and display screens can alternatively, or additionally, serve as the processing device 42 without departing from the novel scope of the present invention. In addition, alternative means of communications between the sensor assembly 31 and the remote operator assembly 40 can be utilized without departing from the novel scope of the present invention. For example, Bluetooth technology, other short distance telemetry protocols, infrared transmitting and reading devices are contemplated for use in the device and method of the present invention. Further, other technological measuring means, including for example global positioning satellite systems (“GPS”), can be substituted or added to the device of the present embodiment without departing from the novel scope of the present invention. Such GPS systems can provide independent verification of the location of a particular job or soil evaluation and can additionally be used to verify the elevation of the drop weight or DCP in relation to the ground surface.
[0046] The third main component of the automated device of the embodiment shown in FIG. 2 is a sensor target 30 , which in a preferred embodiment can be mounted to the shaft 20 of the DCP 10 . While the sensor target illustrated in FIG. 2 is shown in one particular position on the shaft 20 , those having ordinary skill in the art will understand that the target can be positioned in a number of different locations along the shaft 20 and can be adjustably fastened to the shaft by utilizing, for example, an adjustable collar having a locking pin, bolt or screw. The sensor target 30 allows the sensor 34 to determine the distance that the DCP 10 has traveled by measuring the distance between the sensor 34 and the target 30 . In an alternative embodiment, as shown if FIG. 2B , a sensor 34 having, for example, a laser light source, can be employed to emit a narrow beam of concentrated light in the direction of the anvil 24 , in a manner that enables the light to reflect off of the bottom surface of the anvil 24 , and return to be read by a sensing means 39 configured to read and evaluate such light measurements. In this embodiment, use of the sensor target 30 is unnecessary because a laser light source is of sufficient intensity to be detected by the sensor 34 , after being directed at the more non-reflective bottom surface of the anvil 24 . A sensor target 30 may however be used in connection with the embodiment illustrated in FIG. 2B without departing from the scope of the present invention.
[0047] The present invention additionally provides a method of using the automated device in connection with a DCP 10 . Such a method includes placing the housing 32 having the sensor assembly 31 at a fixed position on the ground surface S that is to be evaluated; positioning a DCP 10 having a sensor target 30 mounted to the elongated shaft 20 , such that the target 30 is above the sensor 34 ; and aligning the sensor 34 in a vertical plane such that the sensor target 30 can be seen by the sensor 34 . The initial vertical position of the DCP 10 can then be measured by detecting the distance between the sensor 34 and the target 30 . This distance data is streamed, as an electronic signal, from the wireless transmitter 36 to the wireless receiver 41 mounted to the remote operator assembly 40 . The electronic processing device 42 then monitors the signal as a value, in real-time, such that the value remains constant where the distance between the sensor 34 and the target 30 does not change. The actual test is then carried out with the DCP 10 by raising the drop weight 25 from a first position adjacent to the anvil 24 to a predetermined second position above the anvil 24 and then releasing the drop weight 25 from the second position to allow the weight to fall to the anvil 24 . The contact of the weight 25 with the anvil 24 generates a standardized force that causes the penetrometer to move in a downward direction into the soil such that the distance between the target 30 and sensor 34 decreases. Optical sensor 34 then detects the new distance between it and the target 30 ; and data indicating the new distance between the two is broadcast by the wireless transmitter 36 to the receiver 41 of the remote operator assembly 40 . The new distance is then transmitted to the electronic processing device 42 where it may be recorded and displayed.
[0048] Changes in the streaming value indicate that a blow has occurred, with the new repeating value representing the next distance; the difference between the new value and the previous value is the distance traveled resulting from the blow. By monitoring the total distance traveled by the DCP 10 and the number of blows made, the soil compaction can be determined. Determination can be made in at least one of two ways. First, by counting the total number of blows to travel a known distance, and comparing the number with the minimum required number for adequate soil compacting. Alternatively, the number of blows can be counted until the minimum required number is reached, and comparing the actual traveled distance to a known distance; a passing result occurring if the actual distance is less than the known distance. In addition, other soil properties may be inferred from a continuous record of blowcount versus penetration.
[0049] FIG. 3 illustrates an alternative embodiment of the present invention, which is intended to enable a DCP 10 to be used to evaluate the compaction of a ground surface S at the bottom of a keyhole opening 50 , or other type of small excavations, where a remote reading from the surface is necessary or desired. The present invention features a DCP 10 having general characteristics as described above, in combination with additional components such as an adjustable collar 51 and/or shaft extension unit 52 . As shown in FIG. 3 , the adjustable collar 51 of this embodiment is adapted to fasten around the elongated shaft 20 of the DCP 10 between the anvil 24 and the second end of the shaft 20 . Once a correct position for the collar 51 is determined, it may be fastened to the elongated shaft 20 in a fixed position by means of a locking pin, bolt or screw 53 such that the collar 51 will not slide down the shaft 20 when the drop weight 25 contacts the anvil 24 during the evaluation. The collar 51 can additionally feature cooperative graduations of comparable dimension to the markings of the graduated area on the elongated shaft near the tip.
[0050] In order to match the DCP 10 of this embodiment to the depth of the keyhole opening 50 , the DCP 10 may additionally include one or more shaft extension units 52 that are capable of being fastened to one another at their ends or alternatively to the elongated shaft 20 or the conically shaped tip 23 . When the appropriate number of shaft extension units 52 are used, it is intended that the DCP 10 will extend outside the opening of the keyhole 50 to such an extent that the adjustable collar 51 can be positioned in a manner that enables a portion of the collar to be in generally horizontal alignment with the opening of the keyhole 50 . When this is accomplished, a bar, plate, or other apparatus 54 having a flat surface, can be placed across the top opening of the keyhole 50 , such that the cooperative graduations of the collar 51 can be read against the top surface of the apparatus 54 spanning the opening. For convenience, the apparatus 54 spanning the keyhole 50 can be perforated to allow the DCP 10 to pass through it; or alternatively, can be positioned adjacent to the DCP 10 such that readings can be taken against the edge of the apparatus 54 . This embodiment can further feature the use of a surcharge weight 55 to assist with the evaluation of compaction of the soil S. The surcharge weight 55 can be part of housing 32 or may be a separate component that can be fastened to the housing 32 or merely used on its own. In use, the surcharge weight 55 can be placed directly on soil S so that a single depth of penetration may be sufficient for more soil types, and a single blow-count criterion may likewise be made more nearly universal. As shown in FIG. 3 , the surcharge weight features a centrally located opening 39 so that the shaft 20 and tip 23 of the DCP 10 are able to pass through the weight 55 and contact the soil S.
[0051] Referring now to FIG. 4 , a device and method of another embodiment of the present invention is shown for enabling a surcharge weight 55 to be placed or retrieved from the bottom of a keyhole opening 50 . In this embodiment, flexible cables 56 of an appropriate length are used to attach the weight 55 to the penetrometer (for instance to the bottom of the anvil), so that the weight 55 hangs slightly below the tip 23 . The cables 56 can be adjusted for various shaft lengths provided by the extensions described earlier. Once the surcharge 55 rests on the surface, further descent of the DCP 10 into the soil will result in slacking of the cables 56 , and thus prevent interference with the DCP 10 operation. Upon completion of the test, withdrawal of the DCP 10 will automatically result in simultaneous retrieval of the surcharge weight 55 . It will be further understood by a person having ordinary skill in the art that other connectors can be used instead of cables 56 without departing from the novel scope of the present invention.
[0052] FIG. 5 illustrates a further embodiment of the present invention featuring the use of DCP 10 in a keyhole application in combination with an automated method and device for recording and collecting data generated by the penetrometer. In this embodiment, the housing 32 , having a sensor assembly 31 , is positioned on top of an apparatus 54 that spans the open top of the keyhole 50 . It will be seen that housing 32 can be placed either directly on top of apparatus 54 or on the top of a surcharge weight 55 positioned on top of apparatus 54 . In this embodiment, an additional surcharge weight 55 can also be positioned on the ground surface S, at the bottom of the keyhole opening 50 .
[0053] In operation of the embodiment shown in FIG. 5 , the user of the DCP 10 positions the adjustable collar 51 such that the cooperative graduations 59 are in general horizontal alignment with the top surface of sensor assembly 31 . Once this initial condition is established, the operator may then begin the evaluation process by raising and releasing the drop weight 25 . While use of the automated data collection device and method of the present embodiment can enable the user of the DCP 10 to collect or evaluate the results of a particular test in full automatic mode, the location of the cooperative graduations 59 on the adjustable collar 51 makes it easy for visual verification to be manually performed as well. In addition, while the reflector plate 30 illustrated in FIG. 5 is shown to be mounted directly to the adjustable collar 51 , this is just one possibility, and those persons having ordinary skill in the art will understand that the reflector plate 30 could be mounted to the DCP 10 without being fastened to the collar 51 without departing from the novel scope of the present invention.
[0054] FIGS. 6 and 7 illustrate additional embodiments of the present invention featuring a DCP 10 used in a keyhole application where the sensor assembly 31 is positioned within the keyhole 50 and proximate to the ground surface S. As shown in FIGS. 6 and 7 , a housing 32 having a sensor assembly 31 can be positioned directly on the soil surface S or can instead be positioned on the top of a surcharge weight 55 positioned on surface S. FIG. 6 additionally shows a device and method for remote placement and retrieval of the housing 32 and/or surcharge weight 55 , similar to those previously described for remote placement and retrieval of the surcharge weight 55 (See FIG. 4 ). In FIG. 6 , the sensor target 30 is fixed to the shaft 20 , or a shaft extension unit 52 , at a suitable height above the tip 23 . At least one flexible connector 56 attaches the housing 32 (and surcharge weight 55 if appropriate) to the sensor target 30 , such that the withdrawal of the DCP 10 from the keyhole 50 will automatically result in simultaneous retrieval of the sensor assembly 31 (and surcharge weight 55 if used). The sensor target 30 thus acts as a point of attachment for the automated device 31 and surcharge weight 55 .
[0055] An alternative method for remote lowering and retrieval of the sensor assembly 31 and/or surcharge weight 55 is shown in FIGS. 7 and 7 A. In this embodiment a flange 57 or insert 58 is fastened to the housing 32 having the sensor assembly 31 . The flange 57 and insert 58 are sized to allow free passage of the shaft 20 or shaft extension unit 52 , but not the tip 23 . Such an arrangement will need to take account of whether the combined height of the housing 31 and surcharge weight 55 is greater or less than the height of the tip 23 . In circumstances where the tip 23 has a greater height than the housing 31 , as shown in FIG. 7A , an insert 58 can be affixed to the flange 57 , in order to accommodate for the height differential. The embodiment illustrated in FIGS. 7 and 7 A thus permits lowering the sensor assembly 31 and/or surcharge weight 55 to the surface, whereupon normal operation of the DCP 10 can proceed. Upon withdrawal of the DCP 10 , the top of the cone 23 will engage with the flange 57 or insert 58 , resulting in simultaneous retrieval of the sensor assembly 31 and/or surcharge weight 55 .
[0056] Another embodiment of the present invention is featured in FIG. 8 . In this embodiment an automated device and method is shown for detecting when the drop weight 25 of a DCP 10 has been raised into the correct position before being released to contact the anvil 24 . As shown in FIG. 8 , the device features a weight detection assembly 60 having a detector 61 and transmission element 62 , and a remote operator assembly 40 having a receiver 41 and an electronic processing device 42 . While FIG. 8 shows a the transmission element 62 and receiver 41 to be connected by a flexible wire for transmission of signals to the receiver 41 , it will be understood by those having ordinary skill in the art that wireless transmission may be used to broadcast a signal from the transmission element 62 to the receiver 41 without departing from the novel scope of the present invention.
[0057] As shown in FIG. 8 , the detection assembly 60 is positioned on the flange 22 of the penetrometer, such that the detector 61 is adapted to sense the presence of the drop weight 25 when the weight is raised to a particular position above the anvil 24 . Once the weight 25 is raised into this position, the detector 61 is actuated and the transmission element 62 broadcasts a signal to the receiver 41 of the remote operator assembly 40 . While it is contemplated that the receiver 41 and electronic processing device 42 of this embodiment are the same as that previously described, a separate receiver 41 and processing device 42 can be used without departing from the spirit or scope of the present invention.
[0058] In the present embodiment, there are a number of different means by which the drop weight 25 can be detected. The first is by physical contact, in which the detector 61 is a switch that is actuated when the weight is raised to a point on the shaft at which the detector is depressed. The switch of the detector 61 may be a momentary electric switch or an optical or ultrasonic-proximity switch that is adapted to sense when the weight 25 is a particular distance away. Alternatively, when the drop weight 25 comprises a magnetic field, the detector 61 can be an inductive sensor that senses when the drop weight 25 is at a particular distance away, by detecting the magnetic field. Such sensing can include, for example, determining the amount of time it takes light or sound energy transmitted by the switch to be reflected off of weight 25 . Further, the use of laser or infra-red technologies can also be employed in connection with this embodiment, without departing from the novel scope of the present invention.
[0059] In the use of the device illustrated in FIG. 8 , a method is provided for automatically detecting the presence of a drop weight 25 that is mounted to a DCP. The method includes raising the drop weight 25 , from a first position adjacent to the anvil 24 to a second position above the anvil 24 ; detecting the presence of the drop weight 25 in the second position by a weight detection assembly 60 ; generating an electronic signal indicating that the weight 25 is present in the second position; transmitting the electronic signal to a reception element 41 , of a remote operator assembly 40 (having for example an electronic processing device 42 ); releasing the drop weight 25 , from the second position above the anvil 24 , such that the weight 25 is permitted to fall in a direction towards anvil 24 ; and detecting the absence of the drop weight 25 in the second position upon the release of weight 25 . The method can further include timing the fall of the drop weight from the second position to the anvil in order to verify that the weight was raised to its proper elevation on the shaft and that it was not interfered with after being released.
[0060] The present disclosure includes that which is contained in the appended claims, as well as that of the forgoing description. Although, this invention has been described in its preferred form with a certain degree of particularity, it is understood that the present disclosure of the preferred form has been made only by way of example, and that numerous changes in the details of the elements, compositions and the combination of individual ingredients may be resorted to without departing from the spirit or scope of the invention. | The present invention includes a device and method for more particularly evaluating the compaction of soil by automating the use of a prior art dynamic cone penetrometer such that user error and error caused by field conditions are eliminated. Recordation of penetrometer data previously not recorded is made more precise by the present invention such that standardized measurement results. The device further includes means for facilitating the determination of compaction of soils through keyhole openings and a means for automating the collection and processing of the generated compaction data. | 6 |
This application claims benefit under 35 U.S.C. §119 of U.S. Provisional Patent Application 60/569,349, filed May 7, 2004, which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a fan usable to create a flow of air in a large space, such as a barn.
2. Related Art
Fans for large spaces, such as warehouses, barns used to house dairy cows and the like, generally have very long blades. One such conventional fan has a 24-foot diameter (approximately 7.3 meters). That is, the fan has blades that extend 12 feet (approximately 3.7 meters) from the axis of rotation of the fan. However, the moving air created by such known fans for large spaces generally is in the form of a cylinder having a diameter that is essentially equal to the diameter of the fan. Thus, to create a larger area in which the air moves, it is necessary to provide larger blades to such conventional fans, thus creating a fan having a larger diameter. This in turn creates a larger cylinder of moving air.
SUMMARY OF DISCLOSED EMBODIMENTS
However, merely increasing the size of the fan blades is problematic. In particular, larger diameter fans require heavier-duty motors and gearboxes to drive the longer fan blades. Larger diameter fans are also heavier, and thus are more difficult to mount, require heavier-duty mounting fixtures, and are more likely to fall. For example, the gearboxes in conventional large diameter fans are prone to failure, such as by the gearbox shafts breaking. Additionally, while conventional large diameter fans for large spaces have safety catch devices, the size of such large diameter fans can overwhelm the safety catch device, causing them to fail.
This invention provides a fan for a large space that has an intermediate length blade.
This invention separately provides a fan for a large space that is able to create moving air in an area that is larger in diameter than the diameter of the fan blades.
This invention separately provides a fan for a large space that creates a generally cone-shaped region of moving air.
This invention separately provides a fan for a large space that has fan blades that are attached to a base structure at locations adjacent to leading edges of the fan blades.
This invention separately provides a fan having relatively shorter blades that can create moving air over an area that is at least as large as an area over which a relatively larger conventional large area fan creates the moving air.
This invention separately provides a fan, having a relatively smaller motor and gearbox compared to a conventional fan for large spaces, that has a similar coverage area.
This invention separately provides a fan, having a relatively similarly-sized motor and gearbox compared to a conventional fan for large spaces, that has a larger coverage area.
This invention separately provides a fan having a safety catch that is sufficient to support the weight of the fan blades and mounting structure.
In various exemplary embodiments of a large area fan according to this invention, the fan includes a plurality of relatively shorter blades connected to a rotating plate. The rotating plate is connected to a shaft of a gearbox. The gearbox is connected both to a motor and to a suspension structure.
In various exemplary embodiments, the fan blades have a relatively straight leading edge portion and a generally curved trailing portion. The blades are attached to the rotation plate by their relatively straight leading edges. In various exemplary embodiments, the relatively straight leading edges lay flat against the rotating plate. The relatively curved trailing portions of the blades extend downwardly from the relatively straight leading edge portion and the rotating plate, and interact with the air to create a conical or cone-shaped flow of air from the fan.
In various other exemplary embodiments, at least a portion of the fan blades are in the shape of a segment of a curve, such as a circle, and are attached to the rotating plate at their leading edges. In various exemplary embodiments, such fan blades are twisted such that one end is offset from the other end of the blades. The blades are attached to the rotation plate with the concave side facing down.
In various exemplary embodiments, the suspension structures include a pole, a channel iron or other device usable to support the fan, fan blades, gear box and motor, a swivel device that allows the fan and fan blades to rotate relative to the pole, channel iron or other device, in case of a failure, a safety catch device, and/or one or more adaptor plates usable to connect the gear box and/or safety catch device to the pole, channel iron or other support device. The support structure is connected to and extends from a wall or ceiling that at least partially encloses the large space for which the fan is employed.
In various exemplary embodiments, as the fan blades according to this invention rotate with the rotating plate, they deflect or displace air. In various exemplary embodiments, some of the displaced air moves downwardly from the fan blades, while some of the displaced air moves radially along the fan blade, in addition to or in place of the downward flow. In various exemplary embodiments, the overall air flow has both radial and axial components, such that the air flow forms a cone-like shape as it leaves some exemplary fans according to this invention.
These and other features and advantages of various exemplary embodiments of the compositions, structures and methods according to this invention are described in, or are apparent from, the following detailed descriptions of various exemplary embodiments of the compositions, structures and methods according to this invention.
BRIEF DESCRIPTION OF DRAWINGS
Various exemplary embodiments of the compositions, structures and methods according to this invention will be described in detail, with reference to the following figures, wherein:
FIG. 1 is a bottom plane view of one exemplary embodiment of a fan including a fan blade hub according to this invention, and a first exemplary embodiment of a fan blade according to this invention;
FIG. 2 is a bottom plan view of the fan of FIG. 1 , showing the first exemplary embodiment of the fan blades and stiffening elements in greater detail;
FIG. 3 is a side perspective view along the first exemplary embodiment of the fan blade according to this invention;
FIG. 4 is a bottom plane view of one exemplary embodiment of the fan shown in FIG. 1 that incorporates a second exemplary embodiment of the fan blade according to this invention;
FIG. 5 is a bottom plan view of the fan of FIG. 4 , showing the second exemplary embodiment of the fan blades and stiffening elements in greater detail;
FIG. 6 is a side perspective view along the second exemplary embodiment of the fan blade according to this invention;
FIG. 7 illustrates the flow of air that occurs when the first exemplary embodiment of the fan blades according to this invention rotate;
FIG. 8 illustrates the flow of air that occurs when the second exemplary embodiment of the fan blades according to this invention rotate;
FIG. 9 is a side perspective view of one exemplary embodiment of a support structure according to this invention;
FIG. 10 is a top perspective view of one exemplary embodiment of a fan hub assembly and the support structure shown in FIG. 9 ; of a fan according to this invention;
FIG. 11 is an exploded view of the mounting plate, safety plate and catches, gear box and support structure of FIG. 10 .
FIG. 12 is a side view of the fan hub assembly and the support structure according to this invention
FIG. 13 is a side view of a first exemplary embodiment of a fan according to this invention when installed in a large space; and
FIG. 14 is a side view of a second exemplary embodiment of a fan according to this invention when installed in a large space; and
FIG. 15 is a top perspective view of one exemplary embodiment of the support structure and the fan hub assembly according to this invention as installed.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
FIG. 1 is a bottom plan view of one exemplary embodiment of a fan 100 , including a plurality of a first exemplary embodiment of the fan blades 110 and one exemplary embodiment of a fan blade hub plate 210 according to this invention. As shown in FIG. 1 , in various exemplary embodiments, the fan 100 includes 12 first exemplary fan blades 110 that extend radially from a fan blade hub assembly 200 . The first exemplary fan blades 110 can be any desired length that is useful in a given application. For many typical applications, each fan blade 110 can be about 4 feet to about 8-12 feet long (approximately 1.2 meters to about approximately 2.4-3.7 meters), or longer, as discussed below. In various exemplary embodiments, the first exemplary fan blades 110 are about 96 inches long and are approximately 3-4 inches wide, but can be any desired width that allows for a generally cone-shaped region of moving air to be created.
As shown in FIGS. 1 and 2 , in various exemplary embodiments, the first exemplary fan blades 110 are attached to the underside of the fan blade hub assembly 200 . In the exemplary embodiment shown in FIGS. 1 and 2 , the first exemplary fan blades 110 are bolted on to a fan blade hub plate 210 of the fan blade hub assembly 200 at two places using bolts 122 and 124 . Alternatively, the first exemplary fan blades 110 can be welded or otherwise suitably attached to the fan blade hub plate 210 using any known or later developed technique. In various exemplary embodiments, a support member or stiffening element 120 is also attached to one side of each first exemplary fan blade 110 . In particular, in the exemplary embodiment shown in FIGS. 1 and 2 , the stiffening element 120 is attached to the underside of each first exemplary fan blade 110 using the bolts 122 and 124 , as well as a third bolt 126 . In this exemplary embodiment, the fan blades 110 are held between the fan blade hub plate 210 and the support members or stiffening elements 120 .
It should be appreciated that, in the exemplary embodiment shown in FIGS. 1 and 2 , the bolts 124 are located about one inch away from the hub end of the first exemplary fan blades 110 and about one inch behind the leading edge of the first exemplary fan blades 110 . The bolts 124 are also located approximately 6-8 inches from the center of the fan blade hub plate 210 . Similarly, the bolts 122 are located about one inch away from the outer edge of the fan blade hub plate 210 and about one inch behind the leading edge of the first exemplary fan blades 110 . It should also be appreciated that, in the exemplary embodiments shown in FIGS. 1 and 2 , the fan blade hub plate 220 is 30 inches in diameter and has a 10-inch-diameter reinforcing plate at its center that is used to attach the fan blade hub plate 210 to the spindle of a gearbox. Thus, it should be appreciated that the preceding discussion is exemplary, and different locations for the bolts 122 and 124 relative to the first exemplary fan blades 110 and the fan blade hub plate 210 can be used for the first exemplary fan blades 110 and/or fan blade hub plates 210 having different dimensions.
In the exemplary embodiment shown in FIGS. 1 and 2 , the support members or stiffening elements 120 are generally rectangular prism shaped and extend approximately ⅓ of the length of the fan blades 110 along the first exemplary fan blades 110 . It should be appreciated that the support members or stiffening elements 120 can be omitted if the first exemplary fan blades 110 are sufficiently stiff enough to create the cone of moving air and to reliably rotate with the fan blade hub plate 210 at the rotational speeds that the large area fan 100 is designed to operate at. In general, this will depend, at least in part, on one or more of: the designed operational rotational speeds of the large area fan 100 , the size of the fan blade hub plate 210 , how the first exemplary fan blades 110 are attached to the fan blade hub plate 210 , the material used for the first exemplary fan blades 110 , the width of the first exemplary fan blades 110 , the design of the curvature of the first exemplary fan blades 110 and/or the length of the first exemplary fan blades 110 .
If the support members or stiffening elements 120 are used, it should be appreciated that such support members or stiffening elements 120 are not limited to the shape and/or dimensions outlined with respect to the exemplary embodiment shown in FIGS. 1 and 2 . That is, the length, width, thickness, and/or location of the first exemplary fan blades 110 and/or their connection to the support members or stiffening elements 120 can be anything that appropriately or sufficiently stiffens the first exemplary fan blades 110 to a desired value. Thus, if less stiffening is desired, the stiffening elements 120 can be shorter, narrower, thinner, made of a less stiff material and/or attached differently to the first exemplary fan blades 110 and/or the fan blade hub plate 210 .
FIG. 3 shows the free end of one exemplary embodiment of the first exemplary fan blade 110 according to this invention. In particular, FIG. 3 shows a first exemplary fan blade 110 that was formed by extruding the fan blade material through a die. In the exemplary embodiment of the first exemplary fan blade 110 shown in FIG. 3 , the leading edge 111 of the first exemplary fan blade 110 can be rounded, flat or blunt, and has a thickness of about 0.15 inches. It should be appreciated that other thicknesses for the first exemplary fan blade 110 can be used as desired, so long as the first exemplary fan blade 110 retains sufficient strength and rigidity to withstand use as a fan blade of the fan 100 .
It should be appreciated that, as shown in FIGS. 1 and 2 , because the first exemplary fan blades 110 are curved, the trailing edge of one first exemplary fan blade 110 can extend over the leading edge of the trailing first exemplary fan blade 110 for the portions of the first exemplary fan blades 110 that are adjacent to the fan hub plate 210 .
In the exemplary embodiments outlined above, the first exemplary fan blades 110 can be obtained by extrusion or by bending a strip of sheet metal around ajig or template to obtain the curved portions 116 of the first exemplary fan blades 110 . It should be appreciated that, using this last process, it is possible to apply different degrees of curvature to the strip of sheet metal as it is bent. Thus, for example, at the hub end 112 that is to be attached to the fan blade hub plate 210 , the curved portion 116 of the first exemplary fan blade 110 could have a relatively smaller amount of curvature (i.e., larger radius of curvature), while at the free end 114 , the curved portion 116 of the first exemplary fan blade 110 could have a relatively greater degree of curvature (i.e., smaller radius of curvature). It should further be appreciated that, when using a first exemplary fan blade 110 formed by bending a sheet of material, the curvature of intermediate portions of the curved portion 116 of the first exemplary fan blade 110 could change continuously and constantly, could change continuously but at different rates at different places along the length of the first exemplary fan blade 110 , could change in discrete but constant steps or could change in discrete but differing step sizes for at least some of the steps, or even combinations of these.
In various exemplary embodiments, the curved portions 116 of the first exemplary fan blades 110 are formed as arc segments of a simple curve, such as a circle, an ellipse, a parabola or the like. In various exemplary embodiments, the curved portions 116 of the first exemplary fan blades 110 are formed as segments of a circle. In various exemplary embodiments, the first exemplary fan blades 110 are extruded using 6005 or 6061 aluminum as a starting material. The extruded first exemplary fan blades 110 can then be heat treated or aged. One exemplary set of heat treating parameters include treating the extruded first exemplary fan blades 110 for 5-9 hours at a temperature of 300°-500° F.
In various exemplary embodiments, the first exemplary fan blades are 110 extruded by first heating up a billet or log of material, such as aluminum or other material, that has sufficient strength and rigidity to be usable as a first exemplary fan blade 110 according to this invention. Such other materials can include other metals, such as iron, steel, copper, alloys of one or more of these or other metals and/or other materials, plastics, such as PVC, suitable thermosetting plastics, ceramics, composites and the like. In general, any material that can be formed into an appropriate first exemplary fan blade 110 according to this invention and that has sufficient mechanical properties that permit that material to survive as a first exemplary fan blade 110 in a fan 100 according to this invention for a suitable length of time can be used to form the first exemplary fan blades 110 .
In exemplary embodiments using aluminum as a starting material, before extruding, the aluminum log or billet is heated at temperatures of about 400°-to about 500° C. (about 750° to about 1000° F.). However, it should be appreciated that this range can be extended in either direction depending on the type of aluminum. Once extruded, the aluminum first exemplary fan blades 110 are relatively soft and malleable. After the first exemplary fan blades 110 are extruded, they are aged or heat treated to reduce their malleability, and to increase their hardness and/or stiffness. In various exemplary embodiments, such as for aluminum first exemplary fan blades 110 , the aging process produces a fine dispersion of alloying materials, such as magnesium and silicon, increases the strength of the extruded aluminum material.
It should be appreciated that the extruded first exemplary fan blades 110 can be of any desired width, with any desired radius of curvature for the curved portions 116 , and have any desired arc length and shape for the curved portions 116 . The shape, size, thickness and radius of curvature depend on the shape of the orifice on the steel die used to form the extruded first exemplary fan blade 110 .
In various exemplary embodiments, the fan blades 110 are formed with the trailing edge having a slight thinning or taper and/or with the leading and trailing edges slightly rounded. Typically, the first exemplary fan blades 110 will be approximately 0.14 inch-0.16 inch thick. However, any desired thickness can be used.
In various other exemplary embodiments, the first exemplary fan blades 110 are cut and formed from a sheet of aluminum. This sheet can have any appropriate thickness and can be cut into any desired shape. The sheet can be cut so that the edges meet at right angles, i.e., square, or can be cut at an angle to create an offset between the ends of the first exemplary fan blades 110 . The cut sheets are then bent around a form or jig at the desired radius for the curved portions 116 . The first exemplary fan blades 110 can then be heat treated or aged as desired to improve or control their mechanical properties.
In various exemplary embodiments, such as that shown in FIG. 3 , the thickness of the first exemplary fan blade 110 gradually decreases from some point at or between a leading edge 111 and a trailing edge 113 . The thickness at the trailing edge 113 is, for example, 0.072 inch and, in various exemplary embodiments, is 35% to 70% of the thickness of the leading edge 111 . In various exemplary embodiments, as shown in FIG. 3 the trailing edge 113 is also rounded.
FIG. 4 is a bottom plan view of one exemplary embodiment of a fan 100 , including a second exemplary embodiment of a plurality of fan blades 150 and one exemplary embodiment of the fan blade hub plate 210 according to this invention. As shown in FIG. 4 , the fan 100 includes 12 second exemplary fan blades 150 that extend radially from the fan blade hub assembly 200 . The second exemplary fan blades 150 can be any desired length that is useful in a given application. For many typical applications, each second exemplary fan blade 150 can be about 4 feet to about 8-12 feet long (approximately 1.2 meters to about approximately 2.4-3.7 meters), or longer, as discussed below. In various exemplary embodiments, the second exemplary fan blades 150 are about 96 inches (approximately 2.4 meters) long and are approximately 4-6 inches (approximately 101.6-152.4 millimeters) wide, but can be any desired width that allows for a generally cone-shaped region of moving air to be created.
As shown in FIGS. 4 and 5 , in various exemplary embodiments, the second exemplary fan blades 150 are attached to the underside of the fan blade hub assembly 200 . In the exemplary embodiment shown in FIGS. 4 and 5 , the second exemplary fan blades 150 are bolted on to the fan blade hub plate 210 at two places using bolts 162 and 164 . Alternatively, the second exemplary fan blades 150 can be welded or otherwise suitably attached to the fan blade hub plate 210 using any known or later developed technique. In various exemplary embodiments, a second exemplary support member or stiffening element 160 is also attached to one side of each second exemplary fan blade 150 . In particular, in the exemplary embodiment shown in FIGS. 4 and 5 , the stiffening element 160 is attached to the underside of each fan blade 150 using the bolts 162 and 164 , as well as a third bolt 166 . In this exemplary embodiment, the second exemplary fan blades 150 are held between the fan blade hub plate 210 and the support members or stiffening elements 160 .
It should be appreciated that, in the exemplary embodiment shown in FIGS. 4 and 5 , the bolts 164 are located about one inch (approximately 25.4 millimeters) away from the hub end of the second exemplary fan blades 150 and about one inch (approximately 25.4 millimeters) behind the leading edge of the second exemplary fan blades 150 . The bolts 164 are also located approximately 6-8 inches (approximately 152.4-203.2 millimeters) from the center of the fan blade hub plate 210 . Similarly, the bolts 162 are located about one inch (approximately 25.4 millimeters) away from the outer edge of the fan blade hub plate 210 and about one inch (approximately 25.4 millimeters) behind the leading edge of the second exemplary fan blades 150 . It should also be appreciated that, in the exemplary embodiments shown in FIGS. 4 and 5 , the fan blade hub plate 220 is 30 inches (approximately 762 millimeters) in diameter and has a 10-inch-diameter (approximately 254 millimeters) reinforcing plate at its center that is used to attach the fan blade hub plate 210 to the spindle of a gearbox. Thus, it should be appreciated that the preceding discussion is exemplary, and different locations for the bolts 162 and 164 relative to the second exemplary fan blades 150 and the fan blade hub plate 210 can be used for second exemplary fan blades 150 and/or fan blade hub plates 210 having different dimensions.
In the exemplary embodiment shown in FIGS. 4 and 5 , the support members or the stiffening elements 160 extend approximately ⅓ of the length along the second exemplary fan blades 150 and taper toward the leading edge of the second exemplary fan blades 150 . It should be appreciated that the support members or stiffening elements 160 can be omitted if the second exemplary fan blades 150 are sufficiently stiff enough to create the cone of moving air and to reliably rotate with the fan blade hub plate 210 at the rotational speeds that the large area fan 100 is designed to operate at. In general, this will depend, at least in part, on one or more of: the designed operational rotational speeds of the large area fan 100 , the size of the fan blade hub plate 210 , how the second exemplary fan blades 150 are attached to the fan blade hub plate 210 , the material used for the second exemplary fan blades 150 , the width of the second exemplary fan blades 150 , the design of the curvature of the second exemplary fan blades 150 and/or the length of the second exemplary fan blades 150 .
If the support members or stiffening elements 160 are used, it should be appreciated that such support members or stiffening elements 160 are not limited to the shape and/or dimensions outlined with respect to the exemplary embodiment shown in FIGS. 4 and 5 . That is, the length, width, thickness, and/or location of the second exemplary fan blades 150 and/or their connection to the support members or stiffening elements 160 can be anything that appropriately or sufficiently stiffens the second exemplary fan blades 150 to a desired value. Thus, if less stiffening is desired, the stiffening elements 160 can be shorter, narrower, thinner, made of a less stiff material and/or attached differently to the second exemplary fan blades 150 and/or the fan blade hub plate 210 .
FIG. 6 shows the free end of one exemplary embodiment of a second exemplary fan blade 150 according to this invention. In particular, FIG. 6 shows a second exemplary fan blade 150 formed by extruding the fan blade material through a die. In the exemplary embodiment of the second exemplary fan blade 150 shown in FIG. 6 , the leading edge 151 of the second exemplary fan blade 150 can be rounded, flat or blunt, and has a thickness of about 0.15 inches (approximately 3.81 millimeters). It should be appreciated that other thicknesses for the second exemplary fan blade 150 can be used as desired, so long as the second exemplary fan blade 150 retains sufficient strength and rigidity to withstand use as a second exemplary fan blade 150 of the fan 100 .
It should be appreciated that, as shown in FIGS. 4 and 5 , because the second exemplary fan blades 150 are curved, the trailing edge of one second exemplary fan blade 150 can extend over the leading edge of the trailing second exemplary fan blade 150 for the portions of the second exemplary fan blades 150 that are adjacent to the fan hub plate 210 .
In the exemplary embodiments outlined above with respect to FIGS. 4-6 , the second exemplary fan blades 150 can be obtained by extrusion or by cutting a pipe of constant curvature into sections. As also outlined above, a third exemplary method for obtaining the second exemplary fan blades 150 is to bend a strip of sheet metal around a jig or template to obtain a curved second exemplary fan blade 150 . It should be appreciated that, using this last process, it is possible to apply different degrees of curvature to the strip of sheet metal as it is bent. Thus, for example, the hub end 152 of the second exemplary fan blade 150 that is to be attached to the fan blade hub plate 210 could have a relatively smaller amount of curvature (i.e., larger radius of curvature), while the free end 154 of the second exemplary fan blade 150 could have a relatively greater degree of curvature (i.e., smaller radius of curvature). It should further be appreciated that, when using a second exemplary fan blade 150 formed by bending a sheet of material, the curvature of intermediate portions of the second exemplary fan blade 150 could change continuously and constantly, could change continuously but at different rates at different places along the length of the second exemplary fan blade 150 , could change in discrete but constant steps or could change in discrete but differing step sizes for at least some of the steps, or even combinations of these.
For second exemplary fan blades 150 that are obtained by cutting an 8-inch (approximately 203.2 millimeters) (nominal) inside diameter pipe into six equal portions, due to the saw blade kerf, the second exemplary fan blades 150 have an arc length of, for example, 58.5 degrees. As indicated above, the ends of the second exemplary fan blades 150 are offset circumferentially. In various exemplary embodiments, for second exemplary fan blades 150 that are approximately 96 inches (approximately 2.4 meters) long, an offset of approximately 1 inch (approximately 25.4 millimeters) is appropriate. This results in the second exemplary fan blades 150 being not quite at right angles between the long and short edges. In various exemplary embodiments, for 96-inch (approximately 2.4 meters) second exemplary fan blades 150 with a one-inch (approximately 25.4 millimeters) offset, the edges meet at 89.4 or 90.6 degree angles.
The support members or stiffening elements 160 can be formed using the same technique as for the second exemplary fan blades 150 . For example, when extruding a 96-inch (approximately 2.4 meters) fan blade, a 96-inch (approximately 2.4 meters) support member extrusion will also be formed. After twisting, and heat treating or aging, the support member extrusion is then cut into three approximately 3, 30 to 32-inch (approximately 762 to approximately 812.8 millimeters) segments. These segments are then cut lengthwise to create at least three support members or stiffening elements 160 .
In various exemplary embodiments, the support members or stiffening elements 160 can be formed by cutting each of the support member extrusion segments roughly in half, roughly along a diagonal of the segment. However, it should be appreciated that the support members or stiffening elements 160 are not necessarily, nor even usually, formed by simply cutting along the diagonal. For example, the support members or stiffening elements 160 can be formed by starting the cut into the segment at one end of the segment and about 20%-25% in from the trailing or leading edge and cutting to the other end through a point that is an approximately equal amount in from the leading or trailing edge respectively.
Assuming that the fan blade extrusion section does not have a tapering thickness towards the trailing edge or smaller feature, the section is thus cut into two equal portions, such that 6 support members or stiffening elements 160 can be obtained from one such extrusion. However, if the extruded second exemplary fan blades 150 have a tapering thickness and/or a rounded or feathered trailing edge, the portions of the segments containing the trailing edge of the extrusion may not be usable as stiffening elements or support members 160 . If not usable, those portions of the segments will typically be discarded s scrap.
Additionally, it should be appreciated that, in the exemplary embodiments shown in FIGS. 4-6 , due to the offset between the ends of the fan blades 150 , the portions of the second exemplary fan blades 150 held against the fan hub plate 210 are held against the fan blade hub plate 210 in a slightly more horizontal position than the position of the portions of the second exemplary fan blades 150 that are distant from the fan blade hub plate 210 . Thus, the second exemplary fan blades 150 tend to present a larger profile to the air at the portions of the second exemplary fan blades 150 that are distant from the fan hub plate 210 . This tends to cause air to spill out of the far end of the fan blades 110 as the second exemplary fan blades 150 rotate with the fan 100 .
In various exemplary embodiments, the second exemplary fan blades 150 are formed as arc segments of a simple curve, such as a circle, an ellipse, a parabola or the like. In various exemplary embodiments, the second exemplary fan blades 150 are formed as segments of a circle. While this circle can have any desired radius, one particularly useful second exemplary fan blade 150 is formed as an approximately 60° arc length segment of an 8-inch (approximately 203.2 millimeters) circle. It should be appreciated that this circle radius is typically measured from the inside surface of the second exemplary fan blade 150 , but could be measured from the outside surface. It should also be appreciated that the second exemplary fan blades 150 can have any arc length that allows for a generally cone-shaped region of moving air to be created.
In various exemplary embodiments, the second exemplary fan blades 150 are extruded using 6005 or 6061 aluminum as a starting material. In various exemplary embodiments, after being extruded, the second exemplary fan blades 150 are twisted along their axis such that the free end of the second exemplary fan blades 150 are offset from the hub ends of the second exemplary fan blades 150 in the opposite direction from the direction of rotation. Any desired amount of offset can be used. However, in general, the larger the amount of offset, the greater the radial air flow will be. The extruded second exemplary fan blades 150 can then be heat treated or aged. One exemplary set of heat treating parameters include treating the extruded second exemplary fan blades 110 for 5-9 hours at a temperature of 300°-500° F.
In exemplary embodiments using aluminum as a starting material, before extruding, the aluminum log or billet is heated at temperatures of about 400°-to about 500° C. (about 750° to about 1000° F.). However, it should be appreciated that this range can be extended in either direction depending on the type of aluminum. Once extruded, the aluminum second exemplary fan blades 150 are relatively soft and malleable. Consequently, the second exemplary fan blades 150 are easily twisted to create the desired offset between the hub and free ends of the second exemplary fan blades 150 . In various exemplary embodiments, the second exemplary fan blades 150 are twisted using a fan blade twisting machine specifically designed for that purpose. However, it should be appreciated that any device usable to twist the second exemplary fan blades 150 according to this invention can be used.
After the second exemplary fan blades 150 are twisted, they are aged or heat treated to reduce their malleability, and to increase their hardness and/or stiffness. In various exemplary embodiments, such as for aluminum second exemplary fan blades 150 , the aging process produces a fine dispersion of alloying materials, such as magnesium and silicon, increases the strength of the extruded aluminum material.
It should be appreciated that the extruded second exemplary fan blades 150 can be of any desired width, with any desired radius of curvature, and have any desired arc length and shape. The shape, size, thickness and radius of curvature depend on the shape of the orifice on the steel die used to form the extruded fan blade.
In various exemplary embodiments, the second exemplary fan blades 150 are formed with the trailing edge having a slight thinning or taper and/or with the leading and trailing edges slightly rounded. Typically, the second exemplary fan blades 150 will be approximately 0.14 inch-0.16 inch (approximately 3.6 to approximately 4.1 millimeters) thick. However, any desired thickness can be used.
In various other exemplary embodiments, the second exemplary fan blades 150 are cut from a sheet of aluminum. This sheet can have any appropriate thickness, and can be cut into any desired shape. The sheet can be cut so that the edges meet at right angles, i.e., square, or can be cut at an angle to create an offset between the ends of the second exemplary fan blades 150 . The cut sheets are then bent around a form or jig at the desired radius. The second exemplary fan blades 150 can then be heat treated or aged as desired to improve or control their mechanical properties. It should be appreciated that, if the sheets are cut square, after bending the square-cut sheet, the resulting second exemplary fan blades 150 can be twisted to offset one end relative to the other using the fan blade twisting machine described above.
In various other exemplary embodiments, the second exemplary fan blades 50 are formed by cutting an 8-inch (approximately 203.2 millimeters) (nominal) inside diameter schedule-10 (6063) aluminum pipe. The outer diameter of the pipe is approximately 8.3 inches (approximately 210.8 millimeters), and the thickness of the pipe is approximately 0.148 inches (approximately 3.76 millimeters). The pipe is cut axially, i.e., along, rather than across, the axis into 6 second exemplary fan blades 150 , with each second exemplary fan blade 150 extending in an arc that is approximately 56-60 degrees wide, depending on the kerf thickness. It should be appreciated that, in various exemplary embodiments, the second exemplary fan blades 150 are not cut straight down the pipe, but cut with a slight spiral, so that the free end of the resulting second exemplary fan blade 150 is off set relative to the hub end. That is, one end of the second exemplary fan blade 150 is offset circumferentially relative to the other end by a small amount. In various exemplary embodiments, this offset is approximately one inch (approximately 25.4 millimeters) along the circumference for a 96-inch (approximately 2.4 meters) long fan blade 150 , although any desired offset amount can be used.
As indicated above, it should be appreciated that the second exemplary fan blades 150 can be formed by appropriately bending a metal sheet of suitable thickness, width and length. For example, an exemplary aluminum sheet that is between 0.1″ and 0.2″ thick can be cut into strips that are between 4 and 5 inches (approximately 101.6 and approximately 127 millimeters) wide and of a desired length. These sheet metal strips can then be bent against a form or jig that imparts one or more suitable curves to the sheet metal strip. In some exemplary embodiments of such a fan blade 150 , this exemplary fan blade 150 , when having the above-outlined dimensions, can have approximately the same shape as the second exemplary fan blades 150 outlined above that are cut from the 8-inch (approximately 203.2 millimeters) (nominal) inside diameter schedule-10 aluminum pipe.
It should further be appreciated that the metal pipe or metal sheet need not be made of aluminum, or even metal. Rather, any other suitable metal, such as iron, steel, stainless steel, copper or the like could be used. Furthermore, any suitable non-metal material, such as plastic, such as PVC pipe, or the like can be used in place of the aluminum pipe or sheet. It should be appreciated that, in general, any material that can reliably withstand the stresses of being used as a first or second exemplary fan blade 110 or 150 in a large area fan 100 according to this invention over a sufficiently long period of time is suitably usable for the fan blades 110 or 150 .
In various exemplary embodiments, such as that shown in FIG. 6 , the thickness of the second exemplary fan blade 150 gradually decreases from some point at or between the leading edge 151 to a trailing edge 153 . The thickness at the trailing edge 153 is, for example, 0.072 inch (approximately 1.83 millimeters) and, in various exemplary embodiments, is 35% to 70% of the thickness of the leading edge 151 . In various exemplary embodiments, the trailing edge 153 is also rounded, as shown in FIG. 6 .
In the exemplary embodiment shown in FIG. 6 , the second exemplary fan blade 150 has a nominal arc length of 60° and a nominal radius of curvature of 4 inches (approximately 101.6 millimeters). Thus, the second exemplary fan blade 150 has a nominal width of 4.19 inches (approximately 106.4 millimeters) (2·4·π/6) at its inner face 156 and a nominal width of 4.34 inches (approximately 110.2 millimeters) (2·4.148·/6) at its outer surface 158 . It should be appreciated that the second exemplary fan blades 150 , if designed for a nominal arc length of 60°, can have actual arc lengths between, for, example, at least about 55° and up to about 65° or more. This occurs at least in part due to the method of manufacturing and the method for offsetting the free end relative to the hub end. For example, when extruding the second exemplary fan blade 150 , the second exemplary fan blade 150 does not need to be exactly 60°. Rather, the second exemplary fan blade 150 can have any arc length that allows a sufficiently conical air flow from the fan 100 . Similarly, when cutting the second exemplary fan blade 150 from an 8-inch (approximately 203.2 millimeters) (nominal) inside diameter pipe, a kerf equal to the thickness of the cutting blade will be lost, which could be up to 1°-2° of the arc width of the second exemplary fan blade 150 . It should also be appreciated that any desired arc length could be used, especially when extruding the second exemplary fan blades 150 .
In the exemplary embodiments shown in FIGS. 1 , 2 , 4 and 5 , the fan 100 includes 12 fan blades 110 or 150 . In general, the fan 100 can use any desired number of fan blades 110 or 150 . However, the fan 100 will typically have at least two fan blades 110 or 150 for balancing purposes. The maximum number of fan blades 110 or 150 will generally depend on the length of the fan blades 110 or 150 , the thickness of the fan blades 110 or 150 , the radial distance, that the ends of the fan blades 110 or 150 lie at on the fan hub plate 210 , and the amount of overlap between adjacent fan blades 110 or 150 , if any. It should be appreciated that, for any given fan blade hub assembly 200 , there will be a maximum fan blade weight that the fan blade hub assembly 200 will be designed to safely support, a maximum amount of torque that a motor and a gear box (discussed below) can safely apply to the fan blades 110 or 150 , and a maximum amount of angular stress that the fan blade hub assembly 200 is safely designed to withstand.
That is, the fan blade hub assembly 200 is typically designed to support a maximum dead weight of the fan blades 110 or 150 . Similarly the fan blade hub assembly 200 is typically designed to output a maximum amount of torque to the fan blade hub plate 210 and thus to the fan blades 110 or 150 . Additionally, as the fan blades 110 or 150 rotate, significant forces are applied to the fan blades 110 or 150 by the air as it is moved by the fan blades 110 or 150 . Due to lever arm action, this force can increase significantly as the length of the fan blades 110 or 150 increases. This force is directly translated to the fan blade hub plate 210 and thus to the gearbox and the motor of the fan blade hub assembly 200 .
In general, due to those factors, a particular fan 100 will have a given blade length that generally should not be exceeded for a given full number of blades that that fan 100 is designed to use. To go beyond this given blade length, a number of the fan blades may be removed and/or the rotational speed of the fan may be decreased. For example, for a 12-blade fan 100 designed to use up to 8-ft fan blades 110 or 150 , to use 12-foot (approximately 3.7 meters) fan blades 110 or 150 , the number of fan blades 110 or 150 may be reduced to 9, 8, 6 or even 4 blades, and/or the rotational speed of the fan 100 may be reduced. In general, the number of fan blades 110 or 150 that are removed should be selected to keep the fan blades 110 or 150 in balance around the fan blade hub assembly 200 .
Similarly, to go beyond this given blade length or to add additional fan blades, the sizes of one or both of the gearbox and/or the motor may be increased and/or the rotational speed of the fan 100 may be decreased. In general, for a given combination of motor and gearbox, the number of fan blades 110 and/or 150 and the rotational speed of the fan 100 can be adjusted to keep the fan 100 operating within the limits of the motor and gearbox. Alternatively, if a particular number of fan blades 110 and/or 150 and a particular fan blade length is desired, a different gearbox and/or motor having larger size(s), which are sufficient for the desired number of fan blades 110 and/or 150 and/or fan blade length, can be used with the fan 100 .
For example, for a 16-blade fan 100 having 8-foot (approximately 2.4 meters) fan blades 110 and/or 150 , i.e., a “17-foot” fan 100 , the fan 100 can use a 2 hp motor and a larger, 70-rpm gearbox. Such a fan 100 having this number and length of fan blades 110 and/or 150 will generally move approximately twice as much air as a fan 100 having 12 8-foot (approximately 2.4 meters) long fan blades 110 and/or 150 . In general, it is possible for a fan 100 according to this invention having 12-foot (approximately 3.7 meters) long fan blades 110 or 150 , i.e., a “25-foot” fan 100 , to have between 6 and 16 blades given the appropriate sizes for the fan blade hub 200 , the motor 250 and the gearbox 230 .
It should also be appreciated that the dimensions of the fan blades 110 or 150 and the fan blade hub plate 210 and the number of fan blades 110 or 150 are not limited to those used in the exemplary embodiments outlines above. In general, there is an inverse relationship between the width of the fan blades 110 or 150 and the maximum number of fan blades 110 or 150 . That is, generally, but not necessarily, as the fan blades 110 get larger or smaller, fewer or more fan blades 110 or 150 , respectively, can be used in a large area fan 100 according to this invention. In general, this relationship will depend in part on the amount of overlap between adjacent fan blades 110 or 150 , which in turn depends on the degree of curvature and/or shape of the fan blades 110 or 150 at the fan blade hub plate 210 , as this generally controls how much overlap there can be between adjacent fan blades 110 or 150 at the fan blade hub plate 210 .
It should also be appreciated that the dimensions of the fan blade hub plate 210 and the locations of the bolts 122 or 162 and 124 or 164 relative to the fan blades 110 or 150 , respectively, and the fan blade hub plate 210 are not limited to those set forth in the above-outlined exemplary embodiments. That is, for example, the fan blade hub plate 210 could be larger or smaller than that outlined above. The fan blade hub plate 210 will generally be sized to securely and reliably hold the fan blades 110 so that the fan blades 110 can be rotated at appropriate rotational speeds to move an appropriate column of air in the large space in which the large area fan 100 is installed.
Unlike traditional fan blades that are shaped like propellers or airfoils, the fan blades 110 and 150 do not push, force or displace all of the air that contacts the fan blades 110 and 150 in a downward direction. Instead, as shown in FIGS. 7 and 8 , due to the concave shape of the fan blades 110 and 150 , respectively, while a not insubstantial portion 130 of the air scooped up by the fan blades 110 is redirected downwardly, another portion 132 of the air begins to travel radially outwardly from the fan blade hub plate 210 along the fan blade 110 . It should also be appreciated that, as the distance of a given portion of a fan blade 110 from the fan blade hub plate 210 increases, the linear (not rotational) speed of that portion of the fan blade 110 in the plane of rotation increases relative to air that is stationary along the plane of rotation. Additionally, with respect to the second exemplary fan blades 150 , because the profile of the second exemplary fan blades 150 becomes increasingly perpendicular to the plane of rotation of the fan blades 110 when moving from the hub end 152 to the free end 154 of the fan blades 150 , the increasingly distant portions of the fan blades 150 scoop out increasing amounts of air, while also acting to better contain the radially-flowing air arriving from the closer portions of the fan blades 110 .
As a result of one or more of these factors, while not in a significant portion 130 of the air contacted by the fan blades 110 and 150 is directed downwardly, a portion 132 of the air moved by the fan blades 110 and 150 is directed radially along the fan blades 110 and 150 . That is, there is a vector flow 142 of air downward from the fan blades 110 and 150 and a vector flow 144 of air radially along the fan blades 110 and 150 . The net effect, due to the sum of these two vector air flows, is a vector flow 140 of air that extends downwardly at an outward angle from the fan blades 110 and 150 , as shown in FIGS. 7 and 8 , respectively. Because the fan blades 110 and 150 sweep out a circle in the plane of rotation, as the downward and outward vector flows 142 and 144 of air from the fan blades 110 and 150 are similarly swept out, the overall flow 140 of air from the fan blades 110 and 150 is in the shape of a truncated cone extending from the plane of rotation of the fan blades 110 or 150 .
That is, the air moved by the fan blades 110 and 150 has both a downward vector 142 and an outward 144 vector, causing the air to move from the fan 100 in the shape of a cone. Accordingly, the fan 100 is able to move air through an area that is larger in diameter than the diameter of a circle swept out by the fan blades 110 or 150 . As a result, relative to conventional fans used to move air in large spaces, the fan 100 can use smaller fan blades 110 or 150 to move air through the same area as a larger fan blade or similar sized fan blades 110 or 150 can be used to move air over a larger area.
It should also be appreciated that, relative to conventional fan blades that are shaped like air foils or like propellers, the fan blades 110 and 150 scoop out and redirect a larger volume of air. Thus, the fan blades 110 and 150 tend not only to move air over a larger area, but also move a larger amount of air.
Thus, it should be appreciated that, depending on one or more of the area to be covered by one or more large area fans 100 according to this invention, the number of such large area fans 100 to be used, and the desired amount of moving air per unit area, the number of such large area fans 100 and/or the amount of offset provided to the fan blades 110 or 150 can be adjusted to increase or decrease the area coverage of each large area fan 100 , the number of large area fans 100 needed to cover a given area and/or the air flow per unit area of coverage to desired values.
In the exemplary embodiments shown in FIGS. 4-6 and 8 , the profile of the fan blade 150 changes to present the width of the fan blade 150 that is at least at an increasing angle to the plane of rotation. In the exemplary embodiments outlined above with respect to FIGS. 4-6 and 8 , this increasing profile is due to the offset or twist applied along the axis of the fan blades 150 . It should be appreciated that, as the amount of offset increases, the rate of change of the profile increases and the maximum amount of change increases. It is believed that this tends to increase the size of the radial vector flow 144 , which in turn increases the angle at which the conical flow 140 leaves the fan blades 150 , relative to the axis of the fan 100 . This tends to increase the area coverage of the large area fans 100 according to this invention.
Referring to FIG. 8 in particular, it should be appreciated that, in the exemplary embodiment described above, the varying profile presented by the fan blades 150 results from the twist in the fan blades 150 . As shown in FIG. 8 , due to this varying profile, portions of the fan blades 150 that are distant from the fan blade hub plate 210 tend to scoop up or collect more air than do the portions of the fan blades 150 that are closer to the fan hub plate 210 .
FIG. 9 shows one exemplary embodiment of a support structure 300 usable with the large area fan 100 according to this invention. The support structure 300 is typically attached at one end to a rafter, a ceiling joist or other structure of the building or other space in which the large area fan 100 is to be located that is capable of supporting the weight and forces of the large area fan 100 .
As shown in FIG. 9 , the support structure 300 includes a channel iron, rod or other long support member 310 that is capable of supporting the weight of the large area fan 100 and that is capable of withstanding the rotational forces generated by the large area fan 100 as it rotates. In the exemplary embodiment shown in FIG. 9 , the support member 310 is a u-shaped channel iron. As shown in FIG. 9 , a sleeve assembly 320 is located near one end of the support member 310 just above a mounting plate 330 that is located at the end of the support member 310 . This mounting plate 330 is typically permanently and securely attached to the support member 310 , such as by welding, bolting and/or the like. The support plate 330 generally will have a number of holes drilled onto it through which the fan hub assembly 200 can be attached using bolts and/or the like.
The sleeve assembly 320 includes an inner sleeve member 324 about which are placed a fixed upper outer sleeve member 322 and a free large rotatable lower outer sleeve member 326 . The inner sleeve member 324 will be securely attached to the support member 310 , such as by welding or the like. It should be appreciated that any known or later developed method for securely attaching the upper outer sleeve member 322 to the inner sleeve 324 can be used. Typically, the outer fixed sleeve member 322 will be securely attached to the inner sleeve member 324 . In various exemplary embodiments, the fixed upper outer sleeve member 322 is welded to the inner sleeve member 324 . In various exemplary other embodiments, the fixed upper outer sleeve member 322 is glued or otherwise adhered to the inner sleeve member 324 . It should be appreciated that any known or later developed method for securely attaching the upper outer sleeve member 322 to the inner sleeve 324 can be used.
The lower outer sleeve member 326 typically contains two or more eye bolts or the like that allow guy wires to be attached to the lower outer sleeve member 326 and to support points on the building enclosing the large space in which the large area fan 100 is mounted. The sleeve assembly 320 and the guy wires act to stabilize the position of the bottom of the support structure 300 and the attached fan blade hub assembly 200 . The lower outer sleeve 326 and the guy wires attached to it allow the support structure 300 to rotate around its axis without stretching or otherwise straining or stressing the guy wires. This will be described in greater detail below.
FIG. 10 shows one exemplary embodiment of a fan hub assembly 200 according to this invention, as attached to the exemplary embodiment of the support structure 300 showing FIG. 9 . As shown in FIG. 10 , the fan hub assembly 200 includes the fan plate 210 , a safety and mounting plate assembly 220 , a gear box 230 and a plurality of safety catches 240 . FIG. 11 shows these elements of the fan hub assembly 200 in an exploded view that allows the details of these elements to be seen in greater detail.
As shown in FIGS. 10 and 11 , the fan blade hub plate 210 includes a center mounting plate 212 and a mounting collar 214 . The mounting collar 214 includes a mounting screw set screw or the like 216 that extends through the thickness of mounting collar 214 . In various exemplary embodiments, the mounting collar 214 is welded or otherwise securely attached to the mounting plate 212 , which is in turn, welded or otherwise securely attached to the fan blade hub plate 210 . In various exemplary embodiments, the mounting collar 214 can have a constant thickness or can have a trapezoidal cross section such that the thickness of the mounting collar 214 are thicker near the mounting plate 212 and are thinner away from the mounting plate 212 . In various other exemplary embodiments, the mounting collar 214 and the mounting plate 212 can be machined from a single piece of metal or the like. It should be appreciated that, when the mounting collar 214 is welded or otherwise attached to the mounting plate 212 , stabilizing bars extending at an angle from the outer surface of the mounting collar 214 to the mounting plate 212 can be used to provide additional stability between the mounting collar 214 and the mounting plate 212 .
As further shown in FIGS. 10 and 11 , a series of mounting holes 218 are located around the edge of the fan blade hub plate 210 , while a second series of mounting holes 219 are located around the mounting plate 212 . It should be appreciated that the bolts 222 and 224 respectively will pass through the bolt holes 219 and 218 , respectively. As shown in FIGS. 10 and 11 , in various exemplary embodiments, a pair of inner and outer bolt holes 218 and 219 for a particular fan blade 110 or 150 need not be arranged along a radius of the fan blade hub plate 210 . Rather, as shown in FIGS. 10 and 11 , a single set 217 of the bolt holes 218 and 219 are located such that a particular fan blade 110 or 150 does not lie along a radius of the fan blade hub plate 210 . Rather, a given fan blade 110 or 150 is attached to the fan blade hub plate 210 using the bolt holes 218 and 219 such that the free end 114 or 154 of the fan blade 110 or 150 respectively, is slightly ahead of the hub end 112 or 152 , respectively, along the circumferential direction of the large area fan 100 .
As shown in FIGS. 10 and 11 , the mounting and safety plate assembly 220 includes a mounting plate 222 and a safety plate 224 . As most easily seen in FIG. 11 , the mounting plate 222 includes a first set of bolt holes that align with bolt holes on the mounting plate 330 of the support assembly 300 . A second set of bolt holes on the mounting plate 220 align with bosses provided on the gear box 230 . As shown in FIG. 11 , a fairly large hole is formed in the center portion of the safety plate 224 . As shown in FIG. 10 , when the fan blade hub assembly 200 is assembled, the mounting collar 214 extends through the hole in the safety plate 224 .
As shown in FIGS. 10 and 11 , the gear box 230 includes an output drive shaft or spindle 232 and an input mounting plate 234 . When the fan blade hub assembly 200 is assembled, the output drive shaft or spindle 232 extends through the center opening in the safety plate 224 when the mounting plate 220 is bolted to the gear box 230 . The drive shaft or spindle 232 , along with the mounting and safety plate assembly 220 , is connected to the fan blade hub plate 210 by extending the drive shaft or spindle 232 into the center portion of the mounting collar 214 and tightening the mounting screw 216 . In various exemplary embodiments, the drive shaft or spindle 232 will have a matching hole into which the mounting screw 216 will extend. It should be appreciated that, in various exemplary embodiments, this hole on the spindle 232 can be either threaded or unthreaded.
As shown in FIGS. 10 and 11 , a series of safety catch plates 240 are mounted to the fan blade hub plate 210 and extended up and over the top surface of the safety plate 224 of the mounting and safety plate assembly 220 . As shown in FIG. 10 , pairs of mounting holes 242 on the safety catch plates 240 align with two of the mounting holes 219 on the fan blade hub plate 210 . In general, the bolts 222 are sufficiently long enough to extend through the fan blades 110 or 150 , the fan blade mounting plate 210 and the bolt holes 242 of the safety catch plate 240 to allow the safety catch plates 240 to be securely attached to the fan blade hub plate 210 . In normal operation, the safety catch plates 240 rotate with the fan blade hub plate 210 , with their inter-projecting portions 244 extending over but not contacting the safety plate 224 . However, should the drive shaft or spindle 232 fail, the mounting collar 214 and/or the mounting plate 212 become detached from the fan blade hub plate 210 and/or the spindle 232 slip out of the mounting collar 214 , rather than the fan blade hub plate 210 and all of the attached fans 110 crashing to the ground, the projecting portions 244 of the safety catch plates 240 will catch or hang on the safety plate 224 . Thus, the safety catches 240 , in combination with the safety catch plate 224 , prevent mounting failures between the gear box 230 and the fan blade hub plate 210 from resulting in catastrophic failure of the large area fan 100 .
Accordingly, it should be appreciated that the safety catches 240 be sufficiently strong enough to support the weight of the fan blade hub plate 210 and the attached fan blades 110 or 150 and that the bolts 122 and 162 be sufficiently strong enough to support the weight of the fan blade hub plate 210 , the hub assembly 200 and the fan blades 110 or 150 , respectively. Likewise, the safety plate 224 needs to be sufficiently strong and rigid enough to support the weight of the fan blade hub plate 210 and the fan blades 110 or 150 . Similarly, the connection between the mounting plate 222 and the safety plate 224 and the bolts connecting the mounting plate 222 to the mounting plate 330 need to be sufficiently strong enough to support the weight of the fan blade hub plate 210 and the attached fan blades 110 or 150 .
FIG. 12 is a side view in part cross sectional view of the assembled support structure 300 and fan blade assembly 200 showing the spatial relationships between the fan blade hub plate 210 , the safety catches 240 , the safety plate 224 and mounting plate 222 , the drive shaft or spindle 230 and the mounting collar 214 , along with the bolts 122 or 152 and the various bolts connecting the mounting plate 222 to the gear box 230 and to the mounting plate 330 .
FIG. 13 shows a first exemplary embodiment for mounting one exemplary embodiment of a large area fan 100 and fan blades 110 according to this invention inside a building having a large area to be covered by the large area fan 100 . As shown in FIG. 9 , the building 400 has a ceiling rafter or joist 410 to which the support structure 300 is mounted. The building 400 also has electric service 420 apprising a first conduit 422 leading to a junction box 426 and a flexible wiring element 424 extending from the junction box 426 and extending down the support member 300 to a motor 250 of the fan blade hub assembly 200 . As shown in FIG. 13 , a number of guy wires are attached to the lower outer sleeve 326 of the sleeve assembly 300 . In the exemplary embodiment shown in FIG. 13 , the large area fan is mounted such that the fan blades 110 are more or less parallel to the floor of the building 400 .
FIG. 14 shows a second exemplary embodiment for mounting one exemplary embodiment of a large area fan 100 and fan blades 150 according to this invention inside a building having a large area to be covered by the large area fan 100 . As shown in FIG. 14 , it should be appreciated that the support structure 310 can be attached to the rafter 410 or the like in a way that tilts the fan blades 150 (or 110 ) relative to the floor of the building 400 . In various exemplary embodiments, the tilt is typically on the order of about 5° to about 10°. By tilting the larger fan 100 , the large area fan 100 can be located further to one side of the building 400 , that is, away from the center line of the building 400 . When the large area fan 100 is tilted, and placed off to one side of the building 400 , in operation, the large area fan 100 is still able to generate sufficient air movement to cover the entire width of the building 400 .
FIG. 15 illustrates one exemplary embodiment of the guy wires 350 and the sleeve assembly 320 of the support structure 300 . As shown in FIG. 15 , a number of attachment points or eyelets 328 are mounted on the outer surface of the lower outer sleeve member 326 . A plurality of guy wires, each comprising a wire 352 , a turnbuckle 354 and a hook 356 are attached to the attachment points or eyebolts 328 .
As suggested above, as the fan blades 110 or 150 of the large area fan 100 rotate, a significant torque or rotational force is transmitted from the fan blades 110 or 150 through the fan hub assembly 200 to the support structure 300 . When the fan blades 110 or 150 are rotating in a forward direction, this force is a backwards torque due to the mass of the air being moved by the fan blades 110 or 150 and the distribution of that mass along the fan blades 110 or 150 , as well as the drag generated as the fan blades 110 or 150 move through the air in the large space in which the large area fan 100 in placed. In general, this force will generally gradually build up when the large area fan 100 is first turned on and will generally gradually dissipate once the large area fan 100 is turned off.
However, in various situations, the large area fan 100 may experience an immediate or abrupt loss of power. This can occur due to a loss of power due to a storm or other power outage, a circuit breaker tripping due to a short circuit condition, a power surge or the like, a gearbox failure, a motor failure, or the like. In any case, the large area fan 100 may experience a situation where the fan blades 110 or 150 come to a stop in a very short amount of time. While the fan blades 110 or 150 may immediately stop moving relative to the fan blade assembly 200 , due to the large amount of rotational energy stored in the fan blades 110 or 150 , the fan blades 110 or 150 will typically continue to rotate relative to ground, slightly causing the support member 310 to twist on its axis.
The sleeve assembly 320 allows the support member 310 to twist without putting any additional stress or strain on eyebolts 328 , the guy wires 352 , the turnbuckles 354 and/or the hooks 356 . Without the sleeve assembly 320 , it is possible that this twisting of the support member 310 could stretch one or more of the guy wires 352 and/or break one or more of the eyebolts 328 , the guy wires 352 , the turnbuckles 354 and/or the hooks 356 .
In various exemplary embodiments, the gear box 230 is a 90 degree angle worm gear box, which may or may not include an integral motor. It should be appreciated that, while the fan blades 110 or 150 may put less strain on the gearbox 230 and/or motor 250 than a conventional large area fan, the gearbox 230 and the motor 250 nonetheless must be of sufficiently high duty. The applicant has determined that light duty gear motors, such as the Emerson 45-rpm 3N176 gear motor will experience 50% or more failures within one year of operation. The applicant has determined that heavier duty gear boxes and separate motors, such as a 1 hp Leeson motor and a Boston 44-rpm IL364 gearbox will withstand over one year of normal use without failure.
While this invention has been described in conjunction with the exemplary embodiments outlined above, various alternatives, modifications, variations, improvements, and/or substantial equivalents, whether known or that are or may be presently unforeseen, may become apparent to those having at least ordinary skill in the art. Accordingly, the exemplary embodiments of the invention, as set forth above, are intended to be illustrative, not limiting. Various changes may be made without departing from the spirit and scope of the invention. Therefore, the invention is intended to embrace all known or later-developed alternatives, modifications variations, improvements, and/or substantial equivalents. It should also be appreciated that, in the above description, dimensions have been given in English units with approximate metric equivalents. Where present, the metric units are approximations and are not intended to be further limiting than the previously stated English units. | Conventional large area fans generally create a cylinder of air having a diameter that is essentially equal to the diameter of the fan. Larger diameter fans require heavier-duty motors and gearboxes to drive the longer fan blades and are heavier, and thus are more difficult to mount, require heavier-duty mounting fixtures, and are more likely to fall. One large area fan according to this invention forms a cone of air. Some fan blades according to this invention have a relatively straight leading edge portion attached to the fan and a generally curved trailing portion extending downwardly from the relatively straight leading edge portion that interacts with the air to create a conical or cone-shaped flow of air from the fan. Other fan blades have a curved segment and are attached to the fan at theirs leading edges. In some such fan blades, one end is offset from the other end. | 5 |
FIELD OF THE INVENTION
This invention relates to conductive polymeric strip heaters, and particularly to end seals for such heaters.
SUMMARY OF THE PRIOR ART
In the past several years, conductive polymer based strip heaters (i.e. heaters which are relatively long and thin) have achieved considerable popularity for "heat-tracing" and similar functions. One of their notable advantages over their alternatives, which include steam lines and resistance wire heaters, is their simplicity of installation and use. Because the heating effect is produced by the passage of current through a conductive polymeric composition between electrodes which run the length of the strip, the heater produces a certain output of heat per unit length, and this output is essentially independent of the total length of the heater. Thus the heater may be simply cut to the appropriate length for the desired use, and the electrodes attached at one end to the power supply by means of lead wires, etc.
The basic requisite for the other end of the heater is that a new conducting path (i.e. one which does not pass through the conductive polymer) should not develop between the electrodes. If such a conducting path does develop, the heater may short-circuit or an arc or fire may develop at the end of the heater (the fire is sometimes known as a wet wire fire, since it may readily occur if the heater end is wet with an electrolyte).
The most severe short-circuit problem will occur if the electrodes at the cut end of the heater are allowed to come into contact, and it is thus normal practice to cut off the end of the heater in such a way that the electrodes do not protrude beyond the conductive polymeric layer. This may normally be done simply by a cut perpendicular to the heater axis with a sharp-edged cutting tool.
However, even if this drastic short-circuit is eliminated, the problem of wet wire fires remains of considerable importance.
The conventional approach to the problem has been to attempt to prevent an electrolyte from coming into contact with the cut end. This has usually been achieved by some sort of enclosing of the cut end, as for example by:
(1) enclosing the cut end in an end cap containing a gasket which surrounds the heater and is compressed against it to provide a mechanical seal;
(2) potting the cut end in a curable adhesive, such as an RTV silicone, usually enclosed in an end cap of compatible material; or
(3) recovering over the cut end a heat shrinkable plastic end cap, usually containing a hot-melt or thermoset adhesive.
These prior art methods are, while in general satisfactory for most applications, susceptible to problems, especially when the heater is to be used as an immersion heater.
Problems with the mechanically closed (gasket) end cap include degeneration of the seal between cap and heater and leak development within the cap itself.
Problems with the potted or heat shrinkable end cap include particularly those of compatability between the various materials, i.e. the conductive polymer, the jacketing of the heater, the potting or adhesive compound, and the material of the end cap itself. Differences in these materials make it relatively easy for microscopic leak paths to develop at the interfaces.
Furthermore, if a pinhole should develop in the jacket of the heater outside the end cap or water should be able to enter the other end of the heater, it is possible that an electrolyte leak path could develop down to the end by capillary action.
With these problems in mind, it is desirable to develop an apparatus and method for end sealing strip heaters that will render them less susceptible to short circuits, arcing, and wet wire fires; especially when the heater is to be used as an immersion heater.
DESCRIPTION OF THE INVENTION
Summary of the Invention
I have discovered that if the metallic electrodes of the cut end of a strip heater are shielded from possible contact with an electrolyte by treatment of the cut end so that the conductive polymeric heater material is extruded over the ends of the electrodes, then the probability of short-circuits, arcing, and wet wire fires may be substantially decreased.
BRIEF DESCRIPTION OF THE DRAWING
FIGS. 1A, 1B and 1C show, in cross-section, some examples of strip heaters employing conductive polymers.
FIG. 2 depicts, in plan, an example of an end seal according to this invention while FIGS. 3A through 3H show cross-sections of that seal.
FIGS. 4A and 4B are schematic views of a tool suitable for the end sealing of a strip heater by the method of this invention, while FIGS. 5A and 5B show the seal formed.
DETAILED DESCRIPTION OF THE INVENTION
It has been discovered that, when the conductive polymeric material of a strip heater is extruded to cover the ends of the metallic electrodes, the incidence of electrical problems may be decreased.
A strip heater comprises at least two electrodes, which are generally metallic, and which are embedded in a conductive polymeric material. Such heaters are well-known. FIGS. 1A, 1B and 1C show, in cross-section, some examples of strip heaters. In FIG. 1A, the heater is of approximately circular cross-section; in FIG. 1B it is flat; and in FIG. 1C, it has a narrower central section, usually known as a "dog-bone". In each case, the heater shown generally at 10 comprises electrodes 12, a conductive polymeric composition 14, and an insulating plastic jacket 16. Further jacketing, or reinforcing braid, or both, may overlay the jacket 16 if required, but such has not been shown. My invention is applicable to strip heaters of almost any configuration, though the tool used to perform the sealing will, of course, vary in configuration with the heater to be sealed, as will become obvious from the specification.
Further, although the electrodes have been depicted as being metallic and of circular cross-section, it is to be understood that my invention is applicable to other electrode configurations or materials.
FIG. 2 depicts, in plan, an end seal according to this invention formed in a strip heater of the configuration shown in FIG. 1B. FIGS. 3A through 3H depict a series of cross-sections through the seal of FIG. 2. Though the details of FIGS. 2 and 3A through 3H relate specifically to the configuration of FIG. 1B, it will be understood that the essential feature of this invention, i.e. the extrusion of the conductive polymer over the ends of the electrodes, is merely illustrated by FIGS. 2 and 3, and no limitation to a particular configuration of strip heater is intended.
In FIG. 2, the strip heater shown generally at 10 has been sealed inside on end cap shown generally at 20 which comprises a polymeric cap 22 lined with an adhesive 24. The provision of the end cap 20 over the seal of this invention is a preferred feature.
To provide conductive polymeric material sufficient to cover and seal the ends of the electrodes, polymeric material from between the electrodes is extruded toward the end of the heater. The extrusion illustrated in FIGS. 2 and 3A through 3H is produced by a wedge-shaped die section which produces the indentation shown generally at 26 in the sealed end.
The extent of the extrusion necessary, and the precise die shape to produce the extrusion, will depend on the cross-sectional shape of the heater. For example, when the heater has the cross-section of FIG. 1A, there will be a relatively greater amount of conductive polymer available for extrusion, and a simple crushing of the end under heat and pressure may well prove sufficient. It is also within the contemplation of my invention that the extrusion may be augmented by the provision of a separate piece of polymeric material, especially one compatible with, or identical to, the conductive polymer, at the end of the heater before extrusion occurs. This piece will preferably, under the extrusion conditions, bond to the extruded conductive polymer to augment the seal.
FIGS. 3A through 3H depict a series of cross-sections through FIG. 2. FIG. 3A, a cross-section through line A--A of FIG. 2, is a cross-section of the heater 10 alone, showing electrodes 12, conductive polymer 14, and jacket 16. FIG. 3B shows the beginning of the capped seal, and includes adhesives 24 and cap 22. FIG. 3C is a cross-section through the area of the indentation 26. As can be seen, in the region of the indentation, conductive polymeric material 14 has been extruded, narrowing the cross-section of the heaters. FIGS. 3D and 3E are further cross-sections comprising the indentation 26. FIG. 3F is a section beyond the end of the heater, where the conductive polymer 14 has been extruded by the indentation 26 beyond the end of the electrodes. It is this extrusion and the consequent sealing of the electrode ends, that is the essence of my invention. FIG. 3G is a section beyond the extruded conductive polymer, and shows adhesive 24 and the cap material 22; while FIG. 3H is a section through the cap material 22 alone.
The wedge-shaped indentation 26 in FIGS. 2 and 3A through 3H is particularly advantageous in that it aids in retention of the heater within the sealing tool during the sealing process, but this is not an essential feature of the invention.
The extrusion process to produce the end seal is generally performed at a temperature above the melting point of the conductive polymer material, and that of any additional piece of polymer which may be present to augment the seal. The temperature and pressure required for adequate extrusion will be readily determined by one skilled in the art in view of this disclosure.
FIG. 4 illustrates schematically the tool used to produce the end seal. In them, and in FIGS. 5A and 5B, which illustrates the sealed heater end, no cap or adhesive are shown, though they may be present if desired. The jacket of the heater has also been omitted for clarity. In FIGS. 4A and 4B, a heater shown generally at 10 has been inserted into the tool, which comprises heated dies 30 and 32. Means for heating the dies and for applying pressure to them to cause the extrusion have not been shown. FIG. 4A shows the dies and heater in side view, while FIG. 4B shows them in end view, in each case with the dies apart. The dies 30 and 32 are then closed about the heater 10 so that heat and pressure are applied to the heater to extrude the conductive polymer.
FIGS. 5A and 5B illustrate the resulting configuration of the sealed end, with FIG. 5A being a side view and FIG. 5B an end view.
The sealing and capping of the end of the heater may be performed sequentially or simultaneously, as desired. It is presently considered preferable to perform them sequentially in that the end sealing may be inspected before the seal is covered by the cap.
Having described my invention in detail with respect to certain preferred embodiments and illustrations, it is to be understood that my invention is not limited to these illustrations, but its scope is to be determined solely by the claims. | A method and apparatus for sealing the end of a conductive polymeric strip heater, especially one for immersion use, greatly reduces the possibility of failure due to fluid ingress. | 7 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 60/906,848 filed on Mar. 14, 2007 titled “POROSITY STORAGE RESERVOIRS UTILIZING FLOODPLAIN BANKS FOR PARTIAL ENCLOSURE” which is incorporated herein by reference in its entirety for all that is taught and disclosed therein.
BACKGROUND
Technical Field
[0002] The invention relates generally to storing water in underground reservoirs and, more particularly, to a method for storing an isolated supply of water in the voids found in numerous alluvial deposits.
[0003] It is becoming increasingly difficult, both in terms of cost and availability, to construct conventional open reservoirs for the storage of water. Such reservoirs typically require the construction of a dam across a river, thereby flooding vast expanses of land upstream of the dam while severely curtailing the flow of water downstream from the dam. In light of the increasing value of water and the complexities of the various water laws across different jurisdictions, it is becoming prohibitively difficult to form an open reservoir in this manner. Open reservoirs may also be formed by first mining a large gravel pit and then filling the pit with water, provided that the reservoir is properly lined to isolate the privately owned water from potential commingling with the public domain water in the same general alluvial deposit. Previously, such open reservoirs could be formed by purchasing the rights to abandoned gravel quarries. However, due to the current high demand for water storage, such storage areas created by mining activity are insufficient to keep pace with society's needs. While it is possible to excavate a large pit for the specific purpose of forming an open water reservoir, such a technique requires a great expense of time and money to purchase the land, form the pit and dispose of the excavated material and soil, assuming that the excavated materials have no intrinsic economic value.
[0004] One major disadvantage to open reservoirs is that they preempt any current or future use of the land other than to store water. That is, as additional land surface is devoted to the storage of water in open reservoirs that same land surface is unavailable for alternative uses such as farming or open space. A further disadvantage of storing water in open reservoirs is the high degree of evaporative losses experienced by such reservoirs due to the relatively large air/water interface. Specifically, in arid climates (such as those found in the Western United States) open reservoirs are subject to extremely large evaporative losses.
[0005] A further unfortunate disadvantage to open reservoirs is that the reservoirs are highly susceptible to contamination. While previous concerns have been limited to accidental chemical spills, petroleum leaks, polluted surface-water runoff, and the like, a more immediate threat is that of intentional contamination as part of a terrorist act. Most municipal water reservoirs comprise unfenced bodies of waters in remote areas and are extremely difficult if not impossible to guard. Furthermore, the construction of fences around existing reservoirs would be expensive and time consuming, the fence could be easily breached and thus does not guarantee safety, and even if the fence is not breached, the open reservoirs would be susceptible to contamination from the air.
[0006] One proposed solution to the above-described disadvantages of open reservoirs is the construction of underground reservoirs where water is stored in the voids or interstices found in alluvial deposits. One such method is described in U.S. Pat. No. 4,326,818, issued to Willis and titled “Techniques for the Storage of Water.” The Willis patent describes forming an enclosed flexible wall extending vertically downward toward a natural aquiclude or stone base that is impermeable to water. The wall is formed by a grouting process where a grout pipe is first inserted through the soil until the pipe reaches the aquiclude and is then withdrawn while a grout material is injected under pressure from the end of the pipe. The grout material moves away from the injection zone and fills the pores of the formation where it hardens to form a grout “column.” This process is repeated numerous times to form a closed perimeter wall around a defined reservoir boundary. That is, adjacent grout columns are positioned so that there is little or no space between the columns. A second and third round of grout columns are then formed adjacent the first round of columns to form a wall that is said to be substantially impermeable to water. Conventional wells and feed lines are then constructed within the boundary of the grout wall to withdraw and supply water to the reservoir as needed.
[0007] The specific reservoir described in the Willis patent suffers from a number of drawbacks. Initially, the grout wall construction technique described by Willis (i.e., pressure-grouting clay or other “flexibilized” materials and allowing the grout to “gel” into place) does not typically form uniform subsurface columns. Rather, the grout material disperses from the end of the grout pipe in an uneven and haphazard manner (i.e., permeating different radial distances away from the grout pipe) as the grout pipe is retracted toward the surface. The uneven nature of the grouting process tends to form vertical sand seams between the grouted columns at the outer boundary of the pressure injection. These sand “lenses” or areas of high permeability formed between adjacent grout “columns” result in grout walls that do not form substantially impermeable water barriers and that are susceptible to relatively high levels of water leakage or seepage. Additionally, it is not possible to key the grouted in-situ “columns” into the bedrock or other impermeable basement rock that defines a bottom surface of the underground reservoir. Rather, a small horizontal layer typically remains between the bottom ends of the various grout columns and the bedrock so that water may escape the underground reservoir through this gap between the wall and the bedrock, where the hydrostatic pressure is at its greatest level. Indeed, between the inability to form a solid impermeable wall using the grout technique, and the inability to firmly tie the grout columns to the bedrock defining the lower surface of the reservoir, the water leakage rates of a reservoir built according to the technique of the Willis patent would be prohibitively high.
[0008] A further problem associated with the underground reservoir described in the Willis patent is that there is no recognition of the problems associated with the construction of the massive subsurface walls. Specifically, the installation of any subsurface wall on the scale of that required to form an underground reservoir tends to form a dam to the normal flow of groundwater so that water levels on the upstream or “high” side of the reservoir wall will tend be higher than historic average levels, while the opposite condition (i.e., lower than average water levels) will be found on the downstream or “low” side of the reservoir. Such artificial changes to the historic water table can have severe adverse impacts on neighbors in the region. For example, neighbors on the high side of a subsurface, or underground, reservoir may experience flooded basements, while neighbors on the low side will experience a dearth of water such that alluvial wells may run dry.
[0009] Thus, while the Willis patent describes one design for an underground reservoir, the specifics of the Willis reservoir are not feasible due to the inability to form a water-tight reservoir. Additionally, the grout wall construction techniques described in the Willis patent are prohibitively expensive (costing $40-$200 per square foot of barrier), particularly when used on the scale required for an underground reservoir. Furthermore, the Willis patent does not account for the environmental impact that will be caused by the construction of the potentially massive subsurface walls. Thus, an improved underground reservoir and method for storing water is needed that will address the shortcomings of the Willis design.
[0010] U.S. Pat. No. 6,840,710, issued to Peters et al. and titled “Underground Alluvial Water Storage Reservoir And Method” presents a marked improvement over the Willis design. Peters et al. describes underground porosity reservoirs that are constructed by totally enclosing a portion of an alluvial deposit with a substantially impermeable man-made barrier, such as such as slurry walls keyed into the underlying bedrock formation. However, the economic efficiency depends on the alluvial material enclosed and the amount of slurry wall needed for the enclosure. For alluvial deposits of uniform thickness, generally the larger reservoir sites have a higher enclosure efficiency ratio (the area enclosed by the slurry walls divided by the linear length of the slurry wall that defines the perimeter of the area enclosed) expressed as acres/mile. The two-dimensional enclosure efficiency is also affected by the aspect ratio (the length divided by the width) of the porosity reservoir perimeter. Porosity reservoir sites with approximately equal length sides (substantially square-shaped) are more efficient to enclose an area than are long and narrow sites (substantially rectangular-shaped) that require more slurry wall perimeter to enclose an area. It is with respect to these and other background considerations, limitations, and problems that the present invention is directed.
SUMMARY
[0011] This Summary is provided to introduce in a simplified form a selection of concepts that are further described below in the Detailed Description. This Summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
[0012] In accordance with the present invention, the above and other problems are solved by an underground porosity reservoir for storing water in alluvial deposits that is formed by a combination of: one or more segments of an underground substantially impermeable man-made barrier, such as a slurry wall, pilings, hangar wall, or any other suitable structure that can be keyed into the underlying bedrock formation and partially enclosing an area and extending from a surface level to an aquiclude (e.g., bedrock) beneath the reservoir so that a bottom surface of the slurry wall is keyed into the aquiclude; and keying the two ends of the slurry wall into the natural soils and/or bedrock typical of channel banks near a river and floodplain system where the channel bank between the two ends of the slurry wall form another segment of an underground naturally occurring substantially impermeable barrier. The man-made segments and the naturally occurring segments establish the boundaries of the underground porosity reservoir. The combination of the one or more segments of slurry wall extending from the surface downward and keyed into bedrock on its bottom surface with the two ends of the slurry wall keyed into the natural soils and/or bedrock of the channel bank, and the channel bank between the two ends of the slurry wall, together provide an underground substantially impermeable barrier for the underground porosity reservoir.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0013] FIG. 1 shows a top view of an embodiment of a substantially square-shape bank-sided porosity storage reservoir of the present invention.
[0014] FIG. 2 shows a cross section of the embodiment of the bank-sided porosity storage reservoir shown in FIG. 1 .
[0015] FIG. 3 shows a top view of an embodiment of a substantially rectangular-shaped bank-sided porosity storage reservoir of the present invention.
[0016] FIG. 4 shows a cross section of an embodiment of a bank-sided porosity storage reservoir where the underlying bedrock is substantially flat or slopes away from a riverbed.
[0017] FIG. 5 shows a top view of an embodiment of an oval-shaped bank-sided porosity storage reservoir with multiple man-made and natural segments of the present invention.
[0018] FIG. 6 shows a top view of an irregularly-shaped bank-sided porosity storage reservoir of the present invention shown with bedrock depth contours.
[0019] FIG. 7 shows a cross section of the embodiment of the irregularly-shaped bank-sided porosity storage reservoir shown in FIG. 6 .
[0020] FIG. 8 shows a cross section of an embodiment of a bank-sided porosity storage reservoir in combination with an open reservoir.
[0021] FIG. 9 shows a top view of a bank-sided porosity storage reservoir in combination with an open reservoir shown in FIG. 8 .
DETAILED DESCRIPTION
[0022] Referring now to the Figures, in which like reference numerals and names refer to structurally and/or functionally similar elements thereof, FIG. 1 shows a top view of an embodiment of a substantially square-shape bank-sided porosity storage reservoir of the present invention, and FIG. 2 shows a cross section of the same bank-sided porosity storage reservoir. Referring now to FIGS. 1 and 2 , an exemplary river system or Basin 10 comprising a Riverbed 11 that flows along the top of Alluvial Deposits 23 (e.g., sand and gravel) formed within the Floodplain Limits 15 of a floodplain that extends to either side of the Riverbed 11 . An underground Bank-Sided Porosity Reservoir 14 is preferably formed on three sides with a Substantially Impermeable SIMM Barrier 18 (hereinafter referred to as SIMM Barrier 18 ), such as a slurry wall, and bounded on a fourth side by utilizing the Native Soil 26 , Bedrock 22 , and Topsoil 27 , sometimes delineated by a Bedrock Scour Line 19 below Native Soil 26 and Topsoil 27 , that may be located approximate to Floodplain Limits 15 . Usually, the perimeter of Bank-Sided Porosity Reservoir 14 delineated by SIMM Barrier 18 and Bedrock Scour Line 19 are contained within the bounds of one or more property lines where rights to the water and water storage rights have been obtained.
[0023] Basin 10 is seen in cross-section along line 1 A- 1 A′ in FIG. 2 , showing Riverbed 11 and the lateral and vertical limits of Bank-Sided Porosity Reservoir 14 . FIG. 2 further illustrates that the Bank-Sided Porosity Reservoir 14 is preferably formed by a SIMM Barrier 18 that is keyed into Bedrock 22 or a similar aquiclude where SIMM Barrier 18 extends into Bedrock 22 below the boundary between Alluvial Deposits 23 and Bedrock 22 , forming a substantial seal that prevents water migration from within Bank-Sided Porosity Reservoir 14 to the surrounding soils. It can be seen in FIG. 2 that Bedrock 22 and the overlying Native Soil 26 and Topsoil 27 rise in elevation relative to Riverbed 11 . Bedrock Scour Line 19 was formed thousands of years ago when the river flowed along a different course, scouring Bedrock 22 to form Bedrock Scour Line 19 . By keying the two ends of SIMM Barrier 18 into Bedrock 22 and through Native Soil 26 and Topsoil 27 , water trapped inside Bank-Sided Porosity Reservoir 14 cannot rise high enough in elevation to migrate around the two ends of SIMM Barrier 18 or over/through Bedrock Scour Line 19 .
[0024] Initially, it is noted that SIMM Barrier 18 may be formed in a variety of manners and with a variety of materials. One construction technique forms a slurry wall with a trenching technique that involves excavating a narrow trench that is immediately and concurrently filled with a fluid “slurry” that exerts hydraulic pressure against the trench walls to prevent the trench from collapsing as it is formed. While different materials may be used to form the slurry, bentonite clay mixed with water is a very good slurry for use in constructing SIMM Barrier 18 . This is because the bentonite tends to coat the walls of the trench, thereby preventing the water from being absorbed through the trench walls during and after the formation of SIMM Barrier 18 . Additionally, the bentonite coating helps to enhance (i.e., reduce) the final permeability of SIMM Barrier 18 .
[0025] Slurry wall trenches may be several feet wide and can be dug in excess of 100 feet deep with the use of specialized excavation equipment. Shallower trenches may be formed with conventional backhoes. It is important to remember that the trench must extend down so that it is “keyed” into Bedrock 22 or other confining layer (such as clay) that lies below Alluvial Deposits 23 . In one embodiment, the trench is keyed at least three feet deep into Bedrock 22 . In other embodiments, key depths of four or five feet or more may be required. The slurry-filled trench is then backfilled with a mixture of the previously excavated topsoil and alluvial material, mixed with additional quantities of bentonite. That is, the soil-bentonite mixture is used to fill the open trench where the mixture displaces the water-bentonite slurry and hardens to form the final SIMM Barrier 18 . Care must be taken with this technique to ensure an even backfill and avoid the presence of any voids in the wall or the collapse of any of the untreated soil back into the trench, either of which can form “windows” of relatively high permeability within the wall. With a carefully controlled backfill, soil-bentonite slurry walls having average permeability rates on the order of 1×10 −6 centimeters/sec (“cm/sec”) are obtainable, although permeability rates as low as 1×10 −8 cm/sec may also be obtained with a proper soil-bentonite mixture.
[0026] An alternative construction technique is to use a single-step excavation and in situ mixing process where the bentonite-water slurry is mixed with Portland cement so that the slurry itself hardens to form a “cement-bentonite” SIMM Barrier 18 . While a cement-bentonite slurry wall is formed more quickly than the two-step (backfill) soil-bentonite slurry wall, such one-step walls typically have slightly higher permeability levels (on the order of 1×10 −5 cm/sec). However, the permeability of both the soil-bentonite and the cement-bentonite slurry walls may be improved by adding liners or membranes during the trenching process and prior to forming the hardened SIMM Barrier 18 . These liners or membranes may be high density polyethylene or polyvinyl chloride sheets that are added to the slurry-filled trench either prior to the backfill step of the two-step soil-bentonite slurry wall process, or prior to the hardening of the cement-bentonite wall in the one-step cement-bentonite process. The addition of such liners or membranes further enhances the substantially impermeable nature of the slurry walls where necessary to prevent leakage.
[0027] Generally, a plurality of water extraction/recharge means are distributed about the interior area of the underground porosity reservoir to provide for rapid and substantially even filling and draining. A plurality of wells may be distributed about the underground reservoir, each well connected to a pump to direct water under pressure through the plurality of wells and into the alluvial deposits of the underground reservoir. Alternatively, a series of perforated pipes may be buried at a predetermined depth within the underground reservoir so that the perforated pipes are connected to a central pressurized well that is operated to recharge and extract water from the alluvial deposits through the perforated pipes. Such filling and draining systems are disclosed in the Peters et al. patent.
[0028] FIG. 3 shows a top view of an embodiment of a substantially rectangular-shaped bank-sided porosity storage reservoir of the present invention. Referring now to FIG. 3 , river system or Basin 30 comprises a Riverbed 31 that flows along the top of alluvial deposits (e.g., sand and gravel) formed within the Floodplain Limits 35 of a floodplain that extends to either side of Riverbed 31 . An underground Bank-Sided Porosity Reservoir 34 is preferably formed on three sides with a Substantially Impermeable Man-Made Barrier 38 (hereinafter referred to as SIMM Barrier 38 ), such as a slurry wall, and bounded on a fourth side by utilizing native soil, bedrock, and topsoil. In this instance, SIMM Barrier 38 has two substantially straight short end portions, and the middle portion is fairly long in comparison to the two short end portions, and is irregular in shape as viewed from above. By keying the two ends of SIMM Barrier 38 into the underlying topsoil, native soil, and bedrock, water trapped inside Bank-Sided Porosity Reservoir 34 cannot migrate around the two ends of SIMM Barrier 38 .
[0029] For alluvial deposits of uniform thickness, generally the larger reservoir sites have a higher enclosure efficiency ratio (the area enclosed by the slurry walls divided by the linear perimeter length of the slurry walls), usually expressed as acres/mile. This two-dimensional enclosure efficiency is also affected by the aspect ratio (length to width) of the reservoir boundaries. Reservoir sites with approximately equal length sides are more efficient to enclose a volume than are long and narrow sites that require more linear slurry wall perimeter to enclose a given volume for a porosity reservoir.
[0030] Table 1 below indicates the improved enclosure efficiencies provided with a bank-sided reservoir, for both smaller reservoir sites and ones with poor aspect ratios. This improvement with bank-sided reservoirs is important since most properties suitable for underground porosity reservoirs are typically longer than they are wide, since the length of the river valley is usually much longer than the floodplain is wide. Thus, a bank-sided reservoir not only increases the efficiency of a normally efficient square property (aspect ratio of 1:1), but it improves the efficiency of “long” parcels (aspect ratios of 4:1) to actually equal the improved enclosure efficiency of square bank-sided reservoir sites. Uniform thicknesses of alluvial deposits are assumed in these calculations. It should be noted that the widths of the slurry walls with keys into the natural soils/bedrock and the width of the reservoir are not the same, but they are typically approximately equal due to the scale. For example, a 1,000 foot wide reservoir may have a side key width of 50 feet.
[0000]
TABLE 1
Four-
Bank-
Sided
Sided
Property
Aspect
Acres/
Acres/
Description
Acres
Width
Length
Ratio
Mile
Mile
Square,
160
½
Mile
½
Mile
1:1
80
107
Quarter
Section
Long,
160
¼
Mile
1
Mile
4:1
64
107
Quarter
Section
Half Section
320
½
Mile
1
Mile
2:1
107
160
Square
640
1
Mile
1
Mile
1:1
160
213
Section
Long Section
640
½
Mile
2
Miles
4:1
128
213
Square, Four
2560
2
Miles
2
Miles
1:1
320
427
Sections
Long, Four
2560
1
Miles
4
Miles
4:1
256
427
Sections
[0031] For example, for a four-sided reservoir covering a long quarter section, the perimeter of the slurry walls is ¼+1+¼+1 which equals 2.5 miles. The acres/mile is then derived from the area, 160 acres, divided by the perimeter length, 2.5 miles, yielding 64 acres/mile. For a long quarter section bank-sided porosity reservoir, the perimeter length of the slurry walls is ¼+1+¼ which equals 1.5 miles. The acres/mile is then calculated by dividing the area, 160 acres, by 1.5 miles, yielding 107 acres/mile. It can be seen for all property descriptions, square or rectangular, and with aspect ratios ranging from 1:1 up to 4:1, a bank-sided porosity reservoir is more efficient than any four-sided porosity reservoir due to the increased acres/mile.
[0032] In comparing economic efficiencies of one reservoir site and size to another, the thickness of the alluvial deposit compared to the depth of slurry wall must also be considered. The slurry wall needs to be constructed through native over-burden materials as well as keyed into the underlying bedrock formation. However, slurry walls constructed in these materials is more of an overhead cost to the reservoir. Hence depth efficiency (the depth of alluvium compared to the total depth of slurry wall) is greater with deeper alluvial deposits and/or shallower overburden material, given a required key depth. Hence, a final three dimensional enclosure efficiency can be evaluated as the product of the two-dimensional enclosure efficiency with the depth efficiency.
[0033] As an example, consider a typical or “normal” alluvial deposit of five feet of overburden and top soil, forty feet of alluvial sand and gravel, and a required bedrock key depth of five feet. This site has a depth efficiency of 80% (forty feet of alluvium divided by fifty feet total depth of slurry wall). Compare that to a different “shallow” site with only half the alluvial thickness, or twenty feet and the same five feet of overburden and the same key depth of five feet. This site has a depth efficiency of 67% (twenty feet of alluvium divided by thirty feet total depth of slurry wall). Assuming a “long, quarter section” property in a “normal” depth area and 20% net porosity (which means that only 20% of the volume can store and drain water), a four-sided enclosed porosity reservoir would require 516 square feet of slurry wall to produce one acre-foot of water storage. This is calculated as follows: The perimeter length of the slurry wall from the example above is 2.5 miles, which equals 13,200 linear feet of slurry wall. 13,200 linear feet of slurry wall times a slurry wall depth of fifty feet equals 660,000 square feet of slurry wall. Forty feet of alluvium at 20% porosity equals an equivalent of eight vertical feet of water storage. Eight feet multiplied by 160 acres equals 1,280 acre-feet of water storage. 660,000 square feet of slurry wall divided by 1,280 acre-feet of water storage equals 516 square feet of slurry wall per acre-foot of water storage.
[0034] If the deposit was “shallow” having twenty feet of alluvial material, 619 square feet of slurry wall would be required, calculated as follows: 13,200 feet times a slurry wall depth of thirty feet equals 396,000 square feet of slurry wall. Twenty feet of alluvium at 20% porosity equals an equivalent of four vertical feet of water storage. Four feet multiplied by 160 acres equals 640 acre-feet of water storage. 396,000 square feet of slurry wall divided by 640 acre-feet of water storage equals 619 square feet of slurry wall per acre-foot of water storage. For these same property dimensions and thicknesses, a bank-sided porosity reservoir design would only require 309 square feet and 371 square feet of slurry wall per acre-foot of water storage respectively. Hence, the bank-sided reservoir design even overcomes the depth efficiency disadvantages of “shallow” alluvial deposits. These efficiency ratios easily convert to the cost of slurry walls per acre-foot once the cost per square foot is known.
[0035] Alternately, the three dimensional efficiency of a porosity storage reservoir can be described one-dimensionally as the ratio of volume of water stored (in cubic feet) to the area (square feet) of man-made barrier constructed to effect proper isolation and containment. With the same quarter section of land enclosed by both square and long reservoir configurations, with both normal and shallow alluvial depths as described in the example above, the efficiency of bank-sided porosity reservoirs is 33% to 67% more efficient than four-sided reservoirs, as shown in TABLE 2 below:
[0000]
TABLE 2
Property
Four-Sided,
Bank-Sided,
%
Description
Depth
Feet
Feet
Increase
Square (1:1)
Normal (40 feet)
106
141
33%
Long (4:1)
Normal (40 feet)
85
141
67%
Square (1:1)
Shallow (20 feet)
88
117
33%
Long (4:1)
Shallow (20 feet)
70
117
67%
[0036] For a long property with normal depth (40 feet of alluvium) the calculation for a four-sided porosity reservoir is as follows: An acre-foot is defined by the volume of one acre of surface area to a depth of one foot. Since the area of one acre is defined as 66 by 660 feet (a chain by a furlong) then the volume of an acre-foot is exactly 43,560 cubic feet. Eight vertical feet of storage multiplied by 160 acres multiplied by 43,560 cubic feet, then divided by 660,000 square feet equals 85 feet. For the same property the calculation for a bank-sided porosity reservoir is as follows: eight feet multiplied by 160 acres multiplied by 43,560 cubic feet, then divided by 396,000 square feet equals 141 feet.
[0037] If the square configuration porosity reservoir with normal depths is considered as the baseline of the best efficiency (106 feet) for four-sided porosity storage reservoirs, (with long configurations and/or shallow alluvial deposits decreasing efficiency of enclosure to 70% to 90%), Table 2 above illustrates that bank-sided reservoirs can significantly increase the one-dimensional enclosure efficiency over four-sided porosity reservoirs. This improvement is especially important considering the aspect ratio of most alluvial river valleys tends to be rather long, making normally-efficiently square-configured reservoir sites difficult to come by on a large scale.
[0038] FIG. 4 shows a cross section of an embodiment of a bank-sided porosity storage reservoir where the underlying bedrock is substantially flat or slopes away from a riverbed. Referring now to FIG. 4 , Basin 40 is seen in cross-section, showing Riverbed 41 and the lateral and vertical limits of Bank-Sided Porosity Reservoir 44 . FIG. 4 further illustrates that the Bank-Sided Porosity Reservoir 44 is preferably formed by a Substantially Impermeable Man-Made Barrier 48 (hereinafter referred to as SIMM Barrier 48 ) that is keyed into Bedrock 42 or a similar aquiclude where SIMM Barrier 48 extends into Bedrock 42 below the boundary between Alluvial Deposits 43 and Bedrock 42 , forming a substantial seal that prevents water migration from within Bank-Sided Porosity Reservoir 44 to the surrounding soils. It can be seen in FIG. 4 that Bedrock 42 falls in elevation and the overlying Native Soil 46 and Topsoil 47 stays level or rises in elevation relative to Riverbed 41 . In this situation, the two ends of SIMM Barrier 48 are keyed into Bedrock 42 and through Native Soil 46 and Topsoil 47 at a distance that takes into account the permeability of Native Soil 46 such that water trapped inside Bank-Sided Porosity Reservoir 44 will not move laterally in significant amounts and then migrate around the two ends of SIMM Barrier 48 . The distance that two ends of SIMM Barrier 48 are extended may be primarily determined by a cost/benefit ratio of the amount that the percent of water migration around the two ends of SIMM Barrier 48 is reduced compared to the costs of extending the two ends of SIMM Barrier 48 . It may not be cost effective to achieve zero percent migration, where migration may be fixed at say five percent for a nominal linear extension of the two ends of SIMM Barrier 48 .
[0039] FIG. 5 shows a top view of an embodiment of an oval-shaped bank-sided porosity storage reservoir with multiple man-made and natural segments of the present invention. Referring now to FIG. 5 , Basin 50 comprises a Riverbed 51 that flows along the top of alluvial deposits (e.g., sand and gravel) formed within the Floodplain Limits 55 of a floodplain that extends to either side of the Riverbed 51 . An underground Bank-Sided Porosity Reservoir 54 is preferably formed on a first side with a Substantially Impermeable Man-Made Barrier 58 (hereinafter referred to as SIMM Barrier 58 ), such as a slurry wall formed in the shape of an oval or an arc, and bounded on a second side by utilizing the native soil, bedrock, and topsoil, sometimes delineated by a Bedrock Scour Line 59 below the native soil and topsoil, that may be located approximate to Floodplain Limits 55 . In this example, Bedrock Scour Line 59 falls in elevation between the first and second ends of SIMM Barrier 58 , and thus, would not provide the consistent substantially impermeability needed to trap water within the bounds of Bank-Sided Porosity Reservoir 54 . In this situation, an additional Substantially Impermeable Man-Made Barrier 58 ′ (hereinafter referred to as SIMM Barrier 58 ′) is constructed in the gap. The first and second ends of SIMM Barrier 58 ′ are keyed into the topsoil, native soil, and down to the bedrock level. The bottom surface of SIMM Barrier 58 ′ is also keyed into the bedrock as described above. One skilled in the art will recognize that in certain basin areas, bank-sided porosity storage reservoirs may be multi-segmented, having one or more substantially impermeable man-made barriers connecting with one or more natural substantially impermeable barriers in order to encompass the underground alluvial deposit of interest.
[0040] Usually, the perimeter of Bank-Sided Porosity Reservoir 54 delineated by SIMM Barrier 58 and Bedrock Scour Line 59 are contained within the bounds of one or more property lines where rights to the water and water storage rights have been obtained. One skilled in the art will thus recognize that the substantially impermeable man-made barrier may be formed in a number of shapes, including arcs, ovals, irregularly shaped, one-sided, two-sided, three-sided, and up to n-sided depending upon the topography and property boundaries and other site-specific considerations.
[0041] FIG. 6 shows a top view of an irregularly-shaped bank-sided porosity storage reservoir of the present invention shown with bedrock depth contours, and FIG. 7 shows a cross section of the same embodiment of the bank-sided porosity storage reservoir. Referring now to FIGS. 6 and 7 , Basin 60 comprises a Riverbed 61 that flows along the top of Alluvial Deposits 73 (e.g., sand and gravel) formed within a floodplain that extends to either side of the Riverbed 61 . An underground Bank-Sided Porosity Reservoir 64 is preferably formed on a first side with a Substantially Impermeable Man-Made Barrier 68 (hereinafter referred to as SIMM Barrier 68 ), such as a slurry wall formed in an irregular shape, and bounded on a second side by utilizing the Native Soil 66 and Bedrock 72 .
[0042] Basin 60 is seen in cross-section along line 6 A- 6 A′ in FIG. 7 . Bank-Sided Porosity Reservoir 64 capitalizes on a Scour Region 700 formed by the river path thousands of years ago, where the flow of the river scoured out a depression in Bedrock 72 . Various Contour Lines are is shown in FIG. 6 , indicating the depth below the surface of Alluvial Deposits 73 that the upper surface of Bedrock 72 is located. Contour Line 602 shows that Bedrock 72 is at a depth of twenty feet. Contour Line 604 shows that Bedrock 72 is at a depth of forty feet. Contour Line 606 shows that Bedrock 72 is at a depth of sixty feet. Contour Line 608 shows that Bedrock 72 is at a depth of eighty feet. Greatly increased volumes of water storage are obtainable by taking advantage of such scour regions when they are presented.
[0043] FIG. 8 shows a cross section of an embodiment of a bank-sided porosity storage reservoir in combination with an open reservoir. FIG. 9 shows a top view of the bank-sided porosity storage reservoir in combination with an open reservoir shown in FIG. 8 . Referring now to FIGS. 8 and 9 , combinations of open water and underground porosity water storage are also possible with the bank-sided porosity reservoirs. Embankments constructed above the slurry wall permit traditional open water storage above the porosity storage reservoir. River system or Basin 90 comprises a Riverbed 81 that flows along the top of Alluvial Deposits 83 (e.g., sand and gravel) formed within the Floodplain Limits 95 of a floodplain that extends to either side of the Riverbed 81 . An underground Bank-Sided Porosity Reservoir 94 is preferably formed on a first side or segment with a Substantially Impermeable Man-Made Barrier 88 (hereinafter referred to as SIMM Barrier 88 ), such as a slurry wall, and bounded on a second side or segment by utilizing the floodplain banks comprised of Native Soil 86 , Topsoil 87 , and/or Bedrock 82 . Embankment 802 is formed on top of where SIMM Barrier 88 will be constructed. Material for Embankment 802 may come from utilizing Topsoil 87 and Alluvial Deposits 83 over the surface of Bank-Sided Porosity Reservoir 94 . Topsoil 87 is often excavated within the interior of SIMM Barrier 88 , and may also be utilized to build Embankment 802 . SIMM Barrier 88 is then constructed through Embankment 802 as well as Native Soil 86 , Topsoil 87 , and/or Bedrock 82 . When Topsoil 87 is removed from the top of Bank-Sided Porosity Reservoir 94 , Alluvial Deposits 83 are directly exposed to water injected into Open Water Storage 800 , greatly increasing the percolation rate of water into Alluvial Deposits 83 , which increases the ability to rapidly fill Bank-Sided Porosity Reservoir 94 , as well as increases the volume of open water storage possible. A layer of relatively impervious materials can also be layered on top of Alluvial Deposits 83 should the reservoir operator desire to manage Open Water Storage 800 separately from Bank-Sided Porosity Reservoir 94 . Long-term settlement build-up in Open Water Storage 800 of the combination reservoirs may be removed if needed, while the underlying Bank-Sided Porosity Reservoir 94 could continue in operation. Embankment 802 has Inside Toe Of Slope 804 under water (shown in dashed lines in FIG. 9 ) and Outside Toe Of Slope 806 . The boundary between Embankment 802 and Open Water Storage 800 is Shoreline 808 .
[0044] A Bank Liner 810 could also be installed along the inside face of Embankment 802 and along Flood Plain Bank 902 to retard lateral water migration of Open Water Storage 800 . Bank Liner 810 is typically covered with rock or bric-a-brac to secure it in place. On the Embankment 802 side, Bank Liner 810 would extend from Inside Toe Of Slope 804 to a short distance above Shoreline 808 . On the Flood Plain Bank 902 side, Bank Liner 810 would extend from Inside Toe Of Slope 812 to a short distance above Shoreline 808 . In an alternate embodiment, SIMM Barrier 88 would not extend through Embankment 802 . Instead, Embankment 802 would be constructed to the left of the position shown in FIG. 8 so that Inside Toe Of Slope 804 of Embankment 802 coincides with the top of SIMM Barrier 88 at the juncture of Topsoil 87 /Alluvial Deposits 83 . Bank Liner 810 would be installed and extending from the top of SIMM Barrier 88 on the inside face of Embankment 802 to a short distance above Shoreline 808 .
[0045] Basin 90 is seen in cross-section along line 9 A- 9 A′ in FIG. 8 , showing Riverbed 81 and the lateral and vertical limits of Bank-Sided Porosity Reservoir 94 . FIG. 8 further illustrates that the Bank-Sided Porosity Reservoir 14 is preferably formed by SIMM Barrier 88 that is keyed into Bedrock 82 or a similar aquiclude where SIMM Barrier 88 extends into Bedrock 82 below the boundary between Alluvial Deposits 83 and Bedrock 82 , forming a substantial seal that prevents water migration from within Bank-Sided Porosity Reservoir 94 to the surrounding soils. By keying the two ends of SIMM Barrier 88 into Bedrock 82 and through Native Soil 86 and into Floodplain Bank 902 , water trapped inside Bank-Sided Porosity Reservoir 94 cannot rise high enough in elevation to migrate around the two ends of SIMM Barrier 88 . Water contained within Open Water Storage 800 also cannot rise high enough in elevation to migrate around or over the two ends of SIMM Barrier 88 and over Floodplain Bank 902 .
[0046] By varying the height of the Embankment 802 (increased at the lower elevation end of the site), the water storage on the property can be increased. In high-evaporative climates, the operator would typically use Open Water Storage 800 ′ for shorter time periods, and maintaining Bank-Sided Porosity Reservoir 94 for long-term drought protection, since normal evaporative losses are avoided. As depicted in FIG. 9 , surface water upstream could enter Open Water Storage 800 via Pipe(s) 904 (with control valves) which penetrate Embankment 802 , while passive outflows could occur via similar penetrating Pipe(s) 906 (with control valves). Elevated or submersible Well Structures 908 could be used to inject and extract stored water within Bank-Sided Porosity Reservoir 94 portion of the combination reservoir.
[0047] Although the subject matter has been described in language specific to structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as example forms of implementing the claims. It will be understood by those skilled in the art that many changes in construction and widely differing embodiments and applications will suggest themselves without departing from the scope of the disclosed subject matter. | Natural soils and underlying bedrock typical of channel banks near a river and floodplain system are utilized to improve the economics and efficiency of constructing an underground porosity storage reservoir. A man-made barrier, typically a slurry wall, is keyed into these banks and forms a first portion of a closed boundary for the reservoir. The channel banks between the two ends of the slurry wall form a substantially impermeable natural barrier defining a second portion of the closed boundary for the reservoir, thereby reducing the construction costs on sites appropriate for such a design. Locating the bank-sided porosity storage reservoir over naturally occurring scour regions in the bedrock can greatly increase the storage capacity. By building an embankment and extending the slurry walls higher, an open water storage area can be created on top of the reservoir that is bounded by the elevated slurry wall and the channel bank. | 1 |
THE FIELD OF THE INVENTION
The present invention relates to sweeping machines of the type shown generally in U.S. Pat. No. 4,787,923 owned by Tennant Company of Minneapolis, Minn., the assignee of the present application. More particularly, the present invention relates to an improved filter and the means for cleaning the filter.
It is present practice in the sweeping machine art, as shown in the above-mentioned '923 patent, to place a filter in the air flow path of the sweeping machine in such a position that dust is collected below the filter and clean air passes from the filter to the vacuum fan. Such filters are periodically cleaned, again as shown in the '923 patent, by shaker bars. Shaker bars are not particularly effective as a cleaning device and the filter panel is often cleaned inefficiently and inadequately. The present invention provides electromagnetic shaking of the filter media by the placement of one or more small transformers on the top of the filter media and then the use of bars or other types of metal elements, such as rods arranged to cause movement of the filter media. When power is applied to the transformers, the bars or metal elements will move and in one form of the invention the transformers will be pulsed so that the vibration imparted to the bars and thus to the filter pleats very effectively cleans the filters through shaking, causing the dust to fall down into the dust collection chamber. The electro-magnetic filter cleaning of the present invention is essentially noiseless, simple in construction, and utilizes relatively low vibration of the filter media. The entire filter panel may be cleaned, or segments of the panel may be cleaned, either sequentially or alternately. For example, one portion of the panel may be cleaned and the other portion remain operative to pass air through the air flow path in the sweeping machine. In its broadest context, the invention provides electromagnetic cleaning of the filter of a sweeping machine using at least one transformer or solenoid.
In one form of the invention, a plurality of transformers are positioned above a filter panel formed of generally parallel pleats. Portions of the pleats will be connected together into groups by pleat blocks. On the top of each pleat block there is an elongated metal bar. There will be two pleat blocks associated with each transformer and when the transformer is pulsed, the elongated bars will move toward the transformer. The resultant reciprocal movement of the elongated bars and the consequent movement of the pleat blocks and pleats will result in a substantial shaking or vibration of the pleats which will remove the dust which is caked and embedded therein.
Preferably, the transformers will not be operated simultaneously, but will be operated in a predetermined sequence. This reduces the power drain on a machine which often is battery operated. One or more transformers may be pulsed at any one time and the transformers will be pulsed in a predetermined sequence with the result that over a short period of time the entire pleated filter will be cleaned. The time duration of the application of pulsed power can be controlled as can the frequency of pulsed power as well as the intervals between the application of pulsed power.
The application of pulsed power which will draw the pleat blocks toward the transformer has the result of causing the pleats in adjoining pleat blocks to move toward each other and to at least in part contact each other which enhances the vibration imparted to the individuals pleats to assist in the removal of dust and caked debris from the pleated filter element.
SUMMARY OF THE INVENTION
The present invention relates to sweeping machines and in particular to an electromagnetic filter cleaning device for sweeping machines.
A primary purpose of the invention is a filter cleaning device for the use described which utilizes pulsed transformers positioned above the pleated filter with the filter pleats being associated with metal elements which will be moved by the pulsed power in a manner to shake the pleats for cleaning.
Another purpose is a filter cleaning system as described in which the sequence of transformer activation is controlled to reduce power drain.
Another purpose is a filter cleaning system as described in which the time duration and frequency of transformer operation is controlled to maximize filter cleaning.
Other purposes will appear in the ensuing specification, drawings and claims,
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is illustrated diagrammatically in the following drawings wherein:
FIG. 1 is a diagrammatical illustration of a sweeper of the type using the cleaning system disclosed herein;
FIG. 2 is a top plan view of the filter element illustrating the electromagnetic shaker devices applied thereto;
FIG. 3 is a section along plane 3--3 of FIG. 2;
FIG. 4 is a side view of a pleat block;
FIG. 5 is a top view of a pleat block;
FIG. 6 is a partial top plan view of a modified form of electromagnetic shaker system;
FIG. 7 is a section along plane 7--7 of FIG. 6;
FIG. 8 is a side view of the pleat block of the FIGS.6 and 7 embodiment;
FIG. 9 is a top view of the pleat block of FIG. 8;
FIG. 10 is a top plan view of a modified form of pleat block;
FIG. 11 is a side view of the pleat block of FIG. 10; and
FIG. 12 is an electrical schematic of the control system for the electromagnetic shaker devices illustrated herein.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1 a typical street sweeper of the type illustrated in U.S. Pat. No. 4,787,923, owned by Tennant Company of Minneapolis, Minn., the assignee of the present application is indicated at 10. The sweeper 10 has a brush 12 which directs dust and debris into a hopper 14. Wheels 16 support the sweeper 10. There is a vacuum fan 18 which creates an airflow path in the direction of arrows 20. Positioned within the airflow path is a filter 22 which is illustrated in detail in the following Figs.
As shown particularly in FIGS. 2 through 5, the filter 22 has a peripheral frame 24 which includes side walls 26. Within the confines of the side walls 26 is a pleated filter element 28 which has upper folds 30 and lower or bottom folds 32. The filter element may be conventional and may be formed of paper, or synthetic materials as use dictates. The top of the filter 22 include an aluminum mesh cover 34.
Mounted on top of the filter 22 is a transformer assembly which includes a support bar 36 to which are mounted a plurality of transformers or electric coils 38. The ends of the support bar 36 may be supported by brackets 40 as particularly shown in FIG. 3.
As illustrated in FIG. 2 there are five transformers which may be satisfactory for a 20 inch by 30 inch filter panel. The number of transformers is not essential and may be dictated by the size of the panel. Four transformers may be satisfactory for the same size panel and the number of transformers will in part be dictated by the power and frequency at which the transformers are operated.
As shown in FIG. 3 the pleats 28 may in part be separated into groups and joined together by pleat blocks 42. The pleat blocks 42 which may be formed of a suitable plastic and which have the appearance of a comb have a top surface 44 and a plurality of downwardly extending projections 46 which extend between adjacent pleats with the top folds 30 of the pleats within a group joined by a pleat block extending into the space between the projections 46. There are two groups of pleats joined by pleat blocks positioned adjacent each transformer 38. The adjoining pleat blocks are slightly separated directly beneath the coil of the transformer. Each pleat block 42 carries an elongated metal bar 48 embedded into its upper surface with the bars extending for a substantial portion of the width of the pleat block, although this is not necessary. By separating the pleats into groups and by having the groups positioned to be operatively located next to each transformer there is provided an arrangement of pleat blocks with the most efficient means of cleaning the dirt and caked dust from the pleats.
When each of the transformers is activated by a pulse of electric power, there will be an electromagnetic field formed thereabout. The field will draw the elongated bars 48 towards the center of the transformer. Such movement of the bars will cause concurrent movement of the pleat blocks with the result that the pleats joined by the pleat block will simultaneously move with it. Back and forth movement of adjacent pleat blocks will not only cause vibration of the pleats, but will cause the pleat blocks to contact each other, causing a further impact and shaking of the pleats. Since it is desirable to pulse the transformers, rather than having continuously applied power for every pulse applied to the transformer, the pleat blocks associated with that transformer will move toward each other, and when the power is removed, the pleat blocks will return, because of the inherent resilience of the pleats, back to their at rest position shown in FIG. 3. Thus, the application of pulsed power will cause a vibration or reciprocal movement of the pleat blocks and the pleats joined together by the pleat blocks. This rapid back and forth movement, provided at intervals determined by the control circuit described hereinafter, will cause a shaking or vibration of the pleat blocks to the end that the pleats will be rapidly moved to the point where the dust which has been accumulated on the pleats will be shaken and will fall into the dust collection chamber directly beneath the filter.
The FIG. 2 through 5 embodiment of the invention uses elongated bars extending transversely to the direction of the pleats to react to the electromagnetic fields created by the pulses of power applied to the transformers. The FIGS. 6-9 embodiment of the invention again uses elongated metal elements, but in a different orientation. As particularly shown in FIGS. 6-7, there is an elongated rod or wire 50 embedded in the top fold 30 of one of the pleats joined by the pleat block 52. The rod or wire 50 extends generally substantially the entire length of the pleats as shown in FIG. 6. The wires or rods are metal and will be responsive to an electromagnetic field created by pulsed power applied to the transformer. Again, there are two groups of pleats associated with each transformer and there is a single elongated element located in each pleat block.
In the FIGS. 6-9 embodiment the rods extend parallel to the pleats and will be moved by the application of an electromagnetic field from the transformer. The rods will move towards the center of the transformer and in so doing will move the pleat blocks back and forth in the same manner as the pleat blocks move in the FIGS. 2-5 embodiment. The pleat blocs indicated in FIGS. 8 and 9 are similar to the blocks indicated 4-5 except there is no elongated metal bar embedded into the surface. Again, movement of the pleat blocks results from the use of elongated rods which will move towards the center line of the transformer when pulsed power is applied to it. The movement of the pleat blocks in both embodiments will be substantially the same.
In FIGS. 10 and 11 there is a modified form of pleat block. In this case the pleat block indicated generally at 60 has a comb 62 with a metal bar 64 embedded in the surface thereof. To this extent it is similar to the pleat block shown in FIGS. 4 and 5. Joined to the comb 62 is an elongated carrier 66 which has downwardly extending projections 68 as shown in FIG. 11 and which will sit atop two adjoining pleats. Thus, reciprocal movement of the pleat block toward and away from the transformer, as described in connection with the FIGS. 2 through 5 embodiment will now result in such transverse movement being applied entirely over the length of the pleats in the group. There is no longer reliance Just upon movement of the comb which has limited width, but the carrier 66 will insure that the movement applied to the pleats will extend over the entire length of the pleats within the group.
FIG. 12 illustrates the control circuit for all of the previously described embodiments. The transformer coils are indicated at 70 and are designated as coils 1 through 5. Again the number of coils may vary and is not critical to the invention. There are a series of amplifiers 72, there being one amplifier for each coil. The amplifiers are connected to a sequencer 74 with the sequencer being controlled by a clock 76. The clock 76 and sequencer 74 will determine which coils are operated and in what sequence. For example, it may be desirable to operate a single transformer or coil at a time and with the coils being powered up in a particular sequence, depending upon their placement over the filter element, to achieve the most efficient cleaning effect. It is also within the scope of the invention to have more than one transformer operated at any one time. For example, two coils may be powered up at one time or the coils may be powered up in a manner so that a single coil is on and before it has been turned off a second coil is powered and a third coil is powered before the second coil is turned on. Any desired sequence is within the scope of the invention. What is important is that the power be applied in the form of pulses and that less than all of the coils be powered at any one time so as to avoid an excessive power drain on the sweeping machine power supply which is conventionally a battery.
There is a second clock indicated at 78 and labeled clock number one which determines the time duration of the applied pulses. This clock is activated by the operator through the remote shake button and will initiate a cleaning operation. The output from clock number one, indicated at 78, is a series of pulses with the clock controlling the period of the pulse and thus the time between successive pulses. This series of pulses goes to an intensity generator 80 which has a remote intensity control and a remote frequency control. The output from the intensity generator is a series of pulses, at a frequency and intensity determined by the operator. The intensity, or the amplitude of the pulses will control the electromagnetic field created by each transformer. The pulses from intensity generator 80 are connected to the amplifiers 72 designated as amplifiers A through E. There is an amplifier for each coil. The result of the circuit shown is to provide pulses, at a desired frequency and a desired amplitude and with a predetermined duration between pulses to the amplifiers which will be activated in the desired sequence by clock number 2 to control the power applied to the coils 70.
A 30 hZ frequency for the application of the pulses has been determined to provide efficient cleaning. The sequencer may be set to provide two seconds for each cleaning segment whether it be a single transformer or more than one transformer. During the cleaning cycle an efficient mode of operation is to have the transformers be on 30% of the time and off 70% of the time. Although the invention should not be limited to these specific parameters, such have been found to provide effective cleaning.
Whereas the preferred form of the invention has been shown and described herein, it should be realized that there may be many modifications, substitutions and alterations thereto. | A sweeping machine includes a housing, wheels for moving the housing and a sweeping brush mounted on the housing. There is a hopper positioned adjacent the brush to receive dust and debris from the rotating brush. A dust collection chamber is located on the housing and a vacuum fan mounted on the housing creates an air flow path from the brush through the hopper into the dust collection chamber. A filter element is positioned in the air flow path with the filter element including a plurality of generally parallel pleats extending in a direction transverse to the air flow path. There is a plurality of electric coils positioned adjacent the pleats. A plurality of metal elements are associated with the pleats. Pulsed electric power is applied to the coils with the electromagnetic fields caused thereby moving the metal elements reciprocally back and forth and the pleats associated therewith to impart a shaking, cleaning movement to the pleats. | 0 |
FIELD OF THE INVENTION
This invention relates to combination locks, and more particularly to an electromechanical control mechanism using non-numeric encoding.
BACKGROUND OF THE INVENTION
Safes, vaults, lockers, and keyless entries, among other types of secure systems, use locks requiring a unique combination for access. Typically, the combination is a set of numbers and rotational sequences which align tumblers to a predetermined orientation. The tumblers make a sound when dropping and this “signature” can reveal the combination when sophisticated listening devices are used. Furthermore, telltale wear patterns can develop with mechanical abrasion and can similarly be detected with sensitive equipment.
One method of eliminating the mechanical action of tumblers is to use an optical alignment system. U.S. Patent Application 2206/0037374 to Skelly teaches the use of a light beam received by a sensor through aligned holes in three concentric tubes rotating about the common axis. The tubes can be manipulated by interfacing members on each tube such that a series of discrete rotations of the innermost tube, twisting clockwise and counterclockwise, bring the three into an alignment of the holes. The aligned holes enable a beam originating in the center to pass through to a sensor located outboard. The receipt of the beam passes a command to an unlocking mechanism. There are no tumblers to drop and no sound clues to witness the angular settings of the combination.
Similarly, in U.S. Pat. No. 2,008,150 to Nelson, a light signal traversing a “fence” of aligned holes in a series of disks mounted on a common shaft provides the means for controlling a lock. The combination is the individual orientation of each disk thus aligned. Except for one disk corresponding to a dial, the disks are free to rotate on the shaft, and in like manner to Skelly, each can be set into position by means of rotating the dial and engaging an interfacing geometry. The problem with such a system, however, is that the subsequent rotation of the moving part could disturb the prior setting of a positioned part. The common shaft, the case of Nelson, or the nested tubes, in the case of Skelly, would inevitably create rotational drag on co-journaled elements. What is missing in the prior art is a light fence where each disk can be individually set and registered to position.
The energy source for such opto-electrical systems is typically supplied by battery. If the light is rendered always on, or if it is switched on to initialize the combination setting procedure, battery life will be consumed and ultimately require service. The benefit in safety attendant to such an optical device is thus offset by the inconvenience of maintenance. It would be an advantage, therefore, to provide for conservation of energy use and extended battery life in the design of such systems.
Both Skelly and Nelson use number indices to orient the combination. Even if security breach were not a risk, number patterns are not particularly user-friendly. They can be hard to remember, especially if they are randomly chosen and not resettable in after-market use. Research has shown that visual patterns are processed in the brain in a different way than word or number patterns. Not only is visual recognition instantaneous, it is also easier to remember. Furthermore, visual patterns do not lend themselves to discovery by guessing, in the way that knowledge of an individual's background can sometimes suggest a number combination. Some means to set a visual pattern combination, therefore, would represent a needed improvement.
SUMMARY OF THE INVENTION
In view of the above-mentioned unfulfilled needs, the present invention embodies, but is not limited by, the following objects and advantages:
A first objective is to provide an optical means for controlling a lock.
A second objective is to define the optical means in terms of a light fence represented by concentrically-journaled rotating wheels.
A third objective is to render each wheel individually settable and thereby eliminate any drift in position caused by coaction.
A fourth objective is to provide a means for positively locating each such wheel.
A fifth objective is to provide a visual recognition means for identifying the combination representing the orientation of each wheel in alignment.
A sixth objective is to improve battery life by shortening the use period to a brief pulse.
A seventh objective is to extend the possible combination permutations by including rotation direction as an argument.
An eighth objective is to provide a logic process for validating an unlock command.
A ninth objective is to provide a means for customizing the combination.
In a preferred embodiment of the present invention, an electro-mechanical control for a lock comprises a plurality of mostly tubular shafts journaled concentrically about a common axis. Each shaft is individually rotatable about the axis. Each inner shaft extends from its outer in both axial directions. A matching plurality of wheels is fixed to one end of each shaft. The wheels each have an aperture at a common radial distance from the common axis. A plurality of dials is fixed to the other end of each shaft to thereby manipulate each wheel. Each dial has a preferred orientation corresponding to an alignment of the apertures.
The preferred embodiment further comprises a means for indicating the preferred orientation for each dial. A light source is positioned at one end of the plurality of wheels at the common radial distance. The light source is connected to a source of power through a means for connecting. A photo sensor is positioned on the other end of the plurality of wheels to detect a beam of light from the light source passed through the aligned apertures. Finally, a means is provided for controlling the opening of the lock when the dials have been set to the preferred orientation.
In a particular preferred embodiment, a means is provided for determining whether each wheel rotation was clockwise or counterclockwise. In this case, the means for controlling the opening of the lock includes the preferred direction as well as the preferred orientation. This effectively doubles the number of combination permutations.
In another particular preferred embodiment, the plurality of concentric shafts is provided the additional degree of freedom to translate back and forth along the common axis. This translational movement facilitates a push-pull contact means for connecting, which means can be actuated by a push on the shafts when the last preferred orientation is set. Such a mechanism appreciably reduces power requirements.
In still another particular preferred embodiment, a pawl and detent mechanism is provided to positively indicate and hold registration of the orientation of each wheel. The detents are arrayed to facilitate the preferred orientation. The pawls, when mounted on beam springs, responsively retract the shafts and bias the contact to the open position.
This provides a positive locating mechanism and further facilitates the optimization of power by maintaining a pulse-like interval for contact.
In yet another particular preferred embodiment, the means for indicating is one or more features on each dial the juxtaposition of which presents in a particular visual pattern when in the preferred orientation. The feature could be a distinguishing physical feature or could be a selected color. This provides a visual means for recognizing a combination represented by the preferred orientations and avoids the dependence on a numerical sequence.
In still yet another particular preferred embodiment, a logic process for a microcontroller, serving as the means for controlling, is provided. The logic process comprises the steps of comparing a rotation direction from an initial instance in stored memory to a current instance from an electro-magnetic sensor for each rotation of each dial; storing the information in the event of a match and discarding the information in the event of a mismatch; comparing an instance of light detection from the photo sensor with stored event information; sending a command to unbolt the lock mechanism in the event of a match of a light instance with a set of stored direction instances equaling the plurality and ignoring the light instance in the event of a mismatch; and, erasing stored direction instances in either a match or mismatch event associated with a light instance.
As this is not intended to be an exhaustive recitation, other embodiments may be learned from practicing the invention or may otherwise become apparent to those skilled in the art.
DESCRIPTION OF THE DRAWINGS
Various other objects, features and attendant advantages of the present invention will become fully appreciated as the same becomes better understood through the accompanying drawings, in which like reference characters designate the same or similar parts throughout the several views, and wherein:
FIG. 1 is a front perspective view of the invention;
FIG. 2 is a back perspective view of the invention;
FIG. 3 is a side plan view of the invention;
FIG. 4 is a front plan view, illustrating a first embodiment of a visual means of indicating;
FIG. 5 is a front plan view, illustrating a second embodiment of a visual means of indicating;
FIG. 6 is an exploded perspective view of the invention;
FIG. 7 is a front perspective view of the invention, illustrating a means for customizing the preferred orientations;
FIG. 8 is a block circuit diagram, illustrating power and sensor connections; and
FIG. 9 is a logic process diagram for a microcontroller.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The following is a brief description of function and a presentation of a featured novel concept. Referring to FIGS. 1 and 2 , an electro-mechanical control 1 controls the opening of lock 2 (not shown). Lock 2 is a bolt or latch system which receives a signal from the electro-mechanical control 1 when preset parameters, otherwise known as a combination, are satisfied. Typically, these parameters are a set numbers dialed in a unique sequence. A novel feature of the present invention is to represent such a set of parameters in an easy to recognize and remember visual pattern. Such a pattern is shown in FIG. 1 , where dials 40 display indicator notches 46 in particular angular orientations. Two embodiments of visual pattern 43 are shown in head-on views in FIGS. 4 and 5 .
The pattern of the indicator notches 46 matches to an alignment of apertures 31 on wheels 30 , which are connected to dials 40 by shafts 20 ( FIG. 6 ). The alignment of apertures 31 permits light beam 52 ( FIG. 3 ) to be passed from light source 50 to photo sensor 60 . The receipt of the light beam 52 is the augment for passing a command to the lock 2 whereby an opening action is initiated.
Visual patterns, such as the one of FIG. 4 , are culturally ubiquitous. Orientations involving twelve index positions, for example, such as can be found on an analog clock face, are easily discriminated. In the instant example, the orientations read, from left to right, 11 o'clock, 12 o'clock and 1 o'clock. This reading would be apparent even without indicia markings, as evidenced by certain blank clock faces sold under designer names.
The following is a detailed description of the present invention. Referring to FIG. 6 , a collar 12 of chassis assembly 10 forms a housing for a plurality of shafts 20 . The shafts 20 , essentially of tubular construction, except for the innermost, assemble one inside another to form a concentrically-journaled composite. Each inner shaft extends from its outer in both directions along a common axis 21 ( FIG. 3 ). Each shaft 20 has a proximal end 23 and a distal end 22 . The distal ends 22 of the assembled shafts 20 are located in interior 13 of chassis assembly 10 , the proximal ends 23 extending outward therefrom. Each shaft 20 is individually rotatable about common axis 21 .
A particular multiplicity of index positions, such as twelve in the instant case, is represented by parallel grooves 24 in the exterior walls of shafts 20 . Wheels 30 assemble to shafts 20 in the interior 13 . Each shaft diameter is matched by a bore diameter in a corresponding wheel, and bosses 35 of wheels 30 are interposed with parallel grooves 24 when assembled to the cascaded extensions of distal ends 22 . The interposition of bosses and grooves couples the wheel to the shaft, similar to the splined-shaft couplings of common usage. In a similar manner as wheels, dials 40 with dial bosses 47 assemble to proximal ends 23 to form a unitary rotational element with wheel and shaft. Each wheel 30 has the aperture 31 positioned a common radial distance from common axis 21 .
The assembled components are shown in FIG. 3 . A translational degree of freedom is provided by a gap 55 , which is located both inside and outside of chassis assembly 10 . The gap permits an open position for a push-pull contact 54 . Push-pull contact 54 is closed by pushing on dials 40 to bridge gap 55 through the translation of shafts 20 , thereby providing means for connecting 53 . Means for connecting 53 links a power source 51 (not shown) to the light source 50 for an activation pulse. The power source 51 may be a battery 56 ( FIG. 9 ), such as a Direct Energy Conversion Cell (DEC) having a multi-year life span. The light source 50 may be an energy-conserving LED 57 ( FIG. 9 ), or any other battery-operated light emitter. The photo sensor 60 is positioned opposite the light source 50 , on the opposite side of wheels 30 , and in a line connecting light source 50 and apertures 31 . Photo sensor 60 may be a photo diode 62 ( FIG. 9 ), or similar light-sensitive receiver. Both light source 50 and photo sensor 60 may be hooded to selectively target the light source, thereby defeating any attempt to open the lock by “light flooding”. The outboard end of collar 12 , represented by mounting shank 15 , is an allowance for through mounting, such as through the wall of a safe. In the sense of FIG. 3 , all structure to the right of the shank 15 is external to the safe, and everything to the left is internal.
Referring to FIGS. 2 and 3 , wheels 30 have detents 33 on one facing. Detents 33 are evenly arrayed in a circle and match in number to the index positions embodied by the parallel grooves 24 . Pawls 36 , at the end of beam springs 34 , interface with the detents 33 such that the rotational position of each wheel 30 is positively registered. The beam springs 34 provide sufficient flex for the transition of wheels 30 from one detent position to another, snapping into the next detent when the corresponding dial is turned. In this manner, sequential settings may be made without disturbing a prior position, said position now held fixed by an engaged pawl and detent. The pawl and detent mechanism also provides for discrete dial locating so that angular discrimination is not left to judgment. Finally, beam springs 34 bias the push-pull contact 54 to the open position and instantly retract a push with a pull.
A means for determining rotation 80 is provided by electro-magnetic sensors 81 positioned on each beam spring 34 to read a magnetized wheel 82 . Magnetized wheel 82 may be wheel 30 comprised of a magnetic material, or wheel 30 may otherwise have a magnetic strip 84 applied or embedded ( FIG. 2 ). The electro-magnetic sensor detects whether a rotation is clockwise or counterclockwise. Using direction as a supplemental argument to position effectively doubles the possible combination permutations. In the instant case, the permutations would be 24×24×24, or 13,824. The electro-magnetic sensor 81 may be a Weigand sensor 83 ( FIG. 9 ), or any comparable sensor detecting direction of rotation.
A unique setting of dials 40 will correspond to an alignment of apertures 31 . A specific alignment 32 corresponds to preferred orientations 41 , as shown in FIG. 1 . Preferred orientations 41 demonstrate the visual pattern 43 of dials 40 . Referring to FIGS. 4 and 5 , visual pattern 43 may present as a array of physical feature 44 on each of the dials, such as the indicator notch 46 . Indicia plate 11 , having indicia markings 14 , may be used as a guide in setting the preferred orientation 41 . An alternate embodiment of visual pattern 43 is shown in FIG. 5 , where notches 46 display a unique set of colors 45 from a spectrum of color mounted on a facing surface behind. Referring to FIG. 7 , preferred orientations 41 can be customized by removing dials 40 from shafts 20 and repositioning them to correspond to a preferred pattern. The combination thus selected can be made permanent by bonding the outermost dial to in the innermost shaft, or otherwise fixing it thereto by known means, such as with a fastener.
Turning to FIG. 9 , a means for controlling 70 is represented by microcontroller 71 . Microcontroller 71 receives direction information 85 from Weigand sensors 83 and processes it as stored information 73 in EPROM memory 75 according to logic process 72 ( FIG. 10 ). Microcontroller 71 also receives light information 61 from photo diode 62 and issues a command 75 , following the logic process 72 , to unlock lock 2 . Command 75 may be an RF signal, or other appropriate notice means.
FIG. 10 illustrates logic process 72 . First decision 76 compares directional information 85 from a current instance to a saved initial instance. If there is a match, the event is passed as stored information 73 ; otherwise, it is discarded. Second decision 77 determines that there is a light event from light information 61 and passes this to third decision 78 . Third decision 78 determines that there is match to a complete set of current directional instances in stored information 73 . If there is a match, decision 78 issues command 75 . Whether a match or a mismatch, decision 78 dumps all current event information and requires a start over.
In the preferred embodiment, shafts 20 are comprised of extruded aluminum and fabricated by machining. Any non-ferrous metal material and any suitable fabrication process would suffice as an alternative. For cost reasons, chassis assembly 10 , wheels 30 and dials 40 are preferably injection molded. Aluminum fabrication for all components, however, except possibly in the case of the wheels where magnetization is required, would represent a more robust construction. The resins of choice would be ABS, Santoprene, or any polymer of comparable toughness and strength. In the preferred embodiment, a magnetic material would be molded as a fill material for wheels 30 . Alternatively, magnetic strips could be insert-molded, or otherwise applied as appliques. Further, insert molding could be used to embed conduction paths for the light and sensors, thereby avoiding wiring or other circuitry.
While a particular form of the invention has been illustrated and described, it will be apparent that various modifications can be made without departing from the spirit and scope of the invention. For example, a visual pattern of polarized lighting could be used for a means for indicating. Accordingly, it is not intended that the invention be limited, except as by the appended claims.
The light source and sensor are hooded, requiring the source to come only from the transmitter. This helps prevent opening the lock with ‘light flooding’. Also, a specific frequency of light and tuned sensor (IR, Near IR) can be used on a ‘trade secret’ basis | A light fence represented by aligned apertures in a plurality of wheels permits the passage of a light beam to a sensor to activate an electro-mechanical control for a lock. Such an arrangement avoids the sound-producing mechanical action of the typical tumbler lock and safeguards discovery of the opening combination. Rather than the typical case of a numerical sequencing combination, a novel approach is taken by using visual pattern recognition to align the apertures. The electro-mechanical control of the present invention additionally features optimized energy use, customizable settings, precision positioning, and an expansion of possible combination permutations by including direction of rotation. | 8 |
This application is a continuation of copending application Ser. No. 10/944,714, filed Sep. 21, 2004.
BACKGROUND OF THE INVENTION
Metal buildings having metal roofing have become popular for commercial, industrial and warehousing uses. These buildings often require roof openings for skylights, fans, air conditioning units and the like. The installation of such equipment requires a roof curb for support.
Traditionally, roof curbs have been designed specifically and custom made to provide a relatively horizontal mounting structure for a particular rooftop appliance given the shape and pitch of a particular roof. Designing and building these traditional roof curbs, often formed from a singular piece of metal to uniquely accommodate a particular roof pitch, has been a laborious and time consuming task for roof curb manufacturers and rooftop appliance installers. Further, because these roof curbs are installed in a metal roof system, the actual opening may vary with respect to the roof corrugations, seams or ribs, which may be ascertainable only shortly before installation. This untimely design-and-build practice delays appliance installation.
Manufacturers developed standardized roof curbs to help limit installation delays. See, for example, U.S. Pat. No. 4,559,753, issued Dec. 24, 1985, to Ralph H. Brueske, for Method of Installing a Prefabricated Curb Unit to a Standing Seam Roof, which describes a method of installing a metal roof curb in which the rims of the curbs are pre-welded to a roof panel, and the curb containing-panel is attached to a large opening cut into the roof. However, this method requires cutting a hole in the roof that is larger than the opening for the equipment that may be susceptible to leakage.
Prefabricated roof curbs tend to be quite large, thus have been difficult to ship in a cost effective and timely fashion, let alone by traditional rapid delivery methods. Consequently, roof curb manufacturers have had to ship their products by truck, which is slower and more expensive.
Traditional roof curbs include four coated steel curb walls positioned to define an open rectangular frame joined by factory welding at the corners. Because welding burns off the corrosion resistant coating of the steel, the manufacturer or installer must provide an additional coating of rust inhibitor paint to keep the roof curb from rusting when installed on the roof. Routine rust inhibitor paint coatings are required to protect the roof curb throughout the life of the product. Mechanical attachment, such as with threaded fasteners, may secure the corners without welding. However, on-site sizing and drilling of traditional roof curb panels creates exposure to corrosive weathering.
What is needed is a standardized, corrosion-resistant roof curb that can be shipped in a disassembled state, which an installer may assemble, size, locate and configure to provide an appropriate roof slope on any roof without welding.
SUMMARY OF THE INVENTION
The invention is a standardized, corrosion-resistant roof curb that can be shipped in a disassembled state, which an installer may assemble, size, locate and configure to provide an appropriate roof slope on any roof without welding.
The invention provides improved elements and arrangements thereof, for the purposes described, which are inexpensive, dependable and effective in accomplishing intended purposes of the invention.
Other features and advantages of the invention will become apparent from the following description of the preferred embodiments which refers to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described in detail below with reference to the following figures, throughout which similar reference characters denote corresponding features consistently, wherein:
FIG. 1 is an environmental perspective view of an embodiment constructed according to principles of the invention;
FIG. 2 is an exploded environmental perspective view of the embodiment of FIG. 1 ;
FIG. 3 is an environmental perspective view of a portion of the embodiment of FIG. 1 ;
FIG. 4 is a cross-sectional detail view drawn along line IV-IV in FIG. 2 ;
FIG. 5 is an environmental perspective view of another embodiment constructed according to principles of the invention;
FIG. 6 is an exploded environmental perspective view of the embodiment of FIG. 5 ;
FIG. 7 is a flow chart of a method of making the embodiment of FIG. 1 ;
FIG. 8 is a schematic representation of the embodiment of FIG. 7 ;
FIG. 9 is a flow chart of a method of making the embodiment of FIG. 5 ;
FIG. 10 is a schematic representation of the embodiment of FIG. 9 ;
FIG. 11 is a flow chart of a method of installing the embodiment of FIG. 1 ;
FIG. 12 is a schematic representation of the embodiment of FIG. 11 ;
FIG. 13 is a flow chart of a method of installing the embodiment of FIG. 5 ; and
FIGS. 14 a and 14 b are a schematic representation of the embodiment of FIG. 13 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIGS. 1-3 , an embodiment of a roof curb 100 configured according to the invention includes four walls 105 interconnected with four connection blocks 110 , defining a roof curb base 112 , for mounting on a roof R. Four composite boards 115 mount on walls 105 and support an appliance (not shown).
In practice, walls 105 are cut into standardized lengths that foster ready packaging in standard shipping containers along with other components described herein for conventional or overnight courier delivery. Aluminum extrusion stock permits on-site sizing of the standard pieces without local burning off of corrosion resistant coatings ordinarily required for steel stock. Using aluminum stock also eliminates routine rust inhibitor paint coatings that would be required to protect steel stock.
Referring also to FIG. 4 , each wall 105 is constructed of extruded aluminum having a lower flange 120 and an upper channel 125 . Each flange 120 is inwardly-disposed to limit exposure of fasteners and other mounting mechanisms and sealing to the elements. Each flange 120 has chamfered ends 130 that promote flushness along the entire contacting surface of flange 120 with roof R.
Each channel 125 is configured to receive and retain a composite board 115 . Channels 125 are inwardly disposed so as to define, in conjunction with wall 105 , a generally uniform vertical wall 127 without ledges or partial enclosures that might find favor with unwanted insects and vermin.
Flange 120 , vertical wall 127 and channel 125 define a pocket 128 for receiving insulation, as described below.
Side walls 105 a have an edge 107 a that provides a continuous, water-tight seal with roof R. Top and bottom walls 105 b have notches 109 for alignment with and accommodation of seams or ribs F extending from roof R, thus defining an edge 107 b that also provides a continuous, water-tight seal with roof R.
Referring to FIG. 3 , each connection block 110 is constructed from aluminum and has pre-drilled through bores 114 at predetermined locations. In practice, a roof curb installer introduces holes at the ends of walls 105 according to a template, as shown in FIG. 8 , that register with through bores 114 .
Preferably, composite boards 115 are Trex® boards, which are constructed from a combination of reclaimed wood and plastic. The plastic component shields the wood component from moisture and insect damage, reducing or eliminating rotting or splintering. The wood component protects the plastic component from ultraviolet radiation damage from ordinary sunlight, ensuring integrity longer than would be expected from products constructed from purely plastic or purely wood.
As shown in FIG. 2 , unique to roof curb 100 is a top support channel 135 . Top support channel 135 is similar to bottom support channel 140 , which is common to roof curb 100 and roof curb 200 , as shown in FIG. 6 . Top support channel 135 and bottom support channel 140 each have generally perpendicular ribs 136 and 141 , respectively. Ribs 136 , 141 strengthen and enhance top support channel 135 and bottom support channel 140 load bearing capabilities.
Top support channel 135 has flanges 137 and bottom support channel 140 has flanges 143 that mount onto structural members S supporting roof R. When installed, top support channel 135 and bottom support channel 140 each support a wall 105 b , and support members S support the remaining walls 105 a .
Referring to FIGS. 5 and 6 , another embodiment of a roof curb 200 configured according to the invention provides for diverting water that otherwise might accumulate along the upper, laterally-extending intersection of roof R and roof curb 200 . The water diverting feature of roof curb 200 is intended for larger installations that would be susceptible to collecting large amounts of water. Roof curb 200 includes four walls 205 interconnected with four connection blocks 210 , defining a roof curb base 212 , that mounts on roof R. Four composite boards 215 mount on walls 205 and support an appliance (not shown). Roof curb 200 is similar to roof curb 100 , except as described below.
As shown in FIGS. 5 and 6 , unique to roof curb 200 are a diverter plate 235 and a diverter angle 245 . Diverter plate 235 covers a portion of roof R removed so that ribs F in roof R do not prevent flush mounting of diverter angle 245 on roof R against roof curb 200 . Like top support channel 135 , diverter plate 235 has strengthening ribs 236 for supporting wall 205 and diverter angle 245 .
Diverter angle 245 has upstanding flanges 247 that define an impervious dihedral angle 249 . Angle 249 is such that flanges 247 provide a flow path for water to pass around roof curb 200 , rather than collect against the upwardly disposed wall 205 , which, over time, might cause local corrosion or sealant failures. Diverter angle 245 is sealingly connected to diverter plate 235 . In operation, water flowing down roof R toward roof curb 200 would encounter then flow along flanges 247 , then onto the portion of roof R lateral to roof curb 200 , thereby bypassing roof curb 200 and continuing to flow down roof R.
Referring to FIG. 7 , an embodiment of a method of making 300 roof curb 100 configured according to the invention includes: a step 305 of determining curb size; a step 310 of cutting extrusions; a step 315 of cutting bottom extrusion; a step 320 of cutting steel channels; a step 325 of drilling corner connections; a step 330 of applying corner block mastic; a step 335 of assembling extrusion corners; a step 340 of determining composite board dimensions; and a step 345 of cutting composite boards.
Referring also to FIG. 8 , step 305 involves determining a curb size to ascertain a curb length for walls 105 a , as shown in FIG. 1 , and a curb width for walls 105 b , top support channel 135 and bottom support channel 140 , as shown in FIG. 2 .
Step 310 involves cutting the side extrusions or walls 105 a according to the curb length of step 305 . Preferably, a roof curb assembler uses a 12-inch compound-sliding miter-saw with a carbide tooth blade for cutting aluminum. Mitering the interfaces among walls 105 promotes relative flushness as well as flushness with respect to roof R.
Step 315 involves cutting the top and bottom extrusions or walls 105 b according to the curb width of step 305 . Step 315 differs from step 310 in that a roof curb assembler must cut walls 105 b so as to accommodate seams or corrugations in roof R.
Step 320 involves cutting top support channel 135 and bottom support channel 140 according to the curb width of step 305 . Preferably, a roof curb assembler uses an angle grinder with cutoff blade. Top support channel 135 and bottom support channel 140 also may require notching to accommodate roof support structures.
Step 325 involves aligning a template relative to and drilling pilot holes through walls 105 so as to register with through bores 112 in connection blocks 110 . A roof curb assembler temporarily maintains relative positioning of the template and walls 105 with a locking C-clamp. The roof curb assembler drills two 5/16-inch diameter holes at each end of each of walls 105 .
Step 330 involves applying a 5/16-inch diameter bead of gun grade sealant, preferably Panlastic, to the top, bottom and corner of each of corner blocks 110 with a caulking gun. This provides roof curbs 100 and 200 with an integral water-tight seal that is superior to post-installation sealant treatments common to other roof curbs.
Step 335 involves driving ¼-inch×½-inch phillips head bolts through the holes in walls 105 and corner connection blocks 110 . Tightening the bolts urges walls 105 and corner connection blocks 110 to come together, and urges the mastic applied to corner connection blocks 110 at step 330 to flow into any gaps, thereby sealing the joint.
Step 340 involves determining the slope or pitch of roof R, and an appropriate measurement for the “X” dimension shown in FIG. 8 , corresponding to the pitch so that composite boards 115 provide a generally level mounting area for an appliance (not shown). The “Y” dimension is fixed, preferably at 5-½ inches. Preferably, stock Trex® boards 115 for cutting are 5/4-inch×6-inches.
Step 345 involves using a circular, table or radial-arm saw equipped with a wood-cutting carbide blade to cut stock Trex® boards 115 as required to fit tightly in channels 125 .
Referring to FIG. 9 , an embodiment of a method of making 500 roof curb 200 configured according to the invention includes: a step 505 of determining curb size; a step 510 of cutting extrusions; a step 515 of cutting bottom extrusion; a step 520 of cutting steel channels; a step 523 of cutting diverter plate; a step 525 of drilling corner connections; a step 530 of applying corner block mastic; a step 535 of assembling extrusion corners; a step 540 of determining composite board dimensions; and a step 545 of cutting composite boards.
Referring also to FIG. 10 , method of making 500 is substantially identical to method of making 300 except for an additional step 523 . Step 523 involves cutting diverter plate 235 according to the curb width determined at step 505 , which is similar to step 305 . A roof curb assembler must cut diverter plate 235 so as to accommodate seams, corrugations or ribs F in roof R. Specifically, holes in diverter plate 235 must align with ribs F.
Referring to FIG. 11 , an embodiment of a method of installing 400 roof curb 100 configured according to the invention includes: a step 405 of marking roof for cutout; a step 410 of placing walkboards for support; a step 415 of cutting panel; a step 420 of installing side support channels; a step 425 of installing rear support channel; a step 430 of applying mastic for curb; a step 435 of installing curb base; a step 440 of cleaning area; a step 445 of applying sealant; a step 450 of applying mastic; a step 455 of installing composite boards; a step 460 of applying foam tape and sealant at board joints; a step 465 of cutting out insulation; and a step 470 of installing retainers.
Referring also to FIG. 12 , step 405 involves placing roof curb 100 , as assembled above, onto the portion of roof R where an appliance is desired. Bottom wall 105 b should vertically register with supporting structural purlin. A minimum 6-inch distance should exist between top wall 105 b and the upper supporting structural purlin. A roof curb installer then traces along the interior of flanges 120 of roof curb 100 with a standard lead or grease pencil.
Step 410 involves disposing boards or paneling, having sufficient strength to maintain a roof curb installer's weight on roof R, just outside of the tracing generated in step 405 , proximate to where the roof curb installer will cut roof R.
Step 415 involves drilling ½-inch starter holes in roof R at each corner of the tracing of step 405 , then using a double-cut shear, which minimizes shavings and chips, to cut roof R along the tracing. A roof curb installer will need a reciprocating saw to cut through corrugations in roof R.
Step 420 involves sizing and temporarily clamping in place side support channels on top of any insulation and between the upper supporting structural purlin and lower supporting structural purlin, just outside of the lateral edges of the hole in roof R generated at step 415 .
Step 425 involves sizing and temporarily clamping in place a bottom support channel between the side support channels installed in step 420 , just outside of the bottom edge of the hole in roof R generated at step 415 .
Step 430 involves inserting lockseam plugs on the bottom corrugations occurring along the bottom edge of the hole in roof R generated at step 415 . Once installed, the lockseam plugs may be filled with mastic. A roof curb installer applies ⅛-inch×½-inch Panlastic tape over the lockseam plugs around and aligned with the edges defining the hole in roof R. The tape should be butted, not lapped, at corners. Finally, the roof curb installer applies a continuous bead of sealant on top of the tape.
Step 435 involves positioning roof curb 100 over the prepared hole in roof R and securing flanges 120 of roof curb 100 to the support channels with self-drilling ¼-inch×⅞-inch metal screws at six-inch intervals.
Step 440 involves sweeping or vacuuming away all metal chips and shavings.
Step 445 involves applying a continuous bead of sealant around the intersection of roof R and roof curb 100 .
Step 450 involves applying gun grade mastic in the outer corner of channels 125 of walls 105 and to the butt ends of composite boards 115 .
Step 455 involves attaching composite boards 115 to walls 105 with self-drilling ¼-inch×⅞-inch metal screws, and to adjoining composite boards 115 with self-drilling #6×2-inch screws.
Step 460 involves applying sealant along the joint between walls 105 and composite boards 115 . The roof curb installer then applies foam tape on the top surfaces of the composite boards 115 .
Step 465 involves trimming a four-inch wide roll of insulation from building scrap. The roof curb installer places the insulation in pocket 128 in walls 105 defined by channel 125 , vertical wall 127 and flange 120 , as shown in FIG. 4 . Temporary adhesive may aid in retaining the insulation in pocket 128 . The roof curb installer then slits the building insulation from each roof curb corner inwardly, then removes the insulation from the facing. The roof curb installer folds the facing up each inner side of roof curb 100 and secures the folds thereto with retainers and self-drilling screws. The roof curb installer then tapes each corner to seal vapor retarder completely.
Referring to FIG. 13 , an embodiment of a method of installing 600 roof curb 200 configured according to the invention includes: a step 605 of marking roof for cutout; a step 607 of marking roof for diverter plate; a step 615 of cutting panel; a step 620 of installing side support channels; a step 625 of installing rear support channel; a step 627 of preparing diverter plate; a step 628 of installing diverter plate; a step 630 of applying mastic for curb; a step 635 of installing curb base; a step 637 of preparing diverter angle; a step 638 of installing diverter angle; a step 640 of cleaning area; a step 645 of applying sealant; a step 650 of applying mastic; a step 655 of installing composite boards; a step 660 of applying foam tape and sealant at composite board joints; a step 665 of cutting out insulation; and a step 670 of installing retainers.
Referring also to FIGS. 14A and 14B , method of installing 600 is substantially identical to method of installing 400 except for steps 607 , 627 , 628 , 637 and 638 . Step 607 involves placing diverter plate 235 adjacent to the top edge of the tracing generated in step 605 , which is similar to step 405 , and tracing around diverter plate 235 .
Step 627 involves attaching corrugation plugs to diverter plate 235 over the holes aligned with ribs F in roof R. The roof curb installer applies tape Panlastic over the side and outer edges of diverter plate 235 , being careful to butt and not lap the ends, so that a minimum of ¼ inch is exposed around the panel cut out. The roof curb installer applies gun grade mastic over the tape Panlastic.
Step 628 involves placing diverter plate 235 in the cutout in roof R so that corrugation plugs snugly fit in the corrugations in roof R. Self-drilling threaded fasteners secure diverter plate to roof R. Mastic must be applied around holes on the bottom side of the panel strips.
Step 637 involves applying a 5/16-inch bead of mastic to the back and ⅛-inch×1½-inch tape Panlastic to bottom of diverter angle 245 , then positioning diverter angle 245 against roof curb 200 on roof R.
Step 638 involves securing diverter angle 245 to roof curb 200 and roof R with self-drilling threaded fasteners.
The invention is not limited to the particular embodiments described herein, which should be understood to be merely illustrative of the invention defined by the following claims. | A roof curb is shipped in a disassembled state to an installer who assembles, sizes, locates and configures the curb to accommodate slope on any roof without welding or metal cutting. The curb includes an aluminum walls, each having a channel for receiving the bottom edge of a board, which may be taper cut according to the pitch of the roof to provide a level surface for supporting an appliance. Methods of making and installing the roof curb also are disclosed. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of U.S. Ser. No. 09/166,336, filed Oct. 5, 1998, which issued on Dec. 19, 2000 as U.S. Pat. No. 6,161,339.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable
BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION
This invention relates to arrangements for securing the roof of a structure against damage caused by high winds, earthquakes, and the like.
BACKGROUND INFORMATION
It is known to reinforce a building wall to resist wind and earthquake damage by the use of what will hereinafter be called a “top plate tie down” arrangement in which vertically disposed elongate fastening members that can be loaded in tension (e.g., a threaded metal rod) connect a top plate of the protected wall to an anchor beneath the wall, where the anchor is fixedly attached to a slab or is buried in or otherwise attached to the ground. As described in a parent application now issued as U.S. Pat. No. 6,161,339, a satisfactory anchor for such apparatus may be set in position prior to pouring a concrete foundation slab. The anchor can then be used both to retain a sill plate and to connect an elongate top-plate fastener to the foundation.
The use of conventional embedded anchors can lead to problems in installing a top plate tie down system if the anchors are not embedded at the proper positions along a sill or if the anchors are not set in a fully upright position. Because it is difficult to ensure that a correctly oriented anchor is located at each position where a top plate elongate fastener is to be installed, many builders would prefer to fasten anchors to an already hardened slab.
It is known, for example, to anchor a sill plate to a slab by driving through the sill plate into the slab and then gluing (e.g., with an epoxy cement) an anchor into the hole formed in the slab. If dust from the drilling operation is not carefully removed from the hole before inserting an epoxy-enrobed anchor, this approach results in an anchor with a very low pull-out strength. Although such an anchor may be satisfactory for retaining a sill plate against lateral forces, it can not safely be used as part of a top plate tie down apparatus. Glued, or otherwise bonded, anchors are generally not acceptable for top plate tie down use because of both the high likelihood of there being at least one dust-contaminated and weakened anchor along a wall, and because of the time and expense involved in running a separate pull-out test on each anchor.
Expansion-type anchors are widely used when a high pull-out strength connection must be made to a masonry support. Because this sort of anchor induces a high lateral stress in the masonry, it can cause portions of a masonry body to spall off if the anchor is placed too near a free edge of the body. Top plate tie-down arrangements are, of course, installed on exterior walls near the edge of a foundation slab. Hence, expansion anchors can not be used.
Self-tapping threaded masonry anchors are of interest to the present invention. Notable among commercially available hardware of this sort products sold under the trade name “Wedge-Bolt” by Powers Fasteners, Inc., of New Rochelle, N.Y. Patent references in this technical area include:
U.S. Pat. No. 5,674,035, wherein Hettich et al. teach a thread forming screw having ratios of the sizes of various portions of the screw selected to reduce screw-in torque;
U.S. Pat. No. 5,531,553, wherein Bickford describes a masonry anchor having a dust-relief groove disposed between thread lands; and
U.S. Pat. No. 4,439,077, wherein Godsted discloses a threaded fastener for use in hard aggregates.
BRIEF SUMMARY OF THE INVENTION
The invention provides an improved anchor for a top plate tie down arrangement comprising a plurality of elongate vertical fasteners attached between the top plate and respective anchors disposed beneath the wall. In a preferred embodiment the anchor comprises a stud having one end adapted to be threaded into a concrete foundation slab and a second end threaded to receive a coupling nut for attaching the stud to a respective elongate vertical fastener.
It is an object of the invention to provide a top plate tie down apparatus connecting a top plate of a wall to a concrete foundation. As is conventional in construction practice, the wall extends upward from a sill plate placed on the concrete foundation and having a plurality of generally vertical throughholes through it, where the throughholes can be formed either before or after placement of the sill plate on the sill. The inventive apparatus preferably comprises a selected number of anchors, where the number of anchors is generally selected to match the number of throughholes in the sill. Each of these anchors has a respective portion threadably engaging the foundation beneath the wall along an embedment length of the anchor, each anchor has a respective upper portion threaded along at least a selected penetration length that is selected to accord with the accessible threaded depth of a connecting nut, and each of the anchors has a length equal to a sum of the penetration length, the sill thickness and the embedment length. In addition, the preferred apparatus comprises the selected number of vertical tensile fasteners, where each of the vertical tensile fasteners is connected to the top plate—e.g., by means such as those shown in the parent application hereto. Each of these vertical tensile fasteners further comprises a respective lower threaded portion at a respective lower end thereof, where each of the lower threaded portions has a selected lower portion thread length that, like the thread length on the anchor, is selected to accord with a connecting nut Each of the connecting nuts has a length at least as large as the sum of the penetration length and the selected lower portion thread length and has a first end threaded onto a respective one of the anchors, and a second end threaded onto the respective lower threaded portion of a respective one of the vertical tensile fasteners.
It is an additional object of the invention to provide a method of attaching a top plate of a wall to a slab disposed beneath the wall. The preferred method begins with a step of drilling a selected number of holes into the slab, where each of the holes extends into the slab by more than an embedment length of an anchor bolt, and preferably by about one bolt diameter more than the embedment length. An anchor bolt is then inserted through a throughhole in a sill plate into each of these holes and turned so as to thread the anchor bolt into the hole. In the preferred method a connecting nut threaded onto an upper threaded portion of each anchor bolt provides a set of flat surfaces that can be gripped by a wrench and used to turn the bolt into the hole. Moreover, it is also preferred to place a washer between the connecting nut and the sill plate before turning the bolt into the hole so as to effectively capture the sill plate between the connecting nut and the slab without deforming the sill plate. It will be understood by those skilled in the art that this method can be carried out by the use of a sill plate that has pre-drilled throughholes, or by drilling through the sill plate when drilling the hole into the slab.
Although it is believed that the foregoing recital of features and advantages may be of use to one who is skilled in the art and who wishes to learn how to practice the invention, it will be recognized that the foregoing recital is not intended to list all of the features and advantages. Moreover, it may be noted that various embodiments of the invention may provide various combinations of the hereinbefore recited features and advantages of the invention, and that less than all of the recited features and advantages may be provided by some embodiments.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
FIG. 1 is an elevational view taken perpendicular to a framed wall and showing a plurality of roof framing members transverse to the wall anchored to a foundation beneath the wall.
FIG. 2 is a partly cut-away elevational detail view of an anchor embedded in the foundation.
FIG. 3 is a partly cut-away elevational view of a preferred anchor.
DETAILED DESCRIPTION OF THE INVENTION
Turning now to FIG. 1, one finds a wood framed wall 10 standing on a concrete foundation slab 12 and having a tie down apparatus 13 added thereto. The wall 10 may comprise a sill 14 or foot member laid upon the foundation 12 and bolted thereto; a plurality of vertically disposed framing members 16 or studs, and a top plate 18 that is fastened across the top of the studs 16 . A roof 20 , conventionally supported by the wall 10 , comprises a plurality of roof framing members 22 transverse to the wall 10 and above the top plate 18 . Although the preferred embodiment is depicted with reference to a wooden framed wall, other sorts of wall construction may also be employed. For example, a metal framed wall, of the type commonly used in commercial building construction could be employed. So, for that matter, could a concrete block or brick wall having a top plate 18 disposed thereupon. Moreover, although the invention is herein described and depicted with respect to an exterior wall of a building, the same arrangement could clearly be applied to an interior wall crossed by one or more roof members.
It is conventional in wall construction for a foundation 12 to be made with a selected number of anchors 30 set into the slab. These anchors are spaced out along a line for the purpose of bolting the sill 14 to the foundation 12 . One approach to doing this is to insert a plurality of anchors 30 into the wet concrete of the foundation 12 before the concrete has set. Another is to suspend a plurality of anchors from a horizontal board positioned at the top of the pouring frame and to then pour concrete over the suspended anchors. The bottom end of each anchor 30 is configured to extend laterally outwards (e.g., by clamping a washer 32 between two nuts 34 , or by providing a elbow-like bent portion 36 ) so that the anchor 30 can not be pulled out of the foundation 12 . The plurality of anchors 30 are spaced out along the centerline of the wall 10 , and a corresponding plurality of throughholes are cut into the sill 14 so that when the sill 14 is placed upon the foundation 12 a threaded upper end 38 of a respective anchor 30 projects through each hole. A washer 32 and nut 34 are then put on each anchor 30 in order to secure the sill 14 to the foundation 12 . In an embodiment of the invention disclosed in parent application 09/166,336, now issued as U.S. Pat. No. 6,161,339, similar arrangements are used, but the anchors 30 are selected to have a threaded upper end 38 projecting somewhat higher above the sill than would be the case for a conventional wall so that a connecting nut 40 can be used to connect each anchor 30 to a respective vertical rod 42 portion of the tie down apparatus 13 . That is, the anchor 30 of the preferred embodiment serves both the conventional purpose of bolting the sill to the foundation, as well as serving as part of a means of tying the top plate 18 to the foundation 12 .
In an embodiment described in parent application 09/166,336, now issued as U.S. Pat. No. 6,161,339, the vertical rod has a threaded region 43 on its lower end. The length of the threaded region is selected to be a bit less than half the length of a connecting nut 40 . In one embodiment the connecting nut 40 is one and three quarters inches long and has an internal stop 51 formed by punching a portion of the connecting nut's wall inward so as to limit the penetration depth of a screw thread to be no more than three quarters of an inch. In this case a threaded region 43 having a length of three quarters of an inch is provided on the rod. A worker assembling this tie down apparatus 13 is instructed to initially fully thread the connecting nut 40 to the rod 42 . The rod 42 is then placed vertically above the anchor 30 , and the connecting nut 40 is threaded onto the upper end 38 of the anchor 30 by turning the rod 42 . This assures that the same number of threads on each of the two threaded regions 38 , 43 are captured by the nut so as to provide the strongest possible connection. Prior art top plate bolting arrangements employing a rod threaded along its entire length did not provide this means of assuring that the rod and anchor are joined in a maximum strength configuration. Those prior art arrangement allowed a worker to assemble a connection that is acceptable to all outward appearances, but that is seriously weak because only one thread is engaged on either the rod or the anchor.
In a preferred embodiment, as depicted in FIG. 3, a threaded anchor 24 is turned into a hole 26 drilled into a hardened foundation slab 12 so as to capture a sill plate 14 between a connecting nut 40 and the slab 12 . In one particular case the threaded anchor 24 has an overall length of about nine inches. At one end of this anchor there is a embedment length portion 44 about six inches in length that has a nominal half inch self-tapping lead thread formed on it. The lead thread preferably comprises a helical land having a relatively high helix angle and a helical dust relief groove formed in the body of the anchor. At the other, upper, end there is a second threaded portion 38 adapted to engage a connecting nut 40 . This portion generally has a length about one half the length of an associated connecting nut and may, for example, be about three quarters of an inch long with a {fraction (7/16)}×12 thread. In a preferred embodiment an unthreaded intermediate portion 49 of the anchor has a length approximately the same as the thickness of lumber used for forming a sill plate 14 . As depicted, the preferred arrangement accommodates a washer 32 between the connecting nut 40 and the sill plate. In the exemplar case, the intermediate portion 49 has a length of about one and three quarters inch. It will be understood by those skilled in the art that as long as enough of the upper portion of the anchor is threaded, the penetration depth of the anchor into the connecting nut is limited by an internal stop 51 in the middle of the connecting nut, and not by the threaded length of the upper portion, Hence, it is really not important whether the intermediate portion of the anchor is threaded or not. In any event, as long as the hole is deep enough, the overall length of the self threading anchor will be approximately equal to the sum of the penetration depth of the anchor into the connecting nut, the sill thickness and the embedment length.
To install the preferred self-threading anchor 24 , a hole is drilled through the sill plate and into the concrete slab, preferably by using a special drill bit designed for drilling pilot holes for fasteners that have the self tapping lead thread on the anchor. The preferred hole extends into the slab to a depth of about one anchor bolt diameter (e.g., one half inch) longer than the embedment length 44 of the anchor, and is preferably cleaned (e.g., by means of one or more blast(s) of compressed air) before the anchor 24 is inserted. A connecting nut 40 having a limited thread extent (e.g., that has a detent or other center stop 51 ), is turned onto the end of the anchor that will be uppermost after installation, a washer 32 is placed around the anchor shaft, and the anchor 24 is turned into the hole so as to tightly capture the sill plate 14 between the washer 32 and the foundation 12 .
In the top plate tie down system taught in parent application 09/166,336, now issued as U.S. Pat. 6,161,339, a cable 60 disposed above the top plate 18 is tensed by tightening a respective turnbuckle 48 on each of a plurality of rods 46 . In an arrangement of this sort, if any one of the anchors disposed along a wall pulls out of the slab, the tension in the cable 60 is relaxed. Hence, it is important that each anchor be reliably tied to the slab.
It is easy to test the preferred anchoring arrangement disclosed above to ensure that each and every anchor is secure. Inspection of the anchor is a two-step process in which the inspector first checks to see that the washer 32 is not loose and then tries to apply a test torque to the connecting nut with a pre-set torque wrench. If the connecting nut does not turn responsive to the test torque, the inspector can conclude that the embedment portion of the anchor is securely engaging the slab.
From the foregoing, it can be seen that the invention provides a preferred method of securing a wall to a foundation so as to resist severe wind loads and other stresses tending to detach the roof from the wall, the method comprising the steps of:
a) inserting each of a selected number of anchor bolts into respective holes drilled into a hardened foundation slab so that each anchor bolt presents a vertically oriented threaded upper end extending above a sill. These anchor bolts are spaced out along the center line of the wall and extend through respective throughholes in the sill.
b) tightening each anchor bolt, by means of a respective connecting nut threaded onto the threaded upper end, so that the sill is captured between the connecting nut and the foundation slab;
c) threadably connecting a rod having a length less than the distance between the sill and a top plate of the wall to the upper end of each anchor bolt by means of the respective connecting nut.
d) connecting each rod to tie-down apparatus above the top plate.
Although the present invention has been described with respect to several preferred embodiments, many modifications and alterations can be made without departing from the invention. Accordingly, it is intended that all such modifications and alterations be considered as within the spirit and scope of the invention as defined in the attached claims. | Top plate tie-down arrangements are used for securing the roof of a structure against damage caused by high winds, earthquakes, and the like by anchoring the top plate of a wall to a foundation slab. An anchor for use in a top plate tie-down arrangement has a self-tapping thread on one end that allows it to be threaded into a hole drilled into the slab. The upper end of the anchor, which protrudes through a sill plate, is threaded to engage a connecting nut that ties the anchor to an elongated vertical fastener attached to the top plate. The lengths of various portions of the anchor and of the hole into which it is threaded are selected so that the sill plate is captured between the connecting nut and the slab. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This patent application claims priority under 35 U.S.C. §120 to and is a continuation application of previously filed U.S. patent application Ser. No. 11/597,189, filed Nov. 21, 2006, the entire disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to an apparatus for the filtration of liquids. The invention also relates to a filter cartridge for an apparatus of this type.
2. Description of the Related Art
Filter cartridges are to be understood as meaning on the one hand cartridges which have a screen-like formation for mechanical filtration. On the other hand, filter cartridges are also to be understood as meaning cartridges which, in addition to a screen-like formation, contain at least one filter medium, e.g. in granule form, which is used for the chemical and/or mechanical removal of organic and/or inorganic contaminants and/or to lower the levels of such contaminants. Filter cartridges equipped in this way therefore allow non-mechanical filtration, which may be combined with mechanical filtration. These filter cartridges are used to optimize water, the term optimization being understood as meaning mechanical and/or non-mechanical filtration. This includes, for example, softening and decalcification of drinking water.
A very wide range of embodiments of apparatuses for the filtration of liquids are known.
By way of example, there are filter apparatuses with spherical filter cartridges, which are screwed onto the inlet funnel from below by means of a bayonet catch, as described in WO 2004/014519 A2.
DE 199 05 601 A1 has disclosed an apparatus for the treatment of liquids, having an inlet funnel which has a receiving opening with a sealing rim. The filter cartridge is likewise fitted into the receiving opening from below and is pressed into the receiving opening by means of a separate securing ring. For this purpose, the filter cartridge is provided with a groove on the cartridge upper part below the sealing rim; the lower portion of the securing ring engages in this groove. The upper portion of the securing ring is guided in a groove of a connection piece formed integrally on the funnel base. The filter cartridge is complex to install and remove, requiring particular skill on the part of the operator.
Other embodiments provide for the inlet funnel to have, in its base wall, a receiving opening, into which the filter cartridge is fitted from above. The filter cartridge generally has a conical sealing rim, which bears against the edge of the receiving opening. The filter cartridge may become tilted during insertion, so that the intended sealing position is not adopted.
DE 199 158 29 A1 has disclosed a filter cartridge and an apparatus for treating liquids, in which the sealing rim has additional latching means, which interact with corresponding latching means in the region of the opening in the base of the inlet funnel. The latching means are brought into engagement with one another by a rotational movement.
In this embodiment, the filter cartridge is held only at the edge and is located in the filtrate space. If the apparatus is a kettle, therefore, the filter cartridge is also in the boiling space, which means that the filter cartridge could be damaged during the heating of the filtered liquid. Therefore, it is desirable for the filter cartridge to be arranged such that it is shielded from the filtrate space or boiling space.
Inlet funnels with a receiving chamber for the filter cartridge are used to remedy this problem. In this design too, the conical sealing rim of the filter cartridge bears against the rim of the receiving opening in the base wall of the inlet funnel.
The peripheral and base wall of the filter cartridge is arranged at a distance from the peripheral and base wall of the receiving chamber, so that during filtration, although filtered liquid can collect in this intermediate space, this liquid does not limit the quantitative flow through the apparatus. An outflow opening provided with a closure element is located in the base wall of the receiving chamber.
DE 198 46 583 A1 has disclosed a water filter device of this type, with a collection can and a heating element. The inlet funnel has a receiving chamber, into which the filter cartridge is fitted from above. The receiving chamber is formed by a filter insert, which may be fixedly connected to the inlet funnel or can be fitted into the receiving opening. The filter insert is matched to the conical shape of the filter cartridge and forms a guide element for the filter cartridge. Since the peripheral wall of the filter cartridge bears against the filter insert over its full surface, the two components can only be separated from one another with difficulty, in particular if the user pushes the filter cartridge too deep into the filter insert. On account of the fact that two conical surfaces are sliding along one another, it is not clear to the user when he has reached the limit position which is required for optimum seating of the filter cartridge and defines the sealing position of the filter cartridge.
U.S. Pat. No. 4,020,350 describes a filter system which is connected to a water pipe via two connections. The filter system comprises a housing upper part and a housing lower part, which are screwed together after the filter cartridge has been fitted. The cover and base wall of the filter cartridge have cup-shaped indentations, in which correspondingly shaped connection pieces of the housing parts for supplying the unfiltered liquid and removing the filtered liquid, engage. To change the filter cartridge, the two housing parts have to be unscrewed.
In all the known filter apparatuses, it is necessary for the filter cartridge to be matched to the desired quantitative flow.
BRIEF SUMMARY OF THE INVENTION
It is an object of the invention to provide a filter cartridge and an apparatus for the filtration of liquids with which correct seating of the filter cartridge is ensured and can be established by the user.
This object is achieved by an apparatus in which the inlet funnel has at least one first fixing means below the receiving opening, and the filter cartridge has at least one second fixing means below and at a distance from the sealing rim; when the filter cartridge is being fitted into the receiving opening, the at least one second fixing means interacts with the first fixing means.
The filter cartridge can preferably be fitted into the receiving opening in its axial direction.
The fixing means are arranged in such a manner that during interaction they define the sealing position of the filter cartridge, i.e. when the fixing means interact, the sealing rim of the filter cartridge in its intended position bears against the edge of the receiving opening.
The interaction of the fixing means is associated with a resistance, which is perceptible to the user when he is fitting the filter cartridge and indicates to the user that the intended position of the filter cartridge has been reached.
Since the fixing means define the sealing position of the filter cartridge, it is advantageous if the distance between sealing rim and fixing means is selected to be as great as possible. This prevents the filter cartridge from tilting or being incorrectly positioned.
Therefore, the second fixing means are preferably arranged on the lower half, preferably in the bottom third, of the filter cartridge, in particular in the region of the base wall of the filter cartridge.
The first and/or second fixing means may be spacer elements and/or guide elements and/or latching elements. This means that a fixing means can perform one or more functions, and that it is also possible for a plurality of fixing means of different configurations to be realized in an apparatus.
The fixing means are preferably projections or recesses. The projections or recesses may be cylindrical, conical or frustoconical in form. These forms also include, for example, indentations and protuberances or beads.
In the case of latching elements, latching bosses, latching recesses or annular beads are preferred.
In the simplest case, the fixing means may be spacer elements. By way of example, at least one outwardly facing projection may preferably be formed integrally on the base wall of the filter cartridge as second fixing means, which projection, during fitting of the filter cartridge, is seated on a holding element which is arranged on the inlet funnel and forms the first fixing means.
The first fixing means may, for example, also be the base wall of a receiving chamber arranged at the inlet funnel.
Conversely, by way of example, it is also possible for the holding element, which may form the base wall of the receiving chamber, to have at least one inwardly facing projection, which interacts with the base wall of the filter cartridge, which in this case forms the second fixing means.
The fixing means may also be guide elements, which means that the filter cartridge is guided into its intended position when it is being fitted. By way of example, projections and recesses, in particular indentations on the filter cartridge and on the holding element which, by way of example, may be cylindrical, conical or frustoconical in form, are suitable for this purpose.
According to a further embodiment, the fixing means may also be latching elements which engage in one another as they interact. The latching or snapping into place is generally associated with a noise which indicates to the user that the filter cartridge has reached its intended position.
The fixing means are preferably matched to one another in such a manner that fitting the filter cartridge in the axial direction is sufficient to bring the fixing means together. Therefore, there is no need either for rotary, tilting or other movements of the filter cartridge or for additional components, such as securing rings or the like, which overall makes insertion of the filter cartridge user-friendly.
Furthermore, the fixing means are matched to one another in such a manner that they can be detached from one another without particular effort when the filter cartridge is being exchanged.
This is achieved, inter alia, by the contacting surfaces of the fixing means being kept small in the case of guide elements, in order to prevent the filter cartridge from jamming or sticking in place.
If the fixing means are designed as latching elements, the latching or clamping forces are kept low, in such a manner that the filter cartridge can be removed by simply being pulled out of the receiving opening in the axial direction. The latching elements are therefore preferably designed in such a manner that an axial movement of the filter cartridge is sufficient to fit or remove it.
It is preferable for the first fixing means to be arranged on a holding element arranged at the underside of the funnel base wall. A holding element of this type may be designed in various ways. A holding element in the form of a holding bracket which spans the receiving opening below the latter is preferred.
According to a further embodiment, the holding element may be a receiving chamber which is arranged in the funnel base wall, has at least one outflow opening and has a base wall and a peripheral wall.
Preferably, the base wall of the receiving chamber has at least one first indentation, and the base wall of the filter cartridge has at least one second indentation, which engages over the first indentation. These two indentations may interact in a sliding manner and thereby form guide elements. Moreover, these indentations may also be provided with latching elements which engage in one another when the filter cartridge is being fitted.
Preferably, the first indentation is a cylindrical or frustoconical hollow body, which is formed integrally on the base wall of the receiving chamber, faces inwards and has at least one inwardly facing first bead, which is in the shape of an arc of a circle and leaves clear at least one outflow opening, arranged on its free edge, wherein an outwardly facing mandrel, which engages in the cylindrical or frustoconical hollow body when fitting the filter cartridge, is arranged in the second indentation.
In this embodiment, the first guide element is formed by the at least one bead, which is in the form of an arc of a circle and slides along the outer side of the mandrel when the filter cartridge is being inserted. The bead does not extend over the entire inner periphery of the hollow body, and consequently a free space remains which, after fitting of the mandrel, which represents the second guide element, forms the outflow opening. A plurality of arcuate beads or bead segments may be arranged at a distance from one another in the peripheral direction, so that a plurality of outflow openings are created.
According to a further embodiment, the mandrel has at least one second bead in the shape of an arc of a circle on its outer side, which second bead engages behind the first bead during fitting of the filter cartridge. In this case, the first and second beads form latching elements.
It is preferable for the hollow body and the mandrel each to be arranged centrally. This arrangement has the advantage that in each case only one fixing means is required, and as a result the space required for the fixing means can be kept small, and consequently more volume is available for the filter medium.
It is preferable for the receiving chamber to have the first indentation in the region of base and peripheral wall and for the filter cartridge to have the second indentation likewise in the base and peripheral wall.
The first and second indentations may preferably be cuboidal in form, so that the two indentations each have two side walls, one end wall and one covering wall. The two indentations may be in the form of guide elements which engage in one another or slide into one another.
It is advantageous if the first indentation has first latching means on two side walls and the second indentation has second latching means on two side walls. This embodiment has the advantage that it is possible to realize greater latching forces, for example in devices in which water is heated. The two indentations may have different dimensions, which brings the advantage that there is only one possible position for the filter cartridge.
The fixing means allow accurate positioning of the filter cartridge, so that not only is the optimum position of the sealing rim at the receiving opening ensured, but also a defined distance can be set between the filter cartridge and the wall of the receiving chamber. The cross section of the flow passage between outlet opening of the filter cartridge and outflow opening of the receiving chamber can thus likewise be set in a targeted way.
This also enables a throttling device to be arranged between the outlet opening in the filter cartridge and the outflow opening in the receiving chamber.
The quantitative flow through the filter cartridge substantially depends on the type of filter medium and the size of the outlet opening(s) in the filter cartridge. Depending on the particular application, for example in filter systems of which a high performance is demanded of the filter medium, it may be necessary to reduce the quantitative flow which is predetermined by the filter cartridge. To achieve this, hitherto the cartridge has been modified, i.e. suitable filter cartridges had to be produced and kept in stock for every desired quantitative flow. The advantage of the throttling device is firstly that only one type of filter cartridge is required, and the quantitative flow can be set by selecting a suitable receiving chamber or a suitable inlet funnel.
Secondly, it is advantageous with this configuration that if the cartridge is not present the appliance can be operated without any flow restrictions.
It is preferable for the throttling device to be designed in such a manner that the quantitative flow delivered by the filter cartridge can be reduced by more than 0 up to 95%, in particular by 10 to 80%, particularly preferably by 20 to 70%.
It is preferable for the filter cartridge to be arranged in the region between outlet opening and outflow opening, at a distance from the peripheral wall and/or base wall of the receiving chamber, thereby forming a flow passage. The minimum cross section of the flow passage then forms the throttling device.
The cross section of the flow passage can be accurately set by the fixing means.
A preferred embodiment provides for at least one fixing means to form the throttling device. By way of example, if a spacer element formed integrally on the filter cartridge or the receiving chamber is arranged in the flow passage, the cross section is reduced at this location. The action of the throttling device can easily be set by means of the dimensions of one or more spacer elements of this type.
It is preferable for the indentations of filter cartridge and receiving chamber to be arranged at a distance from one another at least in subregions, so that a reduced cross section of flow, which forms the throttling device, is set between the indentations.
Alternatively, the outflow opening or outflow openings may form the throttling device, in which case the cross section of the outflow opening/openings is smaller than the cross section of the outlet opening/outlet openings in the filter cartridge.
A preferred embodiment provides for the cross section of the outflow opening/outflow openings defined by the bead or beads on the cylindrical or frustoconical hollow body to be selected in such a way that this/these outflow opening(s) has/have a throttling action.
For a predetermined filter cartridge, the throttling device may be adjustable by selecting a receiving chamber of suitable dimensions or with a suitable cross section of the outflow opening.
The desired quantitative flow can therefore be set by means of the inlet funnel, which is advantageous in that the inflow funnel, unlike the filter cartridge, does not represent a consumable item. The consumable item formed by the filter cartridge only has to be produced and kept in stock in one design, and the quantitative flow can be defined by the selection of inlet funnel. This makes it possible to significantly reduce the manufacturing costs of the apparatus and the costs of spares.
It is preferable for the outflow opening in the receiving chamber to be arranged above the outlet opening in the filter cartridge, so as to create a siphon-like arrangement. A siphon-like arrangement of this type has the advantage, in particular in conjunction with the throttling device, that the filter medium is kept moist even in the event of breaks in filtration, and therefore its full operational readiness is ensured even without renewed conditioning.
The presence of fixing means also allows a new type of configuration of the sealing rim of the filter cartridge, allowing the correct seating of the filter cartridge and the sealing position to be improved further.
For this purpose, provision is made for the sealing rim to be a snap-action rim which is connected to one of the two cartridge parts via an integral hinge, it being possible for the snap-action rim to be flipped from a first, lower snap-action position into an upper, second snap-action position and vice versa, and for the funnel base wall to have a sealing seat, which surrounds the receiving opening and into which the snap-action rim snaps in its second position.
With the snap-action rim in its lower snap-action position, the filter cartridge is fitted into the receiving opening from above and pressed downwards until the snap-action rim flips upwards and in the process snaps into the sealing seat. The sealing seat is matched to the snap-action rim in such a manner that when the snap-action rim has snapped into place, the filter cartridge bears in a sealing manner against the edge of the receiving opening and is fixed in place.
The snap-action indicates to the user that the filter cartridge has adopted its predetermined sealing position. This prevents both incorrect positioning by the user and slipping of the filter cartridge during transport.
To remove the filter cartridge, it is simply pulled out upwards, during which operation the snap-action rim flips into its lower snap-action position.
The snap-action rim is preferably formed by a flat edge strip which extends outwards in the radial direction.
In this embodiment, fixing means in the form of guide elements are sufficient. Here, fixing means in the form of latching elements could be disadvantageous since in the event of what is known as double latching at the sealing rim and, for example, in the region of the base, the tolerances which have to be observed make production costs correspondingly high.
In the case of a filter cartridge in which the cartridge upper part has an outwardly facing first securing flange and the cartridge lower part has an outwardly facing second securing flange, via which the two cartridge parts are connected to one another, the snap-action rim is preferably connected to one of the two securing flanges by way of the integral hinge.
The sealing seat at the inlet funnel is matched to this snap-action rim. It is preferable for the sealing seat to merge into a conically protruding rim section with an inwardly open abutment section, on which the outer edge of the snap-action rim engages.
The abutment section may be a groove or a step with at least one inclined surface.
The filter cartridge, which can be fitted into the inlet funnel and has a cartridge upper part with at least one inlet opening, a cartridge lower part with at least one outlet opening and a sealing rim, is characterized by least one fixing means arranged below and at a distance from the sealing rim.
The fixing means at the filter cartridge is preferably a spacer element and/or guide element and/or latching element. The fixing means may be recesses and projections, the projections or recesses preferably being cylindrical, conical or frustoconical in form. The latching element may be a latching boss, a latching recess or an annular bead.
The fixing means is preferably arranged in the region of the lower half of the filter cartridge, preferably in the region of the bottom third and in particular in the region of the base wall of the filter cartridge.
The cartridge lower part has at least one indentation, with an outwardly facing mandrel preferably being arranged in the indentation.
According to a further embodiment, the indentation may also be cuboidal in form.
The sealing rim is preferably a snap-action rim which is connected to one of the two cartridge parts via an integral hinge, it being possible for the snap-action rim to be flipped from a first, lower snap-action position into an upper, second snap-action position and vice versa.
If the filter cartridge has a sealing flange on its upper and lower parts, the snap-action rim is preferably connected to one of the two securing flanges by way of the integral hinge.
The snap-action rim is preferably formed by a flat edge strip which is directed radially outwards.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
Exemplary embodiments of the invention are explained in more detail below with reference to the drawings, in which:
FIGS. 1 a, b show vertical sections through an inlet funnel with fitted filter cartridge in accordance with two embodiments,
FIG. 2 shows a perspective view, partially in section, of an inlet funnel in accordance with a further embodiment,
FIG. 3 shows a vertical section through an inlet funnel with fitted filter cartridge in accordance with a further embodiment, before the filter cartridge has reached its limit position,
FIG. 4 shows a section on line F-F through the apparatus shown in FIG. 3 ,
FIG. 5 shows an enlarged sectional illustration of the region of the two indentations in accordance with FIG. 3 ,
FIG. 6 shows an enlarged sectional illustration of the region of the two indentations after the filter cartridge has been fitted and positioned,
FIG. 7 a shows a plan view of the frustoconical hollow body in accordance with FIG. 3 ,
FIG. 7 b shows a plan view of a frustoconical hollow body in accordance with the a further embodiment,
FIG. 8 shows a vertical section through the frustoconical hollow body on line H-H in FIG. 7 b,
FIG. 9 shows an enlarged sectional illustration of the lower region of the two indentations in accordance with a further embodiment, on line G-G through the frustoconical hollow body in FIG. 7 a,
FIG. 10 shows a vertical section through a filter cartridge,
FIG. 11 shows a plan view of the filter cartridge shown in FIG. 10 ,
FIG. 12 shows an enlarged sectional illustration of an edge region of the filter cartridge illustrated in FIGS. 10 and 11 ,
FIG. 13 shows an enlarged sectional illustration of a region of the receiving opening in the inlet funnel,
FIG. 14 shows an enlarged sectional illustration of the region of the receiving opening in the inlet funnel with initially positioned snap-action rim of a filter cartridge,
FIG. 15 shows an enlarged illustration of the region of the receiving opening of an inlet funnel with the snap-action rim of the filter cartridge snapped into position,
FIG. 16 shows a vertical section through the region of the receiving opening in the inlet funnel in accordance with a further embodiment,
FIG. 17 shows a vertical section through an inlet funnel with a fitted filter cartridge in accordance with a further embodiment,
FIG. 18 shows a section on line B-B through the apparatus shown in FIG. 17 ,
FIG. 19 shows an enlarged sectional illustration of the region of the outflow opening of the apparatus shown in FIG. 17 .
DETAILED DESCRIPTION
FIG. 1 a illustrates a vertical section through an inlet funnel 10 with fitted filter cartridge 100 . The inlet funnel 10 has a peripheral wall 11 , which merges into a funnel base wall 12 which has a receiving opening 13 . A receiving chamber 14 , which once again has a peripheral wall 15 and a base wall 16 , extends downwards from the receiving opening 13 as holding element 20 .
The filter cartridge 100 is fitted into this receiving chamber 14 axially from above; the filter cartridge 100 comprises a cartridge upper part 101 and a cartridge lower part 110 . The cartridge upper part 101 is configured in the shape of a roof and has inlet openings 102 . A sealing rim 160 , which bears against the sealing seat 60 of the inlet funnel 10 in the region of the receiving opening 13 , is provided in the connection region of cartridge upper part 101 and cartridge lower part 110 .
The cartridge lower part 110 of the filter cartridge 100 has a peripheral wall 111 and a base wall 112 , in which outflow openings 113 are arranged.
The receiving chamber 14 is configured in such a manner that the peripheral wall 111 of the filter cartridge 100 is arranged at a distance from the peripheral wall 15 and from the base wall 16 . Consequently, the filtered liquid collects in the lower region of the receiving chamber 14 and flows away via the outflow openings 17 shown to the right and left in the figure.
The receiving chamber 14 with the peripheral wall 15 and the base wall 16 forms a holding element 20 for the filter cartridge 100 . A second fixing means 130 , which in the embodiment shown here forms a spacer element, is formed integrally in the centre of the base wall 112 of the filter cartridge 100 . This second fixing element 130 bears against the inner side of the base wall 16 , which therefore performs the function of a first fixing element 30 .
The filter cartridge 100 is fitted into and removed from the receiving chamber 14 of the inlet funnel 10 in the axial direction, as indicated by the double arrow. When the limit position provided during fitting is reached, the second fixing means 130 bears against the first fixing means 30 , i.e. the base wall 16 of the receiving chamber 14 . The operator notices this as a result of the resistance which then occurs, which indicates to the operator that the limit position has been reached. In this limit position, the sealing rim 160 bears in a sealing manner against the sealing seat 60 of the receiving opening 13 . As a result, the optimum position of the filter cartridge 100 has been reached.
FIG. 1 b illustrates a further embodiment of the apparatus, which differs from the apparatus shown in FIG. 1 a by virtue of the fact that two first fixing means 30 , in the form of indentations 31 designed as spacer elements, are formed integrally on the inner side of the base wall 16 . The base wall 112 of the filter cartridge 100 bears against these two spacer elements 30 .
In this embodiment, the base wall 112 performs the function of the second fixing means 130 .
The two first fixing means 30 are arranged in the flow passage 201 between the outlet openings 113 and the outflow openings 17 and at this location reduce the cross section of flow. Depending on the particular configuration and dimensions, the fixing elements 30 in each case form a throttling device 200 .
FIG. 2 illustrates a further embodiment of an inlet funnel 10 , which does not have a receiving chamber 14 , but rather instead, as holding element 20 , has a holding bracket 21 which comprises the two substantially vertical limbs 22 a, b and a cross-bar 23 . This holding bracket 21 spans the receiving opening 13 below the receiving opening 13 , so that a filter cartridge (not shown) can be fitted. The dimensions of the holding bracket 21 are matched to the dimensions of the filter cartridge 100 to be fitted.
In the central region, the cross-bar 23 has a first fixing element 30 in the form of a first indentation 31 . This indentation 31 is conical in form and extends vertically upwards. The associated filter cartridge 100 (not shown), in the region of its base wall, has a corresponding conical or frustoconical indentation (second indentation 130 ), so that the two fixing elements interact during fitting of the filter cartridge 100 in the axial direction, in such a way as to guide the filter cartridge. In this configuration, the fixing elements 30 , 130 serve as spacer elements and guide elements.
FIG. 3 illustrates a vertical section through a further embodiment of the apparatus. The inlet funnel 10 , of which the upper part has been omitted for the sake of clarity, has a first indentation 31 , which is designed a frustoconical hollow body 32 , arranged in the centre of its base wall 16 . A bead 34 in the form of an arc of a circle is formed integrally on the inner side of the free edge 33 of the hollow body 32 , which bead 34 , as illustrated in FIG. 7 a , does not form a continuous ring, but rather has a free space 18 which forms the outflow opening 17 after the filter cartridge has been fitted.
In its base wall 112 , the filter cartridge 100 likewise has an indentation 131 in which a mandrel 132 , which extends vertically downwards, is formed integrally. When the filter cartridge 100 is being fitted into the receiving chamber 14 , the mandrel 132 engages in the frustoconical hollow body 32 , with the outer surface 133 of the mandrel 132 sliding along the bead 34 . In this embodiment, the mandrel 132 and the bead 34 form first and second fixing means 30 , 130 which serve as guide elements. The outflow opening 17 is formed between the outer surface 133 of the mandrel 132 and the wall 35 of the hollow body 32 .
FIG. 3 illustrates the filter cartridge 100 at the start of the fitting operation. The sealing rim 160 , which in the embodiment shown here is designed as a snap-action rim 161 , is therefore not yet in its limit position. The snap-action rim 161 will be described separately below.
FIG. 4 illustrates a section on line F-F through the apparatus shown in FIG. 3 . It can be seen from this figure that the mandrel 132 bears against the bead 34 in the form of an arc of a circle and at this location also forms a seal apart from the outflow opening 17 (which is not visible in FIG. 4 ).
FIG. 5 illustrates an enlarged view of the lower region of filter cartridge 100 and receiving chamber 14 , illustrating the fitting state in accordance with FIG. 3 . The second indentation 131 has a base wall 134 a and an annular wall 134 b , which extends upwards from the base wall 112 . Spacer ribs 139 are formed integrally on the underside of the base wall 134 a.
In FIG. 6 , the filter cartridge 100 has reached its limit position and therefore its sealing position. A flow passage 201 is formed between the base wall 112 of the filter cartridge 100 and the base wall 16 of the receiving chamber 14 and merges, in the region of the two indentations 31 , 131 , into a rising annular passage 202 which is formed between wall 35 of the hollow body 32 and the annular wall 134 b . The cross section of the annular passage 202 is smaller than that of the flow passage 201 , so that a throttling device 200 ′ is formed.
However, the annular passage 202 only forms the throttling device 200 ′ if the outflow opening 17 has a significantly larger cross section. In the embodiment shown here, there is only a single outflow opening 17 , which has a smaller cross section of flow than the cross section of the annular passage 202 , and consequently the outflow opening 17 can be equated to the throttling device 200 ′. The two fixing elements 30 , 130 in the form of the annular bead 34 and in the form of the mandrel 132 therefore form the throttling device 200 in the assembled state. The spacer ribs 139 bear against the end face 39 of the hollow body 32 and therefore, as spacer elements, form second fixing means 130 .
FIG. 7 b illustrates a further embodiment of the hollow body 32 , which differs from the embodiment illustrated in FIG. 7 a by virtue of the fact that a total of four beads 34 in the form of arcs of a circle are arranged spaced apart from one another, so that free spaces 18 for the outflow openings 17 in each case remain between the beads 34 . Whether the combination of these outflow openings form a throttling device 200 depends on the cross-sectional dimensions of the flow passage, in particular of the annular passage 202 in the region of the frustoconical hollow body 32 .
FIG. 8 illustrates the hollow body 32 in vertical section on line H-H in FIG. 7 b . The triangular shape of the arcuate beads 34 has the advantage of minimizing the surface area of the contact surface with the mandrel that is to be introduced, so that the frictional forces are correspondingly low and the filter cartridge can be fitted and removed without difficulty.
FIG. 9 illustrates a further embodiment, in which the mandrel 132 is likewise provided with a bead (second bead) 135 on its outer surface. In this case, the section through the frustoconical hollow body 32 is taken on line G-G from FIG. 7 a . When the filter cartridge 100 is being fitted, the mandrel 132 engages in the hollow body 32 , with the annular bead 135 engaging behind the bead 34 when the spacer ribs 139 are bearing against the end face 39 . Free spaces (not visible in this figure) are provided between the spacer ribs 139 , so that the liquid can flow to the outflow opening 17 . In this embodiment, the beads 34 and 135 form latching elements, and the spacer ribs 139 form spacer elements, with the end face 39 of the hollow body 32 , as first fixing means 30 , forming a stop.
FIG. 10 illustrates a vertical section through a filter cartridge 100 in order to explain the function of the sealing rim 160 in conjunction with the following figures. The cartridge upper part 101 has a securing flange 120 , which is joined to the securing flange 121 of the cartridge lower part 110 , preferably by welding. The securing flange 120 extends radially outwards and has an integral hinge 162 , via which the snap-action rim 161 is attached in jointed fashion. The snap-action rim 161 is formed by a flat edge strip directed radially outwards.
FIG. 10 illustrates the snap-action rim 161 in its lower position. As illustrated in FIG. 11 , the snap-action rim 161 is designed to run continuously all the way around, as is the integral hinge 162 . A dead centre has to be overcome when the snap-action rim is being flipped from a lower snap-action position into an upper snap-action position.
FIG. 12 illustrates the snap-action rim 161 on an enlarged scale. The integral hinge 162 is formed as an encircling groove 163 on the underside of the securing flange 120 .
FIG. 13 illustrates the corresponding receiving opening 13 in section and on an enlarged scale. The sealing seat 60 with which the snap-action rim 161 interacts during fitting of the filter cartridge has a conically protruding edge section 61 , which merges into the abutment section 62 , which in the embodiment shown in FIG. 13 is designed as a groove 63 . The groove 63 is open on the radially inner side, so that the snap-action rim 161 can engage therein, as can be seen in the following FIGS. 14 and 15 .
FIG. 14 illustrates the start of the snap-action process. The snap-action rim 161 is still in its lower position and is engaging against the conically protruding edge section 61 .
As the filter cartridge 100 continues to be lowered, the snap-action rim 161 is moved into its upper position, with the outer edge 164 of the snap-action rim 161 engaging in the groove 63 , as illustrated in FIG. 15 . There is no need for the whole of the surface of the snap-action rim 161 to bear against the surface 61 . Sealing is effected in the region of the groove 63 .
FIG. 16 illustrates an alternative to the groove 63 . The abutment section 62 comprises a step 64 which has a substantially horizontal surface 66 and an inwardly inclined surface 65 .
FIG. 17 illustrates a vertical section through an inlet funnel 10 with fitted cartridge 100 in accordance with a further embodiment. The filter cartridge 100 has a conventional sealing rim 160 , which bears against the sealing seat 60 in the region of the receiving opening 13 . Two cuboidal indentations 36 and 37 are formed integrally in the peripheral wall 15 and the base wall 16 of the receiving chamber 14 . These indentations 36 , 37 each have two side walls 40 , 41 (not visible), an end wall 42 and a covering wall 43 . The outflow opening 17 is located in the end wall 42 .
The cartridge 100 also has corresponding indentations 136 and 137 , which are likewise cuboidal in design, with side walls 140 , 141 (not visible in FIG. 17 ), end wall 142 and covering wall 143 , with the mutually corresponding walls of cartridge and receiving chamber being arranged at a distance from one another, so that flow passages 201 are formed between the walls.
FIG. 18 illustrates a section on line B-B. Fixing means 30 , 130 in the form of latching elements are provided in the two side walls 40 , 41 , 140 , 141 of the cuboidal indentations 36 , 136 . The latching elements are latching bosses 38 which engage in corresponding latching recesses 138 .
This configuration of the latching elements is to be found on both cuboidal indentations 36 , 37 , 136 , 137 .
FIG. 19 shows an enlarged illustration of the cuboidal indentations 37 , 137 .
List of designations
10
Inlet funnel
11
Peripheral wall
12
Funnel base wall
13
Receiving opening
14
Receiving chamber
15
Peripheral wall
16
Base wall
17
Outflow opening
18
Free space
20
Holding element
21
Holding bracket
22a, b
Limb
23
Cross-bar
30
First fixing means
31
First indentation
32
Frustoconical hollow body
33
Free edge
34
Bead in the form of an arc of a circle
35
Wall of the hollow body
36
Cuboidal indentation
37
Cuboidal indentation
38
Latching boss
39
End face
40
Side wall
41
Side wall
42
End wall
43
Covering wall
60
Sealing seat
61
Conically protruding edge section
62
Abutment section
63
Groove
64
Step
65
Inclined surface
66
Horizontal surface
100
Filter cartridge
101
Cartridge upper part
102
Inlet opening
110
Cartridge lower part
111
Peripheral wall
112
Base wall
113
Outlet opening
120
Securing flange on upper part
121
Securing flange on lower part
130
Second fixing means
131
Second indentation
132
Mandrel
133
Outer surface
134a
Base wall
134b
Annular wall
135
Second bead
136
Cuboidal indentation
137
Cuboidal indentation
138
Latching recess
139
Spacer rib
140
Side wall
141
Side wall
142
End wall
143
Covering wall
160
Sealing rim
161
Snap-action rim
162
Integral hinge
163
Encircling groove
164
Outer edge
200, 200′
Throttling device
201
Flow passage
202
Annular passage | The invention describes an apparatus for the filtration of liquids and an associated filter cartridge 100 , the correct seating of which is ensured and can be established by the user. The apparatus is characterized in that the inlet funnel 10 has at least one first fixing means 30 below the receiving opening 13 , and in that the filter cartridge 100 has at least one second fixing means 130 below and at a distance from the sealing rim 160 , which second fixing means, when the filter cartridge 100 is being fitted into the receiving opening 13 , interacts with the first fixing means 30. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates, in general, to a coupling and, more particularly, to a reinforcing bar coupling which is intended to obtain a mechanical butt-joint between the ends of two reinforcing bars in reinforced concrete work to enhance the strength of the coupled portion and to afford a prompt and convenient coupling operation.
2. Related Prior Art
Since reinforcing bars are produced at certain unit lengths from factories, building works for various structures such as bridges, retaining walls and apartment houses, which extend to several tens of meters in length, require the ends of reinforcing bars to be overlapped. As conventional methods for joining reinforcing bars, a few joint processes are commonly used, which are disclosed as follows.
In the prior art, a lap-joint process, which is carried out in such a way that the ends of reinforcing bars are lapped along certain lengths thereof and the lapped ends of the reinforcing bars are bound with binding wires, is predominantly used. However, the lap-joint process has disadvantages in that distances between the adjacent reinforcing bars become small at the lapped regions, the required number of reinforcing bars is increased due to the lapped regions of the reinforcing bars, a pouring operation of concrete into space between the lapped reinforcing bars is difficult due to the small distances between the adjacent reinforcing bars, and the lap-jointed reinforcing bars are weakened in resistance to axial tensile force and compressive force.
In another process, i.e., in a gas pressure welding process in which the ends of reinforcing bars are butted to each other and the ends of the reinforcing bars are welded to each other by high temperature flame, a specialized technique is required to carry out the gas pressure welding process, the welded portion of the reinforcing bars is weakened by heat, and a post-welding inspection is further required.
In a steel pipe compression process in which the ends of two reinforcing bars are inserted into a steel pipe and the steel pipe containing the ends of two reinforcing bars is compressed by a hydraulic jack, though a specialized technique is not required, special equipment is required to perform the joining operation.
Therefore, to overcome the above problems, a process for mechanically joining two reinforcing bars has been developed and used in recent years.
In this process, the ends of reinforcing bars are subjected to a plastic deformation, i.e., thickened and shortened by hot or cold working, or the ends of reinforcing bars are subjected to cold swaging, causing the ribs of the bars to be collapsed and to be smooth, and then threaded with external threads (male) by a machine tool such as a screw thread rolling machine. Subsequently, the threaded ends of two reinforcing bars are threaded into a coupling having female threads in its internal surface, thereby joining the two reinforcing bars.
However, the above thread-joint process also has disadvantages in that it requires many working steps to form male threads on the ends of the reinforcing bars, and although reinforcing bars are considerably long and apt to be bent due to the material characteristics thereof, two reinforcing bars must be precisely aligned with each other to allow the ends of the reinforcing bars to be threaded into a coupling, thereby involving inconvenience in the joining operation.
SUMMARY OF THE INVENTION
Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a reinforcing bar coupling which is capable of achieving a firm joining between reinforcing bars by a simple operation of inserting wedges between the reinforcing bars and a cylindrical sleeve and hammering the wedges.
In order to accomplish the above object, the present invention provide a reinforcing bar coupling, comprising: a cylindrical sleeve having a cross sectional area sufficient to accommodate two reinforcing bars entered through openings at opposite ends thereof, and which is provided at a part of its inner surface with an uneven surface corresponding to an outer ribbed surface of the reinforcing bars; and a wedge means adapted to be fitted between the cylindrical sleeve and the reinforcing bars to apply radial force to them, thereby achieving butt-joining of the two reinforcing bars.
Furthermore, the present invention provides a wedge means which is configured to have a length substantially equal to that of the cylindrical sleeve and to be fitted into a gap between the cylindrical sleeve and the reinforcing bars, and which comprises a intermediate pad adapted to be in contact with the reinforcing bars and having an uneven contact surface corresponding to an outer ribbed surface of the reinforcing bars, a gap defined between the cylindrical sleeve and the intermediate pad gradually becoming narrower toward the middle point of the cylindrical sleeve, and two wedge elements adapted to be driven into the gap defined between the cylindrical sleeve and the intermediate pad by impact from a striking tool such as a hammer.
The reinforcing bar coupling according to the present invention can be commonly used in joining two reinforcing bars in new construction, rebuilding and repair work of various concrete structures such as bridges and buildings. The reinforcing bar coupling enables easy and firm coupling of reinforcing bars using only a simple striking tool. Furthermore, since reinforcing bars are coupled to each other without overlapping thereof, excessive consumption of reinforcing bars can be prevented and advantageous cost savings can be achieved. In addition, the reinforcing bar coupling exhibits superior bonding strength compared to a conventional coupling method.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and other advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an exploded perspective view of a first embodiment of the present invention.
FIG. 2 is a cross-sectional view showing an assembled condition of the first embodiment of the present invention.
FIG. 3 is a transverse cross-sectional view of the first embodiment of the present invention.
FIG. 4 is an exploded perspective view of a second embodiment of the present invention.
FIG. 5 is a cross-sectional view showing an assembled condition of the second embodiment of the present invention.
FIG. 6 is a transverse cross-sectional view of the second embodiment of the present invention.
FIG. 7 is an exploded perspective view of a third embodiment of the present invention.
FIG. 8 is a cross-sectional view showing an assembled condition of the third embodiment of the present invention.
FIG. 9 is a cross-sectional view taken along line A—A of FIG. 8 .
FIG. 10 is a perspective view showing an assembled condition of the first embodiment of the present invention.
FIG. 11 is an exploded perspective view of an intermediate pad according to a fourth embodiment of the present invention.
FIG. 12 is a cross-sectional view of a reinforcing bar coupling to which the intermediate pad of FIG. 11 is applied; and
FIG. 13 is a transverse cross-sectional view of a reinforcing bar coupling to which the intermediate pad of FIG. 11 is applied.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
This invention will be described in further detail by way of example with reference to the accompanying drawings.
FIGS. 1 to 3 are an exploded perspective view, a cross-sectional view and a transverse cross-sectional view of a first embodiment of the present invention, in which the embodiment of the present invention comprises a cylindrical sleeve 2 , a intermediate pad 3 and a pair of wedges 4 to join two reinforcing bars 1 . A perspective view of a reinforcing bar coupling according to the embodiment of the present invention is shown in FIG. 10 , in which the reinforcing bar coupling is assembled.
The reinforcing bars 1 , the intermediate pad 3 and wedges 4 are separately inserted or pushed into openings 20 of the cylindrical sleeve 2 of a certain length. The size of the cylindrical sleeve is designed according to the diameter of the reinforcing bars to be joined. To this end, the cross section of the cylindrical sleeve 2 assumes a shape similar to an ellipse.
As is well known in the art, a reinforcing bar is evenly formed at its outer surface with ribs to improve strength and adhesion to the concrete. The cylindrical sleeve 2 is provided with an uneven surface on its inner surface by grooves 21 along the length such that the grooves 21 are formed to have an arrangement corresponding to that of the ribs (or the outer shape) of the reinforcing bars. With the grooves 21 formed on the inner surface of the cylindrical sleeve 2 , reinforcing bars cannot be axially displaced once the reinforcing bars are inserted into and engaged to the cylindrical sleeve 2 .
The ribs 11 consist of semi-longitudinal ribs 12 and semi-annular ribs 13 . In some reinforcing bars, the semi-annular ribs 13 may be alternately formed along the semi-longitudinal ribs 12 (not shown). To accommodate for reinforcing bars having such alternate semi-annular ribs, the semi-annular grooves 21 are arranged such that the patterns of the adjacent semi-annular grooves 21 formed on the uneven surface is one-half of the patterns of adjacent semi-annular ribs 13 .
Although not shown, since there may be difficulty to insert reinforcing bars into the cylindrical sleeve such that the reinforcing bars radially coincide with each other, the cylindrical sleeve 2 may be provided with several semi-longitudinal grooves on its uneven surface. If it includes the semi-longitudinal grooves, the uneven surface of the cylindrical sleeve will assume a lattice shape. A contact angle between an outer surface of a reinforcing bar and the uneven surface 22 of the cylindrical sleeve or an inner surface of the intermediate pad may be between 90°-180°, but the contact angle is not necessarily limited to that.
Although a reinforcing bar 1 may be formed with burrs at its cut end or may be uneven in the diameter of its outer surface, the uneven surface 22 of the cylindrical sleeve is adapted to be in close contact with the reinforcing bar. This can be achieved in such a way that an inner diameter of a certain middle section of the cylindrical sleeve (corresponding to a portion at which the ends of reinforcing bars are positioned for joining) is larger than that of the inner surface near the openings 20 at each end of the cylindrical sleeve 2 . That is, though burrs or deformed portions of the ends of reinforcing bars are positioned at the enlarged inner surface, close contact between the reinforcing bars 1 and the cylindrical sleeve 2 is not interrupted.
Furthermore, so as to limit the inserted lengths of reinforcing bars 1 into the cylindrical sleeve 2 , the cylindrical sleeve is provided with a semicircular stopper 24 at its inner middle portion.
An inner slant face 27 of the cylindrical sleeve which faces the uneven inner surface 22 is gradually reduced in its inner diameter from both end openings toward the middle point in order to intensify driving action of the wedges. Details relating to this will be more specifically described hereinafter.
The cylindrical sleeve 2 is formed with semi-longitudinal and semi-annular ribs 25 on its outer surface, similar to ribs 11 of reinforcing bars 1 , to improve cohesiveness with concrete.
The intermediate pad 3 is comprised of a semicircular cylinder having a length corresponding to that of the cylindrical sleeve 2 , and includes on its inner surface an uneven surface 32 having a shape and a function similar to those of the uneven surface of the cylindrical sleeve, thereby enabling the other half surfaces of the reinforcing bars to be in close contact therewith. The intermediate pad 3 is gradually thickened toward its middle portion to assume a symmetrical contour tapered outward. An angle of inclination of the outer slant surface of the intermediate pad is set to achieve a desired correlation with the cylindrical sleeve and the wedges. As is the case with the cylindrical sleeve, the intermediate pad 3 is provided with an enlarged surface 33 at its inner middle portion, which is formed to accommodate undesirable burrs etc., of the reinforcing bars.
Moreover, an outer surface of the intermediate pad is symmetrically provided with a serration. The serration serves as a blocking means for preventing the wedges 4 from sliding cut between the intermediate pad 3 and the cylindrical sleeve 2 once the wedges 4 are fitted between the intermediate pad 3 and the cylindrical sleeve 2 , as shown in FIG. 2 . Functions and configuration of the serration are the same in all of the following embodiments. The serration serves to prevent slippage of the wedges, and the shape of the serration is not limited to that shown in the drawings.
The wedges 4 are rectangular plates, characterized by one end being thinner than the other end. A pair of wedges 4 is fitted into the openings 20 of the opposite ends of the cylindrical sleeve. Each of the wedges 4 is configured such that its upper surface 41 conforms to the inner slant face 27 of the cylindrical sleeve 2 and its lower surface conforms to the outer surface 34 of the intermediate pad 3 . In addition, the lower surface 42 of the wedge is provided with a serration corresponding to the serration of the outer surface 34 of the intermediate pad 3 .
As is well known, the wedge has a shape and a function similar to those of a commonly used wedge. A rear end 44 of the wedge is more enlarged than a front end 43 , and serves to be hit with a striking tool such as a hammer.
The overall length of the wedge 4 is slightly shorter than one half of the overall length of the cylindrical sleeve 2 . The wedge may be optionally provided with one or more semi-longitudinal grooves 45 without the serration to reduce frictional resistance from the intermediate pad 3 during its insertion. The semi-longitudinal grooves 45 may be provided on one surface or on both surfaces. Such semi-longitudinal grooves may also be formed on the intermediate pad or the cylindrical sleeve.
Functions of the first embodiment of the present invention will be described in order of the assembling procedure.
First, two reinforcing bars to be joined are inserted into the cylindrical sleeve 2 through both ends of the cylindrical sleeve such that the ribs 11 of the reinforcing bars 1 are in close contact with the uneven surface 22 of the cylindrical sleeve 2 and the ends of the reinforcing bars are positioned at the enlarged portion. Subsequently, the intermediate pad 3 is fully inserted into the cylindrical sleeve 2 so that the intermediate pad comes into close contact with the ribs 11 of the reinforcing bars. After two wedges 4 are temporarily fitted between the intermediate 3 and the cylindrical sleeve 2 though both ends of the cylindrical sleeve 2 , the wedges are strongly impacted with a striking tool such as a hammer.
By the impact of the hammer, the inner slant face 27 of the cylindrical sleeve 2 and the outer surface of the reinforcing bars 1 are applied with strong radial pressure via the intermediate pad 3 . That is, a firmly engaged condition of the components is achieved by action of the wedges. Furthermore, since the wedges and the intermediate pad are engaged with each other by the serration formed on the surfaces of both components, the wedges cannot slide out of the cylindrical sleeve even if the cylindrical sleeve is subjected to vibration or external force. Moreover, even though strong external tensile force acts on the cylindrical sleeve, the engaged condition of the reinforcing bars is not broken by the uneven surfaces 22 , 32 of the cylindrical sleeve and the intermediate pad engaged with the ribs 11 of the reinforcing bars.
FIGS. 4 to 6 show a second embodiment of the present invention. The essential configuration of the second embodiment is substantially equal to that of the first embodiment, except that wedges 4 , 4 ′ are driven into the cylindrical sleeve by a bolt 5 rather than the impact of a hammer. That is, one wedge 4 of a paired wedges is formed with a longitudinal through hole 47 , and the other wedge 4 ′ of the paired wedges is formed with a threaded hole 48 , which is adapted to be engaged with a male threaded portion 5 a of the bolt 5 .
The bolt 5 has a diameter suitable to the size of reinforcing bars 1 to be joined. To induce the longitudinal cross sectional area, each of the wedges 4 , 4 ′ is shaped as a “U”-shaped clamp in plan, as illustrated in FIG. 4 . The intermediate pad 3 is provided at its outer slant surface with a semi-longitudinal groove 35 to allow the bolt 5 to pass through. Therefore, the cylindrical sleeve 2 can be reduced in its cross sectional area. In an arrangement of a plurality of reinforcing bars, it is generally known that it is preferable to reduce the cross section of the cylindrical sleeve in terms of a building operation and strength of a beam.
A modification which can be derived from this embodiment is configured such that the bolt 5 is longitudinally elongated to fully pass through a wedge 4 ′ with its male threaded end 5 a protruding from the wedge and the threaded end of the bolt is screwed into a nut (not shown). In this case, a seat face and/or seat faces of the bolt and/or the nut can be of course provided with a common washer.
As described above, functions of the second embodiment of the present invention are substantially equal to those of the first embodiment of the present invention. However, this embodiment is different from the first embodiment only in that the wedges 4 are driven into the cylindrical sleeve by fastening action of the bolt 5 between the female threaded hole 48 of the wedge 4 ′ or a nut (not shown) rather than by impact of a hammer.
Another modification which can be derived from this embodiment is designed to employ a combined action of the impact of a hammer and fastening of a bolt and a nut. In other words the wedges 4 are first driven into a cylindrical sleeve by hitting of a hammer and then fastened by the bolt 5 . Since this modification can be fulfilled by designing to adjust angles of inclination of the wedges and the intermediate pad, detailed description thereof is omitted.
The method of coupling reinforcing bars according to the second embodiment of the present invention can be advantageously applied to an operation of coupling new reinforcing bars to existing reinforcing bars 1 which have been previously arranged, or to existing reinforcing bars 1 which are embedded in poured concrete where adhesive force between the existing reinforcing bars and the concrete may be weakened by impact shocks acting on the wedges.
The stopper 24 , the ribs 25 and the inner slant face 27 of this embodiment have the same shapes and functions as those of the first embodiment.
FIGS. 7 to 9 show a third embodiment of the present invention. The essential configuration of this third embodiment is substantially equal to that of the first and second embodiments, except that the driving direction of the wedges 4 is perpendicular or transverse to the reinforcing bars. To this end, a cylindrical sleeve 2 is formed with two wedge fitting openings 29 , which are oriented to be perpendicular or transverse to the reinforcing bars. Furthermore, a intermediate pad 3 is formed at its upper surface 39 with two wedge seat grooves 39 a , which are located at positions corresponding to those of the wedge fitting openings 29 , and each of which has a width equal to or larger than a width of the wedge 4 .
As shown in FIG. 9 , upper surfaces 41 of the wedges 4 and upper surfaces 29 a of the wedge fitting openings 29 of the cylindrical sleeve 2 have serrated surfaces corresponding to each other. The serration serves to prevent the wedges from sliding out of the cylindrical sleeve.
The fitting manner and other details of this embodiment are substantially identical to those of the previous embodiments. That is, the stopper 24 and the uneven surface etc., of the cylindrical sleeve 2 are identical to those of the previous embodiments in function and shapes.
The characteristics of this embodiment are as follows. Widths of the wedge fitting openings 29 of the cylindrical sleeve 2 and widths of the wedge seat grooves 39 a of the intermediate pad 3 are set to be slightly larger than a width of the wedge 4 . Accordingly, even though axial positions of semi-annular ribs 13 of a reinforcing bar are alternately arranged along semi-longitudinal ribs 12 or irregularly arranged so that the wedge fitting openings 29 of the cylindrical sleeve 2 are not aligned with the wedge seat faces 39 a of the intermediate pad 3 , the wedges 4 can be easily fitted into the cylindrical sleeve. In addition, corners of the wedge fitting openings 29 are rounded to prevent the possibility of cracking of the cylindrical sleeve 2 during installation of the wedges.
A groove 45 is provided to reduce resistance during a fitting operation of the wedges, and a rear end 44 to be hit by a striking tool of a user.
A modification which can be derived from this embodiment of the present invention is configured such that the two wedges are integrally formed. In this modification, since the fitting direction of the two wedges are identical to each other and the fitting positions of the wedges are adjacent to each other, the two wedges are integrally connected to each other to form a U-shaped clamp to permit the two wedges to be fitted concurrently.
Referring to FIGS. 11 to 13 , there is shown a fourth embodiment of the present invention. This embodiment is designed to be applied in the case where shapes and positions of semi-annular ribs formed on the outer surfaces of the reinforcing bars provided by various manufacturers are different from one another. That is, where grooves of an uneven surface of an intermediate pad do not coincide with semi-annular ribs of a reinforcing bar in position, the area of the contact surface between the intermediate pad and the reinforcing bar is reduced. To accommodate such nonconformity between the grooves of the intermediate pad and the semi-annular ribs of the reinforcing bars, this embodiment is intended to allow the intermediate pad to be slightly displaced to conform to the reinforcing bar.
To this end, the intermediate pad 3 comprises three intermediate sub pads, as shown in FIG. 11 . In other words, the intermediate pad 3 comprises a first intermediate pad 51 and a pair of second intermediate pads 52 . The second intermediate pads 52 a are provided with uneven surfaces on the lower surfaces thereof, corresponding to an outer surface of a reinforcing bar. The facing surfaces 51 a , 52 b of the first and second intermediate pads are provided with serrations in the form of triangular screw threads so that the first and second intermediate pads are engaged with each other by the serration surfaces 51 a , 52 b . Prior to assembly of the cylindrical sleeve joint, the second intermediate pads can be held in place against the first intermediate pad by means of magnets mounted on the second intermediate pads. As such, since the second intermediate pads are provided with magnets, the number of components required to joint reinforcing bars can be reduced, thereby facilitating maintenance and the joining operation of the coupling.
An upper surface 51 b of the first intermediate pad is provided with a serrated surface for preventing sliding of the wedges 4 , as is the case with the previous embodiments.
FIGS. 12 and 13 are a cross-sectional view and a transverse cross-sectional view showing the intermediate pads used in joining reinforcing bars.
Two reinforcing bars are first inserted into the cylindrical sleeve, followed by the first and second intermediate pads. Then, the second intermediate pads are adjusted in their longitudinal positions to conform to outer surfaces of the reinforcing bars. Thereafter, the wedges 4 are driven into the cylindrical sleeve by a striking action of a hammer to complete a coupling operation of the reinforcing bars.
In this embodiment, although two pieces of the second intermediate pads are shown in FIGS. 11 and 12 disposed at both sides of the cylindrical sleeve, one piece second intermediate pad may be disposed in the cylindrical sleeve. That is, one-piece second intermediate pad may be disposed under the first intermediate pad.
According to the embodiment shown in FIG. 12 , each of the wedges is provided with serrated surfaces at both its upper and lower surfaces, and the cylindrical sleeve is also provided with a serrated surface at its upper surface. As such, the serrated surfaces may be selectively formed at either one or both of the upper and lower surfaces of the wedge.
The cylindrical sleeve 2 , which directly comes into contact with a reinforcing bar, is provided at its lower surface with ridges 22 a in the form of screw threads in order to intensify compressing action to the reinforcing bars due to the driving of the wedges. The ridges can be applied to all the previous embodiments as well as this embodiment.
In still another embodiment of the present invention, reinforcing bars can be joined using only the cylindrical sleeve and the wedges without the intermediate pad. Those skilled in the art will appreciate that this embodiment can be derived from the basic idea of the present invention with reference to the above embodiment.
The components of the reinforcing bar coupling are preferably made from material having strength equal to or higher than that of the reinforcing bars to be joined, to sufficiently resist tensile force or compression force acting on a ferroconcrete building incorporating the coupling. Any one of cast steel, steel, stainless steel, soft iron and synthetic resin can be selected as a material in consideration of service condition, production cost and so on.
As such, the reinforcing bar coupling according to the present invention is capable of joining reinforcing bars in various ways. Those skilled in the art will appreciate that various modifications, additions and substitutions are possible with reference to the above embodiments without departing from the scope and spirit of the invention.
As described above, though a reinforcing bar coupling according to the present invention is mainly used in such a way that wedges are driven into a cylindrical sleeve by the striking action of a hammer, the wedges may be fastened by bolts using a fastening tool such as a spanner if required. Therefore, a coupling operation of reinforcing bars is facilitated. Furthermore, site work becomes convenient owing to reduction of the number of components, and wedges cannot slide out of a cylindrical sleeve, due to engagement between serrated surfaces of the wedges and a cylindrical sleeve. The disclosed reinforcing bar coupling can be used in joining two reinforcing bars in new construction, rebuilding and repair work of various concrete structures, such as bridges and buildings. | A reinforcing bar coupling is provided for simply and quickly applying to a mechanical butt joint of two bars in the concrete constructions. The reinforcing bar coupling is consisted of a cylindrical sleeve ( 2 ) formed an uneven inner surface ( 22 ) to mate with the ribs ( 11 ) formed around outer surface of the reinforcing bars ( 1 ), an intermediate pad ( 3 ) having an uneven semi-circular surface at one side and an inclined-declined flat surface at opposite side, a gap provided between the cylindrical sleeve ( 2 ) and the intermediate pad ( 3 ), and a pair of wedges ( 4 ) being inserted into the gap. The inner surface of the cylindrical sleeve ( 2 ) and the outer surface of the reinforcing bars ( 1 ) are radially compressed to provide the butt joint of the two bars ( 1 ) by the wedging action. | 8 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to dispensing chilled fluids and, more particularly, but not by way of limitation, to a wine cooler and dispenser that provides on demand chilling and dispensing.
[0003] 2. Description of the Related Art
[0004] The packaging of wine for sale and distribution varies from bottles to bag-in-box arrangements. More expensive wines produced in limited quantities are generally packaged in bottles sealed with a cork. Less expensive wines produced in higher volumes may be packaged in bag-in-box arrangements including dispensing spigots. Alternatively, some less expensive wines may be packaged in large bottles sealed with a removable cap.
[0005] Regardless of the packaging, wine is often chilled in a refrigerator. Large gatherings thus present several problems when multiple larger bottles of wine must be chilled. Insufficient refrigerator space can result in a lack of adequate chilled wine for the gathering. Furthermore, even when there is ample refrigerator space, an incorrect estimate of the required number of bottles can occur. In either instance, the persons attending the gathering are forced to consume unchilled wine or chill the wine through the addition of ice directly into wine glasses.
[0006] Accordingly, there is a long felt need for a cost effective on demand chilling and dispensing apparatus for wine.
SUMMARY OF THE INVENTION
[0007] In accordance with the present invention, a method and apparatus for dispensing product includes a product container positioned on a housing. The product dispenser further includes a container cap attachable to a portal of the product container and a first end of a dispense tubing. A second end of the dispense tubing is connectable to a dispensing valve mountable to the housing. A thermal cooling media resides in the housing, thereby cooling the dispense tubing and its contents.
[0008] The invention provides provisions for adapting to varying product container portal sizes as commonly seen in commercial product packaging. The invention further provides for accommodating varying product container sizes. Also provided are provisions for inclusion of a product container as part of the product dispenser to be filled and refilled when emptied. Methods are provided for the installation and operation of the product dispenser, including product container installation, product container changeout, and dispensing of product from the product dispenser.
[0009] In summary, the product dispenser allows for on-demand dispensing of a chilled product directly from the product container. The product flowpath includes the product container, the container cap, the dispense tubing, and the dispensing valve. The product is cooled as it sits in the housing or as it flows through the dispense tubing to the dispensing valve. Use of this apparatus eliminates the need for prechilling of product before consumption.
[0010] It is therefore an object of this invention to provide on-demand dispensing and chilling of a product directly from the product packaging.
[0011] It is another object of this invention to provide for varying sizes of product container portals.
[0012] It is a further object of this invention to accommodate varying product container sizes.
[0013] It is still a further object of this invention to provide the ability to remove or changeout partially evacuated product containers with minimal waste.
[0014] Still other objects, features, and advantages of the invention will become evident to those of ordinary skill in the art in light of the following.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] [0015]FIG. 1 is a side view of the product dispenser with cooling media according to the preferred embodiment.
[0016] [0016]FIG. 2 is a side view of the product dispenser according to the preferred embodiment.
[0017] [0017]FIG. 3 is front view of the product dispenser with the product bottle removed according to the preferred embodiment.
[0018] [0018]FIG. 4 is a perspective view of the product dispenser lids according to the preferred embodiment.
[0019] [0019]FIG. 5 is a method flowchart for use of the product dispenser according to the preferred embodiment.
[0020] [0020]FIG. 6 is a method flowchart for changing of the product container according to the preferred embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] As required, detailed embodiments of the preferred invention are disclosed herein: however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which may be embodied in various forms. It is further to be understood that the figures are not necessarily to scale, and some features may be exaggerated to show details of particular components or steps.
[0022] The invention of discussion is an apparatus for chilling and dispensing fluids as needed for consumption. The device provides for installation and removal of empty and partially empty product containers. The device further provides for chilling a fluid as it is drawn to the point of dispense, therein eliminating pre-chilling requirements.
[0023] As shown in FIGS. 1-4, a product dispenser 100 includes a housing 110 and at least one dispensing circuit 120 . The housing 110 includes a base 112 , a vessel 114 and a plurality of lids 116 . The vessel 114 is a hollow container of any suitable material, such as glass or plastic. The vessel 114 includes a top end 123 and a lower end 124 . The lower end 124 includes a flat circular face 125 that serves as a bearing surface. The top end 123 of the vessel 114 has an aperture 126 leading to an interior cavity 127 . A lip portion 128 of the aperture 126 is formed to prevent the lids 116 from falling off of the vessel 114 .
[0024] The interior cavity 127 of the vessel 114 is designed to hold thermal cooling media, such as ice, ice water baths or the like. The vessel 114 further includes a pair of spout apertures 143 located near the lower end 124 of the vessel 114 . The location and quantity of the spout apertures 143 may vary dependent on the quantity of dispensing circuits 120 and the shape of the vessel 114 . The spout apertures 143 are outfitted with a bushing 146 and a connection tube 142 . The connection tube 142 is a short segment of rigid tubing that connects the interior cavity 127 of the vessel 114 to the environment exterior to the vessel 114 . The bushing 146 is of any suitable material, typically a soft elastomeric material such as rubber. The connection tube 142 and the bushing 146 may be sealed with any suitable sealant, including RTV or silicone to prevent leakage.
[0025] The housing 110 further includes a cap 144 , wherein the cap 144 may be installed on the connection tube 142 by a user. With the cap 144 in place, liquids cannot pass through the connection tube 142 . When the cap 144 is removed, liquids are able to pass through the connection tube 142 , therein providing a drain for the interior cavity 127 of the vessel 114 . In this configuration, the user is able to fill and drain the interior cavity 127 of liquids at will. Solids larger than an interior diameter of the connection tube 142 will not pass through the opening.
[0026] The base 112 is a rigid component having an outer surface 131 and an inner surface 132 . The base 112 is formed and trimmed to produce a flat side 133 where the inner surface 132 and the outer surface 131 come together. The flat side 133 allows the base 112 to rest on any flat or semi-flat surface such as a table or shelf. An upper end 134 of the outer surface 131 includes a depressed area 135 having a circular shape complementary to the flat circular face 125 of the lower end 124 of the vessel 114 for accepting the vessel 114 . In an alternative embodiment, the flat circular face 125 of the vessel 114 and the depressed area 135 of the base 112 may be permanently bonded together through the use of a solvent weld or mechanical fasteners.
[0027] The dispense circuit 120 includes the product container 151 having a top end 153 , a container cap 152 , the dispense tubing 145 , the connector tube 142 and a dispensing valve 150 . The product dispenser 100 may be used with multiple dispensing circuits 120 . In the preferred embodiment, a second dispense circuit 120 may be connected to the unused connection tube 142 . The product container 151 enters the aperture 126 of the vessel 114 and may come to rest on the curved entrance of the aperture 126 . The product container 151 may be the package media in which the product was purchased. In this case, the product container 151 may be used with either one lid 116 as shown in FIG. 1 or two lids 116 for product containers 151 that have a top end 153 smaller than an inner periphery 171 of the lid 116 . Therein, the product dispenser 100 is able to accommodate virtually any size product container 151 .
[0028] Alternatively, the product container 151 may be furnished as part of the product dispenser 100 to be filled with a desired product. The product container 151 , typically a bottle, is a hollow structure having an interior chamber 163 , and a portal 154 at the top end 153 . In this case, the interior chamber 163 of the product container 151 is used to house product. The portal 154 then is used for filling the product container 151 , as well as the removal of product.
[0029] In the preferred embodiment, the lids 116 are in the shape of a half-circle, with a smaller concentric circle removed. Therein, the lids have an outer periphery 170 and an inner periphery 171 . As shown in FIG. 4, the inner periphery 171 of each lid 116 comes together to form a passage for the top end 153 of the product container 151 . With this design, the lids 116 may close out the area between the product container 151 and the vessel 114 , therein insulating the interior cavity 127 from the ambient conditions. Each lid 116 may further include a knob 166 for handling during removal and installation. In cases where the top end 153 of the product container 151 does not fit within the passage, one lid may be used to partially support product container 151 as shown in FIG. 1.
[0030] The container cap 152 is an injection molded component having a hollow cylindrical shell 155 with a first end 156 and a closed end 157 . The first end 156 is complementary to the portal 154 of the package container 151 , wherein the portal 154 fits into the first end 156 of the container cap 152 . This connection may be threaded, spring-loaded or a friction fit as required to prevent leakage. In an alternative embodiment, varying sizes of container caps 152 may be provided to accommodate different package containers 151 .
[0031] The container cap 152 further includes a tubing aperture 158 that is connectable to a first end 160 of the dispense tubing 145 . As such, product may flow from the interior chamber 163 of the product container 151 , through the tubing aperture 158 of the container cap 152 and into the dispense tubing 145 .
[0032] The dispense tubing 145 includes an inner passage 147 through which fluids may flow. The dispense tubing 145 is constructed of a flexible elastomer, in this preferred embodiment silicone, to allow for flexibility in the installation and removal of the product container 151 . The dispense tubing 145 is of sufficient length to form a plurality of cooling loops 164 in the interior cavity 127 of the vessel 114 . The cooling loops 164 increase the amount of surface area of the flowing product exposed to thermal cooling media as it passes through the dispense tubing 145 . The dispense tubing is also of sufficient length to effectively chill the product as it passes from the product container 151 to a dispense point when the vessel 114 is filled with ice or other thermal cooling media.
[0033] A second end 161 of the dispense tubing 145 is connectable to an interior end 148 of the connector tube 142 . The connector tube 142 passes through the bushing 146 and the spout aperture 143 in the vessel 114 wall. An outer end 149 of the connector tube 142 is connectable to an inlet port 172 of the dispensing valve 150 for product dispensing. The connection between the connector tube 142 and the dispensing valve 150 may be of any suitable means, including a friction fit, o-rings or the like. The dispensing valve 150 further includes a handle 162 for activating and deactivating the flow of product and an outlet port 173 for outflow of product. Switching the handle 162 to an on position provides an on demand dispense of a chilled product.
[0034] In summary, the product flowpath commences in the interior chamber 163 of the product container 151 , passes through the container cap 152 , through the inner passage 147 of the dispense tubing 145 , through the cooling loops 164 of the dispense tubing 145 , through the connection tube 142 to the inlet port 172 of the dispensing valve 150 , then exiting through the outlet port 173 .
[0035] In use, a consumer must first remove the lids 116 to gain access to the interior cavity 127 of the vessel 114 as shown in step 5 of FIG. 5. Next, the consumer must open the product container 151 , step 10 . In step 15 , the consumer must attach the container cap 152 to the product container 151 , as shown in FIG. 3. At this point, the majority of the cooling loops 164 are inside of the interior cavity 127 of the vessel 114 . . The user may now fill the vessel 114 with ice or other thermal cooling media, step 20 . After connecting the container cap 152 , the user must insert the top end 153 of the product container 151 into the aperture 126 of the vessel 114 until the product container 151 engages the vessel wall as shown in step 25 . The user may then support the product container 151 with either one or both of the lids 116 , step 30 . The final resting place of the product container 151 is dependent upon the user, since the design of the vessel 114 will accommodate virtually any size product container 151 . Step 30 provides for reinstalling the lids 116 onto the vessel 114 around the product container 151 . The user may now dispense product as shown in step 35 , by activating the handle 162 .
[0036] In the case of a product changeout, the user must remove the lids 116 as shown in step 50 of FIG. 6. The process continues with step 55 and the removal of the product container 151 to be changed. The user must then disconnect the container cap 152 from the product container 151 , step 60 . At this point, the new product package must be opened or alternatively, the product container 151 must be refilled, step 65 . In step 70 , the user must connect the container cap 152 to the product container 151 to be used. Once the cap 152 is connected, the user may insert the top end 153 of the product container 151 into the vessel 114 as shown in step 75 . In step 80 , the user reinstalls the lids 116 to further support the product container 151 . The user may now dispense product, step 85 , by activating the handle 162 .
[0037] Should it become necessary to store the opened product container 151 , the user must follow steps 50 through 60 of FIG. 6 to remove the product container 151 for storage. Should the thermal cooling media have melted, the user must remove the cap 144 from the connector tube 142 to the open position to allow the water to drain from the interior cavity 127 of the vessel 114 .
[0038] Although the present invention has been described in terms of the foregoing preferred embodiment, such description has been for exemplary purposes only and, as will be apparent to those of ordinary skill in the art, many alternatives, equivalents, and variations of varying degrees will fall within the scope of the present invention. That scope, accordingly, is not to be limited in any respect by the foregoing detailed description; rather, it is defined only by the claims that follow. | A method and apparatus for on demand chilling and dispensing of product from a commercially available product package is disclosed. The product dispenser includes a product container positioned on a housing that is adapted to receive thermal cooling media. The product dispenser further includes a container cap attachable to a portal of the product container and a first end of a dispense tubing. A second end of the dispense tubing is connectable to a dispensing valve mountable to the housing, thereby regulating delivery. The thermal cooling media resides in the housing, thereby cooling the dispense tubing and its contents. Also provided are provisions for inclusion of a product container as part of the dispenser that can be filled and refilled. Further provisions include the ability to adapt to varying product container portal sizes and varying product container sizes, as commonly seen in commercial product packaging. Methods provided include installation of the product container and operation of the product dispenser. | 1 |
CROSS-REFERENCES TO RELATED APPLICATIONS
Copending application Ser. No. 492,267 filed July 26, 1974, discloses the improved hyperfiltration module sealing arrangement developed for the purposes of the present invention and also disclosed herein.
BACKGROUND OF THE INVENTION
The growing emphasis in recent years on measures to deal with water pollution problems has led to a substantial displacement of starch as the previously established standard cotton textile sizing material because of its inordinately high biological or biochemical oxygen demand value (BOD). In addition, the greatly increasing use of polyester fibers, either in blends with cotton or by itself, in the manufacture of textile fabrics has made it more difficult to obtain adequate adhesion with a starch size.
A notable alternative sizing material providing significant advantage in dealing with both of these problems is polyvinyl alcohol, which has a much reduced BOD value as well as adhering well to polyester. However, the chemical oxygen demand (COD) of polyvinyl alcohol is still appreciable and currently proposed anti-pollution standards make it necessary to avoid stream or sewer dumping of effluent from desizing operations where this alternative sizing material or others of the same sort, such as carboxymethycellulose, are used just as fully as when starch is used for sizing.
The present invention provides for handling desizing effluent in compliance with the anti-pollution standards now in prospect in a practical manner which allows advantageous recovery of the sizing material for reuse and recycling of the remaining effluent for desizing purposes.
SUMMARY OF THE INVENTION
Briefly characterized, the treatment of textile desizing effluent according to the present invention involves separation of the sizing material from the effluent in a closed loop system that returns the stripped effluent to the desizing operation. Usually, as where the size is polyvinyl alchohol, the desizing operation will be an aqueous washing procedure and the effluent will be spent wash water containing the removed size. The closed loop system provided by the invention directs this wash water effluent to selective separation means by which enough water is extracted to concentrate the contained size for recovery while making the extracted water available for recycling to the desizing operation by the system.
The selective separation means employed operates on the basis of molecular weight so as to concentrate the size by rejecting its complex molecule while passing water to produce the aqueous extract for recycling. A hyperfiltration device is preferably employed as the selective separation means because the semipermeable membrane of such a device can be selected to modulate the separation so that degraded portions of the sizing material are passed along with the extracted water to improve significantly the reuse potential of the size rejected for recovery, as is noted further in describing the invention in detail below.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flow diagram of a desizing effluent treating system embodying the present invention;
FIG. 2 is a schematic illustration of a representative hyperfiltration loop suitable for use in the treating system of the present invention;
FIG. 3 is a graphical representation of the effect of serially arranged staging of hyperfiltration loops;
FIG. 4 is a graphical representation of the variation of pertinent factors when percentage concentration of recovered size is increased while using a given number of loop stages;
FIG. 5 is a central longitudinal section of a representative hyperfiltration module for use in a treating system loop;
FIG. 6 is a bottom plan view corresponding to FIG. 5;
FIG. 7 is an enlarged sectional detail taken at the 7--7 circle in FIG. 5;
FIG. 8 is an enlarged sectional detail taken at the 8--8 circle in FIG. 5;
FIG. 9 is a corresponding section showing a modified arrangement of the FIG. 8 detail; and
FIG. 10 is an enlarged sectional detail taken at the 10--10 circle in FIG. 5.
DETAILED DESCRIPTION OF THE INVENTION
Consideration of the treating system arrangement diagrammed in FIG. 1 of the drawings should begin with the desizing washer 10 from which the effluent comes that is treated by the system. The "blowdown" indicated in FIG. 1 as leaving the system of the desizing washer 10 represents overflow wasting that is necessary, in addition to normal system losses, to avoid size buildup in the system, as will appear further presently, and to allow a substantially level size content to be maintained in the washing liquid effluent for the purposes of the present invention. The relative amount of this overflow wasting will usually be so small as to raise no pollution problem, but if it does the problem can be dealt with readily by combining it with the washer effluent for treatment in the system and making the necessary provision against size buildup by disposing appropriately of a compensating amount of the size concentrate subsequently obtained.
The desizing washer 10 may have any suitable form desired, and any washing liquid or sizing material may be used. As water is the usual washing liquid employed, and as the treating system of the present invention has been reduced to practice with polyvinyl alcohol desiring effluent, it will be assumed that the effluent is aqueous and polyvinyl alcohol is the sizing material in proceeding with the system description.
Because the weight of fabric being desized can change substantially from batch to batch, the size concentration in the desizing effluent usually varies widely, whereas efficient operation of the treating system of the present invention requires that this concentration be maintained substantially constant. Accordingly, provision is made at the desizing washer 10 to monitor the effluent as indicated at 12 and regulate the addition of makeup water, through a control valve at 14, in relation to this monitoring. Alternatively, the feed of recycled permeate to the desizing operation might be regulated instead, but water conservation considerations will normally favor regulating the makeup water. Monitoring of the desizing effluent concentration is suitably accomplished with a comparator unit operating on the basis of refractive index to sense the size content. It would also be possible to adjust the makeup water feed acceptably as a function of the weight fabric being desized, but monitoring of the effluent is preferable because it provides a continual check on size concentration. Maintenance of a substantially even concentration of size in the effluent is necessary according to the present invention for efficient operation of the treating system at the size recovery stage. An effluent size concentration of about 1% will normally be a practically convenient level to maintain.
The thus controlled desizing effluent at substantially level size content is directed first to a pre-filter unit 16 by which foreign particles are removed prior to size recovery treatment. In the case of spun yarn fabrics the foreign particles removed from the desizing effluent will consist largely of lint, which leaves the system at filter 16 as indicated in FIG. 1. A vibrating screen filter removes the lint effectively as a damp mass which can be disposed of readily. Where filament yarn fabrics are being desized foreign particle continuation of the effluent is not nearly as great, but it is still advisable to employ the prefiltering step as a means of guarding against accumulation of extraneous matter in the system.
Filtered effluent from the pre-filter 16 is collected in a buffer tank 18 for supplying the size recovery operation that follows. Buffer tank 18 serves the purpose of allowing an even feed for size recovery despite the cyclic nature of the desizing washer 10 operation in handling successive fabric batches. The size recovery operation involves concentrating and separating a predominant portion of the effluent size content in a effluent portion so that the remaining effluent can be recycled for desizing use. Such concentration and separation can be effected by any of a number of available procedures, such as evaporation or reverse osmosis, but the preferred procedure employed according to the present invention is hyperfiltration in which selective separation is obtained on the basis of molecular weight because a procedure of this sort can be modulated to recover size in a particularly advantageous manner for reuse.
The hyperfiltration units 20 preferably used to obtain this advantage in the treating system of the present invention incorporate porous carbon tube supported semipermeable membranes of the sort described in the March 1974 issue of Product Engineering at page 13. Modulation of the selective separation obtained with this type of hyperfiltration element is accomplished by choosing the membrane for the separation result desired. The particular advantage for present purposes that is obtained with such hyperfiltration elements appears to result from the ability of a properly selected membrane to provide a high percentage rejection of sizing material having a complex molecule, such as that of polyvinyl alcohol, while allowing degraded or short chain portions thereof to pass through with the effluent permeate.
This apparent result has likely significance because the sizing material is subjected to sufficient heat during slasher application, singeing of the woven fabric, and subsequent desizing, to expect some degradation, and chromatographic analysis for molecular weight distribution not only indicates such degradation but also serves to demonstrate an appreciable elimination of the resulting short chain portions during size recovery. Thus, upon such analysis of polyvinyl alcohol samples of desizing washer effluent at 1% concentration (Sample A), of a 4% concentration of the effluent (Sample B), of a further concentration of the effluent to 8.25% (Sample C), and of the virgin polyvinyl alcohol, produced the results tabulated as follows:
______________________________________APPARENT MOLECULARWEIGHT DISTRIBUTION Below BelowSample Low Mean High 10,565 31,625______________________________________A 2,291 165,200 631,000 4.0% 11.8%B 3,981 193,700 602,600 0.7% 2.7%C 6,918 151,800 602,600 0.2% 3.3%D 18,190 204,000 631,000 0% 0.6%______________________________________
While the foregoing molecular weight values are apparent values that should be understood to have significance mainly in a relative sense, the relations shown demonstrate a marked change at the low side of the molecular dispersity toward the distribution of the virgin sample (d) as the desizing effluent is concentrated, and it is believed that this circumstance accounts for the excellent reuse results noted further below that are obtained with size recovered in accordance with the present invention.
A representative arrangement for a hyperfiltration unit 20 suited for use in the treating system of the present invention is diagramed in FIG. 2 as comprising a main circulation pump 22 piped for recirculation of desizing effluent in a loop 24 containing two hyperfiltration modules 26 such as are detailed further in FIGS. 5-10 and will be additionally described below in connection with those drawing figures. Desizing effluent is delivered to the hyperfiltration unit 20 by an injection pump 28 connected with loop 24 in series with the main circulating pump 22 ahead of the filtration surfaces. Recirculating flow is maintained in loop 24 at a rate of about 2,000 gallons per minute resulting in a flow velocity of about 15 feet per second along the filtration surfaces.
Permeate consisting of the filtered effluent portion that passes through the filtration surfaces leaves the modules 26 continually and is recycled to the desizing washer 10, as indicated in FIG. 1, while the circulating effluent portion remaining in loop 24 at a proportionately increasing size concentration is taken off under the control of a valve 30 when its concentration has reached a suitable level or the level corresponding to the optimum capability of the hyperfiltration unit 20, the control valve 30 being employed to regulate the take off rate so that the concentration is maintained at this level. For the most efficient use of filtration surface area in size recovery, hyperfiltration units 20 are employed in serially arranged stages as indicated in FIG. 1 and as will be noted further presently. Upon leaving the hyperfiltration means, or whatever other concentration means is employed, a bactericide is preferably added to the recovered size concentrate in quantities of about 0.075%, as from a supply tank at 32 through a flow meter 34 under the control of a valve 36 (see FIG. 2), so that bacteriological activities, and particularly odor, are effectively dealt with.
The significance of arranging hyperfiltration units 20 in stages is graphically illustrated in FIGS. 3 and 4. For plant design purposes it is assumed in FIG. 3 that a 95% rejection of polyvinyl alcohol size is provided by the hyperfiltration units employed, that a 10% size concentration is to be obtained, that effluent is delivered from the desizing washer at 1% concentration, and that effluent is delivered at a rate of 100 gallons per minute. Under these conditions a plot of the number of stages (N) against the fraction of size recovered (rT) shows that recovery initially improves substantially as the number of stages is increased, while the related FIG. 3 curves show that at the same time the number of hyperfiltration units or loops required (nT) decreases substantially along with the plant cost per pound of size recovered.
As the FIG. 3 curves indicate that the major advantage of staging is obtained with four stages, the FIG. 4 curves plot the percentage size concentration obtained against the same factors on the assumption that four stages are used with other conditions remaining the same. The decreasing fraction of size recovered (rT) that appears in FIG. 4 with increasing size concentration recovery (KCN) is a reflection of the greater opportunity for degraded size portions to pass through the filtration surfaces with the permeate as the total number of hyperfiltration units or loops (nT) is increased to obtain higher size concentration recovery; and, as was true in FIG. 3, the indicated FIG. 4 plant cost per pound of size recovered correlates with the number of loops required (nT).
In staging the hyperfiltration units 20, an equal number of units or loops is arranged in each stage and the desizing effluent to be handled is divided equally between the first stage units which deliver to corresponding units of the next stage and so on while the concentrate outputs from the final stage are combined to proceed therefrom through the system. Thus, as 24 units or loops are indicated for the four stage conditions represented in FIGS. 3 and 4, each stage would contain six units or loops under these conditions and the 100 gallon per minute delivery of desizing effluent would be directed at the rate of 61/4 gallons per minute to each unit of the first stage for serial progress through the corresponding units of the following stages. It should be understood, of course, that the foregoing arrangement is the one indicated by the assumed conditions and the hyperfiltration arrangement will have to be designed in similar fashion for any differing set of conditions encountered. It should also be noted that when staging is employed only one injection pump 28 is required for each staged series of units and bactericide need not be added until the concentrate output from all the staged series has been pooled.
If the pooled concentrate output from the hyperfiltration means is to be reused it is preferably treated by a polishing filter, as indicated at 38 in FIG. 1, to insure a satisfactory evenness before being collected in one or more storage tanks as at 40 in FIG. 1. Such storage capacity should be equipped with heating means and with some means for keeping the stored concentrate in motion to prevent surface film formation. If the stored concentrate must be transferred to another location for reuse, the recovered size concentrate is shipped as such or it may be reduced to a dry state at a flaker as indicated respectively at 42 and 44 in FIG. 1. In any event, the recovered size concentrate is reused by moving it from storage, either directly or by one of the transfer arrangements noted above, to a sizing kettle 46. Since some of the size remains in the effluent permeate portion and there are normal system losses by reason, for example of incomplete size removal at washer 10, a virgin size supplement must be added at this stage, and it is for this reason that a compensating "blowdown" must be allowed elsewhere in the system as noted earlier. That is, as all of the size removed at washer 10 is retained either in the recycled effluent permeate or in the size concentrate recovered, addition of the virgin size supplement would cause a size buildup in the system unless a balancing "blowdown" is provided.
The virgin size supplement is added in the amount needed to bulk the amount of recovered size concentrate employed to 100%, and it has been found that loom efficiencies are equaled or bettered with recovered size mixes as compared with virgin size and that the mixture ratio is not critical. Thus, in comparative tests under identical and conventional weaving conditions with the various polyvinyl alcohol size mix ratios indicated in the following tabulation, the indicated loom efficiencies were obtained.
______________________________________LOOM EFFICIENCIES OBTAINED WITHINDICATED VIRGIN/RECOVERED SIZE MIXESTest 100/0 50/50 25/75 10/90______________________________________1 97.33 95.97 95.68 98.112 95.89 95.97 95.90 96.13______________________________________
As FIGS. 3 and 4 show that size recovery can approach 90% with a treating system arranged according to the present invention, the feasible mix ratio will be in the order of 10/90 under usual circumstances. It is also notable that the wax or the like commonly added to virgin size as a lubricant is recovered by hyperfiltration with the size concentrate so that no more than a proportionate amount of such lubricant need to be added with the virgin size supplement and the indications are that no addition of lubricant with the supplement is needed unless the performance demands during weaving are particularly heavy.
Upon suitable preparation of the size mix at kettle 46 it is delivered to a slasher 48 for warp application and the sized warp yarn is then supplied to a loom 50 where filling yarn is added to produce a fabric that is desized at washer 10 to complete the treating system circuit. The result is a closed treating system by which compliance with restrictions against desizing effluent dumping is made possible in a practical manner by reconditioning a substantial portion of the effluent for recycling and by allowing recovery of a predominant portion of the size contained in the effluent for reuse, so that signicant savings in both washing liquid requirements and in size consumption may be realized.
FIGS. 5-10 of the drawings detail the particulars of a structural arrangement suitable for hyperfiltration modules 26 when used in the treating system of the present invention, and illustrate an improved sealing arrangement for such modules as developed for the purposes of the present invention. As shown, the modules 26 incorporate a bundle of elongate, porous carbon tubes 52 lined with semipermeable membranes of the sort noted earlier. This tube bundle is fixed in sealed relation within a chamber formed in principal part by a cylindrical housing 54 so that liquid to be filtered is directed in parallel through the tubes of the bundle. The improved tube sealing arrangement comprises closure members 56 fixed, as by welding, adjacent each end of housing 54 and having a pattern of apertures 58 formed therein for respective slip fit disposition of end portions of each tube 52 therethrough. As the outer face of each closure member 56 a resilient O-ring 60 is disposed around each tube 52 and a face flange 62 having a corresponding pattern of apertures 64 formed therein for receiving the tube end portions is bolted in place over the O-rings 60 by means of studs 66 at which spacer elements or washers 68 are interposed (as seen best in FIG. 7) in a thickness proportioned to limit compression of O-rings 60 by the bolted face flanges 62 sufficiently to prevent destructive stressing of the tube end portions while allowing enough O-ring compression for effective external sealing of tubes 52 at the closure members 56.
The apertures 64 in face flanges 62 may be formed like those in closure members 56 for slip fit reception of the tube end portions as illustrated in FIG. 8, or these apertures may be enlarged in relation to those in the closure members 56, as at 64' in FIG. 9, in which case a washer 70 is additionally disposed around each tube end portion over the O-ring sealing members 60 for compressing the same when the face flanges 62 are bolted in place. Provision of enlarged face flange apertures 64' as in the FIG. 9 arrangement provides the advantage of facilitating assembly of the face flanges 62 by rendering close alignment with the closure member apertures 58 and axial trueness of the tubes 52 less critical, but involves the disadvantage of requiring that a considerable number of the additional washers 70 be handled along with the O-rings 60. No matter which of the FIG. 8 or FIG. 9 face flange arrangements is used, an end plate 72 is additionally bolted along with the face flange 62 to the closure member 56 at the outlet end of the module 26, and this end plate 72 also has a corresponding pattern of apertures 74 formed therein that are of sufficiently smaller diameter than that of the hyperfiltration tubes 52 to maintain these tubes 52 in place against endwise thrust in the outlet direction without obstructing flow therethrough (see FIG. 10). As a matter of inactive assembly the tubes 52 are held in place adequately by the O-ring sealing members 60, but static pressure differential across the module 26 and dynamic pressure at the inlet side which develop during operation exert enough endwise thrust at tubes 52 to require opposing support by the illustrated end plate arrangement.
The module housing 54 is also fitted at each end with assembly flanges 76 by which modules 26 are installed in a hyperfiltration loop unit 24 such as is diagramed in FIG. 2, and has lateral access ports 78 as well as laterally opening pipe couplings 80 adjacent each end (see FIG. 5). The access ports 78 permit installation and maintenance access to the hyperfiltration tubes 52, while the pipe couplings 80 provide respectively for withdrawal of effluent permeate and venting of module 26 depending on the vertical orientation with respect to the direction of recirculating flow in loop unit 24. That is, the upper pipe coupling 80 in FIG. 5 would be used for venting the right loop unit leg in FIG. 2 and as a permeate outlet in the left leg.
While hyperfiltration means such as has been described at length above is preferred for use in the treating system of the present invention because of the advantageous selective size recovery it evidently allows, it should also be noted that there is significant advantage in the reconditioning of the desizing effluent by the treating system for recycling and that this advantage is obtained whether or not the size is recovered in reusable form. Accordingly, the foregoing exemplary disclosure based mainly on the arrangement and operation of a treating system employing hyperfiltration and handling polyvinyl alcohol size should not be understood to exclude the use of other size separation techniques when desired or to indicate that operating results are any less effective when other types of size must be handled. | Apparatus is disclosed for treating textile desizing effluent so as to provide effective pollution abatement, and to render feasible the recovery of sizing material from the effluent for reuse as well as the conditioning of the effluent so that it may be recycled for desizing purposes. | 3 |
This application claims priority to Turkey Patent Application No. 2013/01119 filed 30 Jan. 2013, the entire contents of which is hereby incorporated by reference.
TECHNICAL FIELD
The present invention relates to a home appliance and particularly relates to a refrigerator comprising a body and a door pivotally connected to said body; and a transfer element like a cable or a pipe between the body and the door.
PRIOR ART
In some home appliances in the present art, fluid transfer is required from the home appliance body to the door or from the door to the body. For instance, in some refrigerators, water is supplied from the body to the water dispenser provided at the door. Or the water, accumulated in the waste water compartment of the water dispenser, is transferred to a chamber or to a drain provided in the body. In this case, a transfer element like a pipe should be used between the door and the body.
Again, in most of the home appliances provided in the present art, mechanisms requiring power, for instance like control panel, screen, heating resistance, etc., are provided on the door connected to the home appliance body. Said power is generally supplied by the power supply connected to the body or provided in the body. Therefore, there is a cable or a similar transfer element between the body and the door.
Said transfer elements like cable or pipe can remain between the body and the door during opening and closing of the door. Therefore, closing of the door can be prevented and the transfer element may be damaged physically. This affects operation of the home appliance in a negative manner. Moreover, the transfer element, which can be accessed easily, can be damaged by incompetent persons.
There are some embodiments in the present art for providing a solution to the described problems. As an example to this, the arrangement described in the document US 2010/176701 A1 can be given. Accordingly, the arrangement transfers a cable, exiting out of the body of a home appliance or a furniture element, to a hinged door. The arrangement includes at least one first holding member and at least one second holding member for guiding the cable. The first and second sections of the hinge are movable with respect to each other and provide opening and closing of the door. The cable is held on the hinge by means of the holding members in a manner not preventing closing of the door. However, in the document, there is no information of usage of the arrangement without the hinge.
OBJECT OF THE INVENTION
The object of the present invention is to provide a home appliance where no hinge is needed for positioning the transfer element provided between the body and the door.
In order to reach said object, the present invention is a home appliance, particularly a refrigerator, comprising a body; a door connected to the body with a hinge; a transfer element provided between the body and the door; and a guiding device guiding the transfer element between the body and the door; and that the guiding device comprises a body element fixed to the body; a door element fixed to the door; and at least one bridge element connected to the body element and the door element as compatible with the movement of the hinge and guiding the transfer element between the body element and the door element. Thus, the transfer element is carried between the door and the body by means of a guiding device carried by the door and by the body. A hinge is not needed for assembling the mechanism to the home appliance. Moreover, the transfer element is guided from the body to the door without preventing closing of the door, without giving damage and in a visually hidden manner.
In a preferred embodiment of the present invention, the guiding device comprises more than one bridge element pivotally connected to each other in series such that the first bridge element of the series of bridge elements is pivotally connected to the body element and the last bridge element of the series of bridge elements is pivotally connected to the door element. Thus, in home appliances having a door opened by means of a movement different from pivoting known in the related art or having pluralities of pivoting points, the transfer element can be guided.
In a preferred embodiment of the present invention, the guiding device comprises a connector providing the connection at at least one connection point of the guiding device. Thus, it becomes possible that one of the two elements connected to each other and particularly one of the two elements connected in a pivotal manner can pivot 180 degrees with respect to the other one. The reason of that, in some embodiments of the guiding device, the elements shall become parallel with respect to each other by means of pivotal movement. However, due to the structure of the elements, rotation of 180 degrees is not possible when the elements are connected to each other directly. Moreover, since the transfer element is folded by following an arc with a wide diameter, the fatigue on the transfer element is minimized thanks to the structure of the connector.
In a preferred embodiment of the present invention, the body element and/or the door element comprises a pin housing or a pin providing connection with the bridge element. Additionally, the connector comprises a pin housing or a pin providing connection with the bridge element and/or body element and/or door element. Moreover, the bridge element comprises a pin or a pin housing provided on at least one end of the bridge element. Thus, the axial connection between the body element, bridge element, connector and the door element is provided without the need for additional element and for additional cost.
In a preferred embodiment of the present invention, the pin housing comprises a strength element provided around the pin housing. Thus, in the elements made of a material whose strength is low, the pin housing is provided to be more resistant and to have a longer lifetime. Since material is used only in the region where strength is required, the production costs are lowered.
In a preferred embodiment of the present invention, the upper face of the pin is inclined. Thus, during the assembly, the wall having the pin housing slides on the upper face of the pin. This facilitates the assembly process.
In a preferred embodiment of the present invention, a face of the bridge element comprising the pin or the pin housing is longer than a face of the bridge element not comprising the pin or the pin housing; and excess part of the longer face of the bridge element comprises the pin or the pin housing. Thus, while the door is brought to the closed position, the transfer element is prevented from being squeezed and damaged between the bridge element and another element connected thereto. Moreover, said excess part can bend during assembly and it facilitates the assembly process.
In a preferred embodiment of the present invention, the body element comprises a groove guiding the transfer element from the body to the bridge element connected to the body element. Thus, the groove remaining between the body and the body element forms a pipe-like structure for the transfer element. Since the body is used for the pipe-like structure, in the present invention, the material costs are kept at a low level. At the same time, the molding process used for obtaining the grooved body element can be realized in an easy and rapid manner.
In a preferred embodiment of the present invention, the door element comprises a groove guiding the transfer element from the bridge element connected to the door element to the door. Thus, the groove, remaining between the door and the door element, forms a pipe-like structure for the transfer element. Since the door is used for the pipe-like structure, in the present invention, the material costs are kept at a low level. At the same time, the molding process used for obtaining the grooved door element can be realized in an easy and rapid manner.
In a preferred embodiment of the present invention, the groove comprises a C-shaped support element holding the transfer element in the groove. Thus, the transfer element is kept inside the housing. Moreover, since the support element is obtained in an orthogonal manner with respect to the walls of the housing, it supports the strength of the walls. This leads to less material usage and lower cost.
In a preferred embodiment of the present invention, the body element comprises a connection section to connect the body element to the body. Thus, the guiding device can be carried on the body without needing a hinge carrying the guiding device.
In a preferred embodiment of the present invention, the door element comprises a connection section to connect the door element to the door. Thus, the guiding device can be carried on the door without needing a hinge carrying the guiding device.
In a preferred embodiment of the present invention, the bridge element has a pipe-like form guiding the transfer element. Thus, when the door is in open position, direct physical and visual access to the transfer element is prevented. This prevents incompetent persons or harmful external effects from accessing the transfer element and provides positive contribution to the usage lifetime of the transfer element.
In a preferred embodiment of the present invention, the transfer element is a cable and/or a pipe. Thus, optionally, a fluid as water or power can be provided to an element provided on the door.
In a preferred embodiment of the present invention, the body element and/or the door element comprises a bridge housing in that the bridge element is disposed when the door is in closed position. Thus, when the door is in closed position, access to the bridge element is prevented. Moreover, in a preferred embodiment, the pin or the pin housing providing axial connection is provided on the walls of the bridge housing, the bridge element connected to the body element and/or to the door element can realize 180 degrees of pivotal movement with respect to the body element and/or with respect to the door element. Thus, when the door is in closed position, the bridge element can become parallel with respect to the body element and/or to the door element. By means of this, since the transfer element is folded by following an arc with a wide diameter, the fatigue on the transfer element is minimized.
BRIEF DESCRIPTION OF THE FIGURES
In FIG. 1 , the view of the home appliance having a guiding device and whose hinged door is in open form is given. The home appliance is viewed from the upper front side. The upper section of the home appliance is illustrated partially.
In FIG. 2 , the view of the home appliance having a guiding device and whose hinged door is in closed form is given. The home appliance is viewed from the upper front side. The upper section of the home appliance is illustrated partially.
In FIG. 3 , the isometric view of the body element of the guiding device is given. The body element is viewed from the bottom rear side.
In FIG. 4 , the isometric view of door element of the guiding device is given. The door element is viewed from the upper rear side.
In FIG. 5 , the isometric view of the bridge element of the guiding device is given.
In FIG. 6 , the isometric view of the connector of the guiding device from the upper section is given.
In FIG. 7 , the isometric view of the rear section of the guiding device which is preferably invisible by the user is given. The home appliance and the hinge are not illustrated.
In FIG. 8 , the isometric view of the front section of the guiding device which is preferably visible by the user is given. The home appliance and the hinge are not illustrated.
In FIG. 9 , the frontal isometric view of the guiding device in closed position is given. The home appliance and the hinge are not illustrated.
DETAILED DESCRIPTION OF THE INVENTION
In this detailed description, the preferred embodiments of the subject matter home appliance ( 1 ), particularly of a refrigerator are explained in the light of the annexed figures without forming any restrictive effect in order to make the subject more understandable. The direction statements like front, upper and bottom described in this document are stated with referencing the viewed section of the body ( 10 ) of the home appliance ( 1 ) presented in FIG. 1 as the “front” section of the body ( 10 ). Moreover, when the door ( 20 ) of the home appliance ( 1 ) is accessed by considering only itself, the section of the door ( 20 ) illustrated in FIG. 1 is referenced as the “front” section of the door ( 20 ).
The present invention relates to a home appliance ( 1 ), particularly relates to a refrigerator comprising a body ( 10 ); a door ( 20 ) connected to the body ( 10 ) by means of a hinge ( 21 ); a transfer element ( 30 ) extending between the body ( 10 ) and the door ( 20 ); and a guiding device ( 40 ) guiding the transfer element ( 30 ) between the body ( 10 ) and the door ( 20 ).
In FIG. 1 , the left door ( 20 ) wing and the body ( 10 ) of a two-door refrigerator presented as example to the subject matter home appliance ( 1 ) are illustrated. The door ( 20 ) is in open position. In the example home appliance ( 1 ), the hinge ( 21 ) has three pivot points such that there is one each pivot points on the doors ( 20 ) and there is one pivot point on the body ( 10 ). Thus, when the door ( 20 ) passes to closed position as in FIG. 2 , it roughly takes the form of Z shape. The preferred embodiment of the guiding device ( 40 ) comprises three pivot points or in other words three folding points in a similar manner to the hinge ( 21 ). However, if the design allows, the hinge ( 21 ) or the guiding device ( 40 ) may have less than three or more than three pivot points.
Even if the guiding device ( 40 ) is positioned just above the hinge ( 21 ) in the preferred home appliance ( 1 ), the guiding device ( 40 ) does not need a hinge ( 21 ) for assembly to the home appliance ( 1 ) as described above and as exemplified in the figures. Since, the guiding device ( 40 ) comprises a body element ( 100 ) fixed to the body ( 10 ), a door element ( 200 ) fixed to the door ( 20 ), a bridge element ( 300 ) carried by them or pluralities of bridge elements ( 300 ) connected in a series manner so as to make pivoting movement.
In FIG. 3 , the preferred body element ( 100 ) embodiment is illustrated. In a compliant manner, the body element ( 100 ) is a long and linear element. Roughly, it comprises two parallel plates as the bottom face ( 104 ) and the upper face ( 102 ) and a wall ( 106 ) between them provided in an orthogonal manner with respect to them. The upper face ( 102 ) comprises a connection section ( 110 ) providing fixation to the body ( 10 ). The connection section ( 110 ) is preferably a plate extending along the body element ( 100 ). There is one or more than one connection hole ( 111 ) thereon. It is fixed to the front frame ( 11 ) of the body ( 10 ) by means of a screw and a similar fixation element through the connection hole ( 111 ). In other words, the body element ( 100 ) extends in a parallel manner with respect to the upper edge of the body ( 10 ).
The upper face ( 102 ), the bottom face ( 104 ) and the wall ( 106 ) form a groove ( 140 ) on the side facing the body ( 10 ). This groove ( 140 ) provides the transfer element ( 30 ) to be guided from the body ( 10 ) to the bridge element ( 300 ). After the body element ( 100 ) is fixed to the body ( 10 ), the open face of the groove ( 140 ) is covered by the front frame ( 11 ). Thus, the transfer element ( 30 ) is hidden in a channel like a pipe whose four sides are closed.
In the preferred embodiment, there is a C-shaped support element ( 141 ) inside the groove ( 140 ). The support element ( 141 ) preferably comprises an inner gap having a width wherein a cable known in the related art can be placed. The support element ( 141 ) is in the form of a plate extending between the upper face ( 102 ) and the bottom face ( 104 ) in an orthogonal manner with respect to said faces. When the plate is viewed from the front side, the C form can be seen. There are preferably pluralities support elements ( 141 ) at certain intervals along the groove ( 140 ) ( FIG. 3 ). The support element ( 141 ) provides the transfer element ( 30 ) to be kept inside the groove ( 140 ). Moreover, since it extends between the upper face ( 102 ) and the bottom face ( 104 ) in an orthogonal manner, it supports the strength of both of said faces.
There is a bridge housing ( 120 ) on the side of the wall ( 106 ) of the body element ( 100 ) which is opposite with respect to the groove ( 140 ). The bridge housing ( 120 ) is formed by the parts of the upper face ( 102 ) and of the bottom face ( 104 ) remaining on the other side of the wall ( 106 ) with respect to the groove ( 140 ). The bridge housing ( 120 ) is formed by the wall ( 106 ) and by means of the upper face ( 102 ) and the bottom face ( 104 ) ( FIG. 3 ). The single lateral face and the ends of the bridge housing ( 120 ) are open like the groove ( 140 ). The bridge housing ( 120 ) is preferably a housing having the same length as the bridge element ( 300 ). There is a pin housing ( 130 ) or a pin on the upper face ( 102 ) and on the bottom face ( 104 ) forming the bridge housing ( 120 ), providing direct or indirect connection with the bridge element ( 300 ). In the preferred embodiment, the bridge element ( 300 ) is directly connected to the body element ( 100 ). Therefore, in order for the guiding device ( 40 ) to be folded completely ( FIG. 9 ), there has to be a sufficient gap around the rotation axis. For this reason, the pin or the pin housing ( 130 ), preferably the pin housing ( 130 ) is positioned at the corner, where the open face of the bridge housing ( 120 ), and the end of the body element ( 100 ), where the bridge element ( 300 ) is connected, intersect ( FIG. 3 ).
The preferred door element ( 200 ) is illustrated representatively in FIG. 4 . The door element ( 200 ) has a first section ( 201 ) and a second section ( 202 ). The first section ( 201 ) and the second section ( 202 ) are preferably in one-piece form. The first section ( 201 ) has the same structure as the body element ( 100 ), it is long and linear. The only difference is that the first section ( 201 ) is shorter than the second section ( 202 ) in length. In a compliant manner to this, the two parallel plates as the bottom face ( 204 ) and the upper face ( 203 ) comprise a wall ( 205 ) in between which is orthogonal with respect to said faces. However, there is not a connection section ( 210 ) on the upper face ( 203 ). However, the first section ( 201 ) may comprise one or more than one connection sections ( 110 ) optionally.
The upper face ( 203 ), the bottom face ( 204 ) and the wall ( 205 ) form a groove ( 240 ) on the side facing the door ( 20 ). This groove ( 240 ) provides the transfer element ( 30 ) to be guided from the bridge element ( 300 ) to the door ( 20 ). After the door element ( 200 ) is fixed to the door ( 20 ), the open face of the groove ( 240 ) is closed by the door ( 20 ). Thus, the transfer element ( 30 ) is hidden in a channel whose four sides are closed and which is similar to a pipe.
In the preferred embodiment, there is a C-shaped support element ( 241 ) inside the groove ( 240 ). The support element ( 241 ) preferably comprises an inner gap having a width wherein a cable known in the related art can be disposed. The support element ( 241 ) is in the form of a plate between the upper face ( 203 ) and the bottom face ( 204 ) and it extends orthogonally with respect to said faces. When the plate is viewed from the front, the C form can be seen. Preferably, there are pluralities of support elements ( 241 ) at certain intervals along the groove ( 240 ) ( FIG. 4 ). The support element ( 241 ) provides the transfer element ( 30 ) to be held inside the groove ( 240 ). Moreover, since it extends in an orthogonal manner between the upper face ( 203 ) and the bottom face ( 204 ), it supports the resistance of both these faces.
There is a bridge housing ( 220 ) on the side of the wall ( 205 ) of the door element ( 200 ) opposite with respect to the groove ( 240 ). The bridge housing ( 220 ) is formed by means of the portions of the upper face ( 203 ) and of the bottom face ( 204 ) which remain on the other side of the wall ( 205 ) opposite with respect to the groove ( 240 ). The bridge housing ( 220 ) is formed by the upper face ( 203 ) and the bottom face ( 204 ) and the wall ( 205 ) ( FIG. 4 ). One lateral face and the ends of the bridge housing ( 220 ) are open in a similar manner to the groove ( 240 ). The bridge housing ( 220 ) is a housing which preferably has the same length as the bridge element ( 300 ). There is a pin housing ( 230 ) or a pin, providing direct or indirect connection with the bridge element ( 300 ), on the upper face ( 203 ) and the bottom face ( 204 ) forming the bridge housing ( 220 ). In the preferred embodiment, the bridge element ( 300 ) is directly connected to the door element ( 200 ). Therefore, there has to be sufficient gap around the rotation axis in order for the guiding device ( 40 ) to be completely folded ( FIG. 9 ). For this reason, the pin or the pin housing ( 230 ), preferably the pin housing ( 230 ), is positioned at the corner where the open face of the bridge housing ( 220 ) and the end of the door element ( 200 ), the bridge element ( 300 ) is connected thereto, intersect ( FIG. 4 ).
The second section ( 202 ) of the door element ( 200 ) is preferably orthogonal with respect to the first section ( 201 ) and parallel with respect to the lateral edge of the door ( 20 ). The second section ( 202 ) is structurally like the continuation of the first section ( 201 ). For this reason, the upper face ( 203 ), the bottom face ( 204 ) and the wall ( 205 ) continue in a structural manner, and extend in a slightly orthogonal direction by drawing an arc of 90 degrees. However, preferably the upper face ( 203 ) draws an arc in an earlier manner than the bottom face ( 204 ). Therefore, the groove ( 240 ) obtains a form having a width such that only a transfer element ( 30 ) is placed. For this reason, there is no support element ( 241 ) therein ( FIG. 4 ). The upper face ( 203 ) and the bottom face ( 204 ) preferably do not extend towards the other side of the wall ( 205 ) with respect to the door ( 20 ) ( FIG. 8 ).
There is preferably one connection section ( 210 ) of the door element ( 200 ) and it is preferably provided in the second section ( 202 ). The connection section ( 210 ) is a plate in ring form provided in an orthogonal manner with respect to the bottom face ( 204 ) at the side of the bottom face ( 204 ) remaining outside of the groove ( 240 ). Thus, a connection hole ( 211 ) is formed. The door element ( 200 ) is fixed to the door ( 20 ) by means of a fixation element like a screw and similar element through the connection hole ( 211 ). Optionally, more than one connection section ( 210 ) can be formed. The connection section ( 210 ) comprises one or more than one support wall ( 212 ) between the bottom face ( 204 ) and the connection section ( 210 ) in order to increase resistance ( FIG. 8 ).
In the home appliance ( 1 ) presented in the figures, a fixation element passing through the connection section ( 210 ) provides the connection of the hinge ( 21 ) to the door ( 20 ). However, this does not mean that a hinge ( 21 ) is needed for fixing the door element ( 200 ) to the door ( 20 ). The door element ( 200 ) can be fixed to the door ( 20 ) without the hinge ( 21 ).
In FIG. 5 , the preferred embodiment of the bridge element ( 300 ) is illustrated. The bridge element ( 300 ) preferably comprises an upper face ( 302 ), a bottom face ( 304 ) and two mutual lateral faces ( 306 ) in a pipe-like manner. The bridge element ( 300 ) has a rectangular cross section. It is long and linear; however, it is preferably shorter than the first section ( 201 ) of the door element ( 200 ) and of the body element ( 100 ). The transfer element ( 30 ) can pass therethrough easily. The bridge element ( 300 ) can accommodate the transfer element ( 30 ) which is longer than the bridge element ( 300 ) in order for the bending in the transfer element ( 30 ) to be unproblematic during folding of the guiding device ( 40 ).
The bridge element ( 300 ) comprises a pin ( 300 ) or a pin housing provided on at least one end thereof. In the preferred embodiment, there is one each pins ( 310 ) on both ends of the bridge element ( 300 ) at the upper face ( 302 ) and at the bottom face ( 304 ). The upper face ( 302 ) and the bottom face ( 304 ) of the bridge element ( 300 ) are longer than the lateral faces ( 306 ). The pin ( 310 ) is provided at this long section, in other words, it is provided in the excess sections with respect to the lateral faces ( 306 ). Preferably, the length of the excess section is equal to the diameter/width of the pin ( 310 ).
In FIG. 6 , the preferred embodiment of the connector ( 400 ) used in the present invention is illustrated. The connector ( 400 ) can be optionally used in every pivot point of the guiding device ( 40 ). For this reason, the elements, which have to be connected in the related rotation point, are connected indirectly by the connector ( 400 ). However, in the preferred embodiment, the connector ( 400 ) only connects the adjacent bridge elements ( 300 ) when pluralities of bridge elements ( 300 ) are used ( FIGS. 7 and 8 ).
The connector ( 400 ) comprises a wall ( 440 ) between the upper face ( 410 ) and the bottom face ( 420 ) parallel with respect to each other, and said wall ( 440 ) extends orthogonally with respect to said faces. The upper face ( 410 ) and the bottom face ( 420 ) have a quadrangular and preferably a rectangular area. The wall ( 440 ) joins only a single edge of the quadrangles. Thus, the three lateral faces of the connector ( 400 ) are open. The wall ( 440 ) moreover has an arc form; it does not have a flat form. Thus, it presents a wider area during folding of the transfer element ( 30 ).
Since the connector ( 400 ) is used for interconnecting two elements, on each of the upper face ( 410 ) and of the bottom face ( 420 ), there are two pin housings ( 430 ), two pins or one pin-one pin housing ( 430 ). The preferred connector ( 400 ) comprises two pin housings ( 430 ) on each face ( 410 , 420 ).
On the outside face of the wall ( 440 ) of the connector ( 400 ), there is a strength element ( 441 ) extending along the wall ( 440 ). It is preferably in the form of an orthogonal prism formed in an integrated manner in the intermediate section of the wall ( 440 ) ( FIG. 6 ).
All of the elements of the guiding device ( 40 ) are preferably obtained from a flexible and resistant material like plastic. However, a material known in the related art can also be used.
There is preferably a strength element ( 131 , 231 , 431 ) around the periphery of all the pin housings ( 130 , 230 , 430 ) provided in the invention. The strength element ( 131 , 231 , 431 ) is formed by keeping the material thickness around the pin housing ( 130 , 230 , 430 ), which is in hole form, wider than the other regions ( FIGS. 3 , 4 and 6 ).
The pins ( 310 ) are placed to the pin housings ( 130 , 230 , 430 ) of the door element ( 200 ), the body element ( 100 ), the connector ( 400 ) and/or the adjacent bridge element ( 300 ). Thus, said pivot connections are provided. The upper face ( 311 ) of the pins ( 310 ) present in the invention is preferably formed in inclined manner. Thus, during the assembly of the guiding device ( 40 ), the faces ( 102 , 104 , 203 , 204 , 410 , 420 ) having pin housings ( 130 , 230 , 430 ) can advance on the upper face ( 311 ) of the pin ( 310 ) by sliding. Thus, the assembly process is facilitated.
In the preferred embodiment, only the bridge element ( 300 ) comprises a pin ( 310 ). Therefore, the height of the lateral faces ( 306 ) of the bridge element ( 300 ) is shorter than the inner height of the bridge housings ( 120 , 220 ) and shorter than the height between the upper face ( 410 ) and the bottom face ( 420 ) of the connector ( 400 ). Thus, the ends of the bridge element ( 300 ) can enter into the related gaps.
The transfer element ( 30 ) used in the present invention and described above with reference to the figures is preferably an electrical cable. However, it can be a different purpose cable or a fluid pipe.
Both of the connection sections ( 110 , 210 ) provided in the body element ( 100 ) and the door element ( 200 ) can optionally be a long plate as the connection section ( 110 ) or a ring as the connection section ( 210 ).
When the preferred guiding device ( 40 ) having two bridge elements ( 300 ) is desired to be assembled;
The body element ( 100 ) is fixed to the body ( 10 ) thanks to the connection section ( 110 ), A bridge element ( 300 ) is pushed into the bridge housing ( 120 ) from a corner of the bridge housing ( 120 ) where the pin housing ( 130 ) is provided through the end thereof where the pin ( 310 ) is provided, and the pins ( 310 ) exit out of the pin housings ( 130 ) outwardly from the bridge housing ( 120 ), The free end of the bridge element ( 300 ) is pushed into the connector ( 400 ) in the same manner, the pins ( 310 ) are placed to the pin housings ( 430 ) of the connector ( 400 ); however, here connection is realized such that the wall ( 440 ) of the connector ( 400 ) is at a point far from the door ( 20 ) as in FIG. 1 , Afterwards, the second bridge element ( 300 ) is connected to the other pin housings ( 430 ) of the connector ( 400 ) in the same manner, The free end of the second bridge element ( 300 ) is connected in the same manner to the bridge housing ( 220 ) of the door element ( 200 ), Finally, the door element ( 200 ) is fixed to the door ( 20 ).
However, the door element ( 200 ) is preferably fixed to such a point that even if the door ( 20 ) is opened completely, the angle of the two bridge elements ( 300 ) in a manner facing the door ( 20 ) is equal to 180 degrees or smaller than 180 degrees. Moreover, when the connector ( 400 ) is connected as described, it prevents said angle from being more than 180 degrees.
REFERENCE NUMBERS
1.
Home appliance
10.
Body
11.
Front frame
20.
Door
21.
Hinge
30.
Transfer element
40.
Guiding device
100.
Body element
102.
Upper face
104.
Bottom face
106.
Wall
110.
Connection section
111.
Connection hole
120.
Bridge housing
130.
Pin housing
131.
Strength element
140.
Groove
141.
Support element
200.
Door element
201.
First section
202.
Second section
203.
Upper face
204.
Bottom face
205.
Wall
210.
Connection section
211.
Connection hole
212.
Support wall
220.
Bridge housing
230.
Pin housing
231.
Strength element
240.
Groove
241.
Support element
300.
Bridge element
302.
Upper face
304.
Bottom face
306.
Lateral face
310.
Pin
311.
Upper face
400.
Connector
410.
Upper face
420.
Bottom face
430.
Pin housing
431.
Strength element
440.
Wall
441.
Strength element | A home appliance, e.g., a refrigerator, includes a body; a door connected to the body with a hinge; a transfer element provided between the body and the door; and a guiding device guiding the transfer element between the body and the door. The guiding device includes a body element fixed to the body; a door element fixed to the door; and at least one bridge element pivotally connected to the body element and the door element as compatible with the movement of the hinge and guiding the transfer element between the body element and the door element. | 5 |
BACKGROUND OF THE INVENTION
[0001] The invention relates to telescopes, and more particularly relates to optical telescopes that are capable of operation in the visible and near-infrared portions of the electromagnetic spectrum. In its most immediate sense, the invention relates to optical telescopes and optical telescope arrays that are suitable for use in spacecraft (such as satellites) and other remote sensing applications.
[0002] Universities use nanosatellites for research in astronomy, climatology, and earth science. And, use of nanosatellites for both commercial and governmental purposes has been contemplated. For example, a nanosatellite network could be used to monitor the entire length of a pipeline in order to prevent oil or gasoline thefts by detecting persons who bring unauthorized truck-sized vehicles in the pipeline's vicinity. Alternatively, nanosatellites can be used for e.g. border control (monitoring aircraft that may be transporting drugs, monitoring movements of guerrillas) or prevention of environmental disasters (such as international fires in large extensions of protected forests).
[0003] An optical telescope intended for use in a spacecraft such as a nanosatellite must meet demanding constraints. It must be small, light, well-balanced, and mechanically robust. It must also be easily customizable; some nanosatellite applications will require a wide field of view, while others will require high resolution images, and still others will require the ability to acquire spectroscopic data or polarimetry data.
[0004] Therefore, objects of the invention are to provide an optical telescope and an optical telescope array for use in spacecraft and remote sensing applications such as nanosatellites, which telescope and array are small, light, well-balanced, mechanically robust, and easily customizable.
[0005] Conventional catadioptric optical telescopes of the Maksutov-Cassegrain type have excellent mechanical features; they are small, light, well-balanced, and mechanically robust. However, when used at wavelengths of between 400 and 1000 nm (visible to near-infrared radiation, which are required for nanosatellite applications) they have unacceptable levels of astigmatism, coma, and color spherical aberrations. And customizing a conventional Maksutov-Cassegrain telescope to meet the requirements of different nanosatellite applications would be quite difficult.
[0006] The invention proceeds from two realizations. The first of these is the realization that if a conventional Maksutov-Cassegrain telescope design is modified to employ second-surface reflection for the primary mirror and the secondary spot mirror (instead of first-surface reflection, which is conventional) the optical aberrations of the original design can be brought within acceptable limits while still preserving its advantageous features insofar as size, weight, balance, and robust character are concerned.
[0007] The second realization is that by using a binocular array made up of two telescopes having such a modified design, customization can be accomplished easily and inexpensively. This can be done by changing the orientation of the telescopes with respect to each other, changing the coatings on the lenses, and changing the filters that are used. If for example the telescopes are parallel with each other so that their fields of view coincide to be the same at the intended distance from the satellite, a high-resolution image can be obtained. Alternatively, if an image of a large area is desired, the telescopes can be precisely disinclined so that the fields of view at the intended distance are non-overlapping. Acquisition of spectroscopic and polarimetry data can be accomplished by using suitable coatings on the lenses and suitable filters, and it is possible to acquire both image data and spectroscopic or polarimetry data by configuring one telescope to acquire an image while configuring the other to acquire the non-image data desired.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The invention will be better understood with reference to the following illustrative and non-limiting drawings, in which:
[0009] FIG. 1 is a schematic representation of the operation of a conventional catadioptric Maksutov-Cassegrain optical telescope;
[0010] FIG. 2 is a schematic representation of the operation of a catadioptric optical telescope in accordance with the invention;
[0011] FIG. 3 is a schematic diagram of a telescope in accordance with a preferred embodiment of the invention;
[0012] FIG. 4 is a schematic diagram of a binocular telescope array in accordance with the invention;
[0013] FIG. 5A is a schematic illustration of the operation of a first preferred embodiment of a binocular telescope array in accordance with the invention; and
[0014] FIG. 5B is a schematic illustration of the operation of a first preferred embodiment of a binocular telescope array in accordance with the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0015] In all the Figures, each element is always identified by the same reference numeral, and corresponding elements are identified using primed reference numerals. The Figures are not to scale; dimensions have been enlarged or reduced for clarity.
[0016] FIG. 1 shows a schematic representation of how a conventional catadioptric Maksutov-Cassegrain optical telescope operates in the wavelength range of 400 nm to 1000 nm. Incoming rays 2 , 4 , 6 , and 8 enter the entrance end 200 of the telescope through its spherical meniscus corrector lens 10 , which is made of optical glass and disperses them radially outwardly. They then strike the spherical reflective surface of the primary mirror 12 (which has an aperture 16 in its center) and are reflected back toward the corrector lens 10 , where they are made incident upon a secondary “spot” mirror 14 . After reflection from the secondary spot mirror 14 , the rays 2 , 4 , 6 , and 8 are directed towards a circular aperture 16 that is located in the center of the primary mirror 12 .
[0017] Each of the mirrors 12 and 14 is formed by a layer of reflective material located on the first surface of the mirror. (The term “first surface” is used because the ray of light is reflected from the first surface it encounters.) As a result, by the time the rays 2 , 4 , 6 , and 8 have reflected off the secondary spot mirror 14 , the image formed by those rays suffers from aberrations, which include distortion, astigmatism, coma, and color spherical aberration. Corrector lenses 18 are used to correct for these aberrations, and the rays 2 , 4 , 6 , and 8 then pass through a field flattener lens 20 to become incident upon a sensor 22 (such as a CMOS sensor) at the exit end 210 of the telescope.
[0018] FIG. 2 is a schematic illustration of the operation of a telescope in accordance with the invention. Here, rays 2 , 4 , 6 , and 8 are dispersed radially outwardly by a spherical meniscus corrector lens 10 ′ at the entrance end 200 ′ of the telescope and are incident upon the primary mirror 12 ′. The primary mirror 12 ′, is of the Mangin type; it is a negative meniscus lens with a circular aperture 16 ′ in its center. Here, the reflection is from the second surface of the primary mirror 12 ′; the primary mirror 12 ′ is made of optical glass and the rays 2 , 4 , 6 , and 8 pass through its first surface and are reflected only when they reach its second surface. The primary mirror 12 ′ thus acts not only as a mirror, but also as a triplet lens (because the light rays are deflected twice, once when they enter the primary mirror 12 ′ and once when they leave it).
[0019] After reflection from the second surface of the primary mirror 12 ′, the rays 2 , 4 , 6 , and 8 are made incident upon a secondary spot mirror 14 ′ that is located on the second surface of the corrector lens 10 ′. As in the case of the primary mirror 12 ′, the secondary spot mirror 14 ′ also functions as a lens because the corrector lens 10 ′ is a spherical meniscus lens.
[0020] As can be seen by comparing FIG. 1 and FIG. 2 , a telescope in accordance with the invention does not require corrector lenses located between the corrector lens 10 or 10 ′ and the primary mirror 12 or 12 ′. It requires only a field flattener lens 20 ′, which is located ahead of the CMOS sensor 22 at the exit end 210 ′ of the telescope.
[0021] FIG. 3 is a diagram schematically illustrating the dimensions of a preferred embodiment of a telescope in accordance with the invention. In this preferred embodiment:
[0022] a cylindrical baffle 30 is located in front of the corrector lens 10 ′;
[0023] another cylindrical baffle 32 is located in front of the primary mirror 12 ′;
[0024] a conical baffle 34 is located behind the corrector lens 10 ′; and
[0025] a filter 24 is interposed between the field flattener lens 20 ′ and the detector 22 .
[0000] Baffles such as 30 , 32 , and 34 are conventionally used in Maksutov-Cassegrain optical telescopes; the baffles are made of aluminum and they block stray light. As will be discussed below, the filter 24 is selected in accordance with the data to be captured by the detector 22 .
[0026] The glass used in the preferred embodiment shown in FIG. 3 is N-BK7, which has a refractive index n=1.5168. The focal length of this preferred embodiment is 1500 mm and its speed is f/10. At an intended observation distance of 700 km (i.e. the distance between a microsatellite in a 700 km orbit and at the earth) the preferred embodiment has a field of view that is 20 km in diameter.
[0027] In accordance with the invention, a binocular array of catadioptric optical telescopes is constructed. Advantageously, each of the telescopes is the above-discussed preferred embodiment of a telescope in accordance with the invention. As will become evident below, this permits the array to be easily and inexpensively customized for particular applications.
[0028] An array in accordance with the preferred embodiment is made up of two telescopes as described above. The telescopes 100 and 110 are mounted in a housing 120 ( FIG. 4 ) made of a ceramic having the same thermal coefficient as the glass in the corrector lenses 10 ′ and the primary mirrors 12 ′. The housing 120 has an entrance end 120 A where the corrector lenses 10 ′ are located and an exit end 120 B where the CMOS sensors 22 are located.
[0029] If a particular application requires a high-definition visual image, the housing 120 can be constructed with the axes of the telescopes 100 and 110 being non-parallel, whereby the telescopes 100 and 110 have the same approximately 20 km field of view at an intended observation distance of 700 km ( FIG. 5A ). At that distance, an array in accordance with the preferred embodiment can produce an image having a resolution of approximately 3 m. Alternatively, if it is more important to have a larger field of view, the housing 120 ′ can be constructed with the axes of the telescopes 100 and 110 being parallel, whereby the array has a field of view that is approximately 40 km wide ( FIG. 5B ).
[0030] A telescope in accordance with the preferred embodiment can operate in the visual and near-infrared portions of the electromagnetic spectrum, between wavelengths of 400 nm and 1000 nm. To customize a telescope and a telescope array in accordance with the invention, the coatings on the various lenses and the filters 24 are chosen to correspond to optimize the performance of the telescope and array in the portion(s) of the electromagnetic spectrum that is or are of interest. Advantageously, BEAR antireflection coating is used on lens surfaces that transmit light, and protected silver is used for surfaces that reflect light. Typical filters 24 are precision band-pass filters working at different wavelength bands, such as 400 nm-700 nm and 700 nm-1000 nm. Furthermore, an array in accordance with the invention can be customized in such a manner that one of the telescopes is optimized to operate in the visual portion of the electromagnetic spectrum while the other is optimized to operate in the near-infrared so as to collect spectroscopic or polarimetry data. Alternatively, the array can be customized in such a manner that one of the telescopes is optimized to collect spectroscopic data while the other is optimized to collect polarimetric data. In such instances, the two telescopes will usually share the same field of view, so that acquired image data correlates with acquired infra-red data and so that acquired data from one portion of the electromagnetic spectrum correlates with acquired data from another portion.
[0031] Although a preferred embodiment has been described above, the scope of the invention is limited only by the following claims: | A catadioptric telescope is a modified version of a conventional Maksutov-Cassegrain optical telescope. In accordance with the invention, the reflecting surfaces of the primary mirror and the secondary spot mirror are on the second surfaces of the primary mirror and correcting lens, respectively. In further accordance with the invention, two of these telescopes can be joined together to form a binocular telescope array. The array can be easily customized to suit different remote sensing/satellite applications. | 6 |
BACKGROUND OF THE INVENTION
This invention relates to an on-machine calender which can be connected to a paper machine or the like for finishing treatment of a fiber web, which calder includes a first hard roll and a second hard roll at a distance from the first one and in addition at least two elastic rolls mounted on bearings in movable supporting means in a way which permits the elastic rolls to be moved into a working position so as to define calendering nips with the hard rolls and, in addition, a number of paper guiding rolls for leading the web run through said calendering nips.
Furthermore the invention relates to a method in an on-machine finishing treatment of a web-like material which treatment takes place in a calendering apparatus in which a first and a second hard roll and at least two elastic rolls are employed, the elastic ones being arranged so as to define calendering nips with said hard rolls which nips all are substantially at a same horizontal level and in which calender the hard rolls are substantially at a same horizontal level and in which the elastic rolls are, with respect to each other, substantially at a same horizontal level which is above that of the hard rolls.
An important stage in finishing treatment of the paper is its calendering by which an influence exerted on the smoothness and gloss of the surface of the paper and the thickness and the density of the paper. Calendering takes place while passing the continuous paper web through particular pressing points, or nips, formed between coacting calender rolls.
Conventionally the calendering of paper is effected by means of a so-called machine calender which is directly associated with the paper machine said calendering treatment being complemented, if necessary, by a supercalendering treatment in a separate so-called supercalender which gives the paper more gloss.
The rolls used in calenders are either hard or elastic rolls. By hard rolls are meant in this context rolls having a shell material of e.g. chill-cast iron or steel and of which the surface acting on the paper is ground glossy. A conventional machine calender has hard rolls only and the nips between them are so-called hard nips.
Elastic rolls refer in the following to rolls in which the surface acting on the surface of the web is of resilient material. This kind of rolls which are used in supercalenders define together with the hard rolls so-called soft nips.
As material for the mantles of the elastic rolls paper sheets are commonly used which are cut into disks, assembled as courses on the roll shaft and thereafter pressed in a direction parallel with the shaft into a solid, compact and quite thick covering of the rolls. Nowadays various plastic-based coverings are also used which are commonly relatively thin due to which it is possible to equip the body of the roll with internal deflection compensation means without increasing the diameter of the roll to an excessive extent.
As is known in the prior art, machine-calendering can also be carried out with a single-nip calender, that is with a calender in which only one pair of rolls defines a nip, depending on the brand of the paper to be treated and the requirements therein imposed. In most cases, however, a machine-calender includes four to eight rolls which thus define three to seven hard nips. As a result of the machinecalendering process the possible thick areas in the web are smoothed out so that the web achieves the required thickness, or the so-called caliper.
Conventionally, by means of a supercalender provided with soft nips only, it is usually attempted to achieve equal gloss for both sides of the web. This requires at least two soft nips and in addition arranged usually in such a way that both sides of the web will be against the surface of a hard roll in an equal number of nips which surface primarily gives gloss for the web. A separate supercalender may include as many as ten pairs of nips. As a result of supercalendering the web usually acquires even density and smoothness.
To boost the production of a paper machine it has been found necessary to attempt to accomplish such an immediately to a paper machine connected calender unit which combines the functions of both a machine-calender and a supercalender. Such calenders have been disclosed e.g. in U.S. Pat. Nos. 4,128,053; 4,332,191; and 4,375,118.
Although machine-calenders and supercalenders usually include eight to ten nips it has been found that even two soft nips alone can give the paper produced such a gloss and smoothness and/or additional properties which are sufficient for most purposes. This results from the fact that the paper coming from the paper machine to calendering treatment is in respect of its formation and fibre distribution usually considerably more even and can be thus more easily calendered than e.g. paper produced according to the technology in use of e.g. about twenty years ago due to the today's web-formation techniques and the control systems therein involved. The development on one hand in the materials for elastic coverings and on the other hand in the properties of the paper to be glazed which can be influenced by applying a thin layer of a suitable paste on the surface of the paper, or coating the semi-finished web e.g. at some stage of the drying in a paper machine, makes it possible to use calender structures which differ from and are even more simple than the previous ones.
The most generally accepted comprehension of the influence of the supercalendering on the web to be processed is that a higher gloss is produced on the surface facing the hard roll in the nip. There are, however, several factors which together affect the gloss and smoothness such as nip load, the possible difference in the rotation speeds of the elastic roll and the hard roll, and as an important factor, the material of the elastic covering. Development work is continuing, especially regarding the last-mentioned factor, and covering materials new and/or under development may give reason to revise theories about calendering.
SUMMARY OF THE INVENTION
This invention relates in particular to such on-machine combination calenders or machine-supercalenders in which there are two nips only in their most simple embodiments.
The object of this invention is to improve previously known so-called on-machine supercalenders connected to either paper machines or cardboard machines in which calenders there are at least two soft nips, meaning nips formed between an elastic roll and a hard roll by means of which a matt, so-called soft-gloss or -smoothness is obtained on the web.
An additional object of the invention is to provide a soft-calendering apparatus more simple than those previously known in which apparatus one of the elastic rolls which is damaged during the operation of the calender, or any function of said roll can, as quickly as possible, be replaced with a new one, in many cases during the continuous operation of the calender.
Furthermore, the object of the invention is to provide a softcalendering apparatus by means of which, if necessary, an intensified treatment may be induced on either one side of the fiber web.
Still one object of the invention is to provide a calender in which the nip pressures may be adjusted separately and independently of each other. A further additional object is to provide a calender which is structurally open in a way which makes it possible to place possible devices for spreading and damping the paper web and measuring its moisture in an advantageous way and, if necessary, even before each calendering nip. Another additional object is to provide a calender in which there is a possibility for tail threading by means of a rope carrier system known in itself.
To attain the above-mentioned aims and others, which will become apparent later on, the on-machine calender of the invention for finishing treatment of a fiber web is mainly characterized in that the hard rolls are at substantially the same horizontal level, and in that the elastic rolls are, with respect to each other, at the same horizontal level above that of the hard rolls.
The proceudre of the invention is for its part mainly characterized in that the paper web is treated in the calendering nips formed between the hard rolls and said elastic rolls so that in the first nip the lower side of the web faces the first hard roll and so that in the nip or nips in connection with the second hard roll the opposite side, that is, the upper side of the web, faces the hard roll.
The calendering nips are preferably defined against either upper quadrant of both hard rolls. Preferably, the nips are defined on the periphery of a hard roll, within an area the width or circumferential angle of which is about 30°-60° with respect to the horizontal level. The circumferential angle is more preferably about 40°-50° with respect to the horizontal level.
BRIEF DESCRIPTION OF THE DRAWINGS
In the following, the invention shall be described in detail, with reference being made to certain embodiment examples of the invention, presented in the figures of the attached drawing, to the details of which the invention is not strictly confined. In the drawings,
FIG. 1 displays diagrammatically a calender roll group of the invention, which includes two hard rolls and three elastic rolls as a two-nip version, in which the middle one of its three elastic rolls acts as a reserve roll, and the course of the web through the roll group;
FIG. 1A displays an alternative course of the web, in accordance with a calender roll group shown in FIG. 1;
FIG. 2 displays diagrammatically the course of the web through a two-nip version of a calender roll group according to the invention in which version the elastic reserve roll has been moved so as to define a calendering nip with the latter hard roll in the direction of the web run;
FIG. 3, correspondingly, displays a calender roll group of the invention as a two-nip application in which the elastic reserve roll defines a nip with the first hard roll in the direction of the web run;
FIG. 3A displays an alternative passage of the web, in a calender roll group according to FIG. 2.
FIG. 4 displays the diagrammatically the passage of the web in a calender roll group of the invention in which the elastic reserve roll acts as an additional active roll against the latter hard roll; in this case the calender operates as a three-nip calender so that the upper surface of the web being calendered will face the same hard roll in the two last nips;
FIG. 5 displays a calender roll group of the invention in which the elastic reserve roll acts as an additional active roll against the first hard roll; the calender operates as a three-nip calender so that in this case the lower surface of the web faces the same hard roll consecutively in the first two nips;
FIG. 6 shows, mainly according to FIG. 1, an on-machine calender with its frame structure and supporting means for the various rolls and loading means for the various nips.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A diagrammatically depicted structure shown in FIG. 1, in which the passage, indicated by W in -W out , of the web W to be treated goes from right to left in the direction shown by the arrow, includes a first hard roll 1 and a second hard roll 2 and three elastic rolls 3,4 and 5 of which at least hard rolls 1,2 and advantageously also elastic rolls 3,4 and 5 are equipped with speed-controlled drive means. In addition to the working rolls defining calendering nips the calender includes a number of web-guiding rolls 6,7,8,9,10 and 11 by means of which the travel of the web W may be directed through calender nips N 1 and N 2 in a desired manner. The first elastic roll 3 in the travel of the web W defines a soft nip N 1 with the first hard roll 1, the calender being an on-machine calender. The web W coming from drying section of a paper machine or the like (not shown) is guided to this nip N 1 in such a way that makes the lower surface of the web W face the hard roll 1. The web W may flutter before the nip N 1 so as to cause wrinkling of the web. To avoid this and to restrain the fluttering, the guide roll 6 is placed so that the web W wraps the roll 1 before the nip N 1 in a sector of at least appr. 10° to 20°.
After the nip N 1 the web is transferred guided by the rolls 7 and 8 underneath the latter (i.e. second) hard roll 2 to the second nip N 2 , defined between the elastic roll 5 and the second hard roll 2. In this nip in its turn the upper surface will face the hard roll. Thus both sides of the web W receive, in principle, the same kind of treatment, provided that the nip load is substantially the same in both nips. After the nip N 2 the travel of the web is passed via the guide roll 9 further to the reeling device which can be of the conventional Pope-type (not shown). What was presented above of restraining the fluttering of the web before the first calendering nip applies also in the case of the nip N 2 as well. Accordingly, the guide roll 8 is placed so that the web W wraps the roll 2 in a sector of at least appr. 10°-20° before the nip N 2 .
The hard rolls 1 and 2 and also the elastic rolls 3,4 and 5 may be equipped with deflection compensation means known per se in the art and which rolls may be e.g. so-called Kusters-rolls. Deflection compensation is almost indispensable in both hard and elastic rolls at least in calenders of large working width. Narrow calenders can be without accomplished deflection compensation. As is well known, the rolls can be crowned instead, but in that case an even line pressure is achieved at a certain nip load only.
The elastic rolls 3 and 5 shown in FIG. 1 have been mounted on bearings in special supporting arms in the frame columns of the calender which are more in detail presented in FIG. 6 later on. The loading of rolls 3 and 5 against hard rolls 1 and 2 is effected by means of e.g. hydraulic working cylinders actuating the supporting arms by means of which the required nip pressure may be imposed. By means of the same working cylinders and supporting arms the rolls may also be completely released from nip contact e.g. in the start-up phase of the paper machine or in case of operational trouble in the threading of the web W.
In FIG. 1 the elastic roll 4, which is provided in the calender for serving as a reserve roll ready for use in the case that either one of the elastic rolls 3 or 5, would become damaged, has been mounted on bearings in a vertical supporting arm, as is presented in more detail in connection of FIG. 6. The roll 4, if necessary, can be quickly moved into nip contact with either the first hard roll 1 or the second hard roll 2.
The roll combination and the calendering nip arrangement displayed in FIG. 1A is the same as the one shown in FIG. 1. What is different is however that threading of the web W is arranged to take place over the reserve roll 4, guided by the rolls 10 amd 11. According to this solution the length of the run of the web W between the nips N 1 and N 2 is increased to be about 11/2 times longer compared to that shown in FIG. 1, and it allows the width of the web W to increase freely in case the web W has been moisturized close to the nip N 1 (either before or after the nip) e.g. by water spraying or steam treatment (not shown) which can separately and adjustably be directed toward both the upper and lower surfaces so as to control the two-sidedness of the paper. That side of the web which is more uneven requires usually more effective moisturizing.
According to FIG. 2, the third elastic roll 5 is shown as having been disconnected, e.g. for reparation, from nip contact with the hard roll 2 shown in FIG. 1 and the nip in question, nip N 2 , has been replaced by the nip N 2 formed between roll 4 and roll 2. Also in this alternative nip N 2 the upper side of the web W will face a hard roll and the run of the web W through the calender and the treatment given to web W corresponds to that displayed in FIG. 1. In order to change the nip N 2 of FIG. 1 →N 2 of FIG. 2, the web has to be guided counterclockwise around the roll 4. To make this possible either the web has to be cut purposely or alternatively the nip change may take place during such a production break that occasionally occurs in the normal operation of a paper machine.
According to FIG. 3, the first elastic roll 3 has been shown as having been disconnected from nip contact with the hard roll 1 e.g. for maintenance which nip N 1 , has in this case been replaced by nip N 10 defined between the reserve roll 4 and the hard roll 1. This change of nip N 1 →N 10 does not require any cutting of the web W and may therefore be effectd in various ways during the continuous run of the paper machine. One possibility is to move the roll 4 first to a working position, that is, into nip contact with the hard roll 1 which roll momentarily will be in contact with two elastic rolls 3 and 4. It is not necessary, however, to load these in full simultaneously, which arrangement may be accomplished by some automatic means known in the art. Immediately after the roll 4 has reached full load, or nip pressure in the nip N 10 , the nip N 1 is opened after which the roll 3 may be demounted from its supporting arms for maintenance.
The roll combination and calendering nip arrangement displayed in FIG. 3A is the same as shown in FIG. 3. The difference is, however, that the web is led to the latter (second) calendering nip N 2 from an opposite direction compared to that shown in FIG. 3, which constructively requires changing the direction of rotation of the hard roll 2. Regarding the calendering procedure itself, the solution means that the lower surface of the web to be calendered receives an intensified treatment since it faces a hard roll in both the nips N 1 and N 2 . This kind of treatment can come into question in cases when calendering a web made with a single-wire fourdrinier paper machine, in which cases the lower surface of the web may show occasionally a very heavy wire marking.
As shown in FIG. 4 the elastic rolls 4 and 5 operate simultaneously against the hard roll 2 so that in the nips N 1 and N 21 thereby defined the upper surface of the web W faces the hard roll 2 and obtains thus a higher gloss (ironing effect) than the lower surface which faces the elastic rolls 4 and 5. This function of the calender corresponds to the structure shown in FIG. 1 with the exception that the reserve roll 4 also is in this case in a working position. The course of the web W has to be guided around the roll 4 in the same way as in FIG. 2. This cannot be arranged during the continuous run of the calender but requires an either accidental or intentional break in production in order to move the reserve roll 4 from its rest position into a working position displayed in FIG. 4, and guiding the web accordingly.
FIG. 4 furthermore displays an in some cases favourable operational solution in which the web W is guided over a springy suspended additional roll 10 between the nips N 2 and N 21 . The purpose of this arrangement is to eliminate the effects of the possible stretching of the web W between nips N 2 and N 21 which otherwise may result in wrinkling of the web in the nip N 21 . It is not, however, necessary to lead the web in this way.
Also in the structure displayed in FIG. 5, an intensified treatment of one side of the web is accomplished and in this case of the lower side. In this case, the elastic rolls 3 and 4 define two consecutive nips N 1 and N 11 with the first hard roll 1 so that the lower surface of the web W face the hard roll 1 and obtains a higher gloss onto its lower surface (ironing effect). Forming of consecutive nips N 1 and N 11 against the hard roll 1 is possible even during continuous operation by moving the roll 4 from its rest position against the roll 1. It is advantageous, however, in the same way as shown in FIG. 4, to arrange the course of the web W to be guided over an additional, flexibly supported spring roll 11 which eliminates the disturbing effect which is caused by the stretching of the web to the function of the calender between nips N 1 and N 11 . A short production break in the operation of the calender is required also in this case for the re-threading of the web.
An intensified calendering treatment is usually applied to that surface of the web W which is more uneven caused by the function of the wet end of the paper machine. In manufacturing certain special paper brands, this intensified burnishing may be applied to the upper web surface which by nature is smoother than the lower wire side e.g. in paper made by a fourdrinier-machine.
FIG. 6 displays, in elevational view from the tending side, one frame structure of the calender of the invention including the supporting and loading means of the rolls thereof. The frame 100 of the calender consists of two vertical columns 6a and 6b and a connecting horizontal beam 7 therebetween. Corresponding beams and columns are on the drive side of the calender at a distance determined by the working width of the calender.
The hard rolls 1 and 2 included in the calender are mounted fixedly on bearings resting on supporting brackets 8a and 8b. Of the elastic rolls 3,4 and 5 of the calender the rolls 3 and 5 are mounted substantially on bearings on supporting arms 11a and 11b placed on vertical columns 6a and 6b. Opening and closing of the nip N 1 between the rolls 1 and 3, and the adjustment of corresponding nip load are effected by means of a working cylinder 10a resting on a console 9a which cylinder influences on the supporting arm 11a by turning it around the pivot shaft 12a. Correspondingly, the adjustment of operation and load of the nip N 2 between rolls 2 and 5 is effected by means of the supporting arm 11b. The elastic roll 4 provided for acting as a reserve roll is mounted on bearings on the substantially vertical supporting arm 13, the position and movement of which around the pivot point 17 is actuated by the working cylinders 16a and 16b which are supported by bracket means 15a and 15b. The working cylinders 16a and 16b are most appropriately hydraulically operated and with the aid of them the pendular movement of the supporting arm 13 is brought about so that the roll 4 may define nip N 10 (FIG. 3) either with roll 1 or nip N 2 (FIG. 2) with roll 2.
In the start-up phase, the web may arrive in the calender occasionally, irregularly wrinkled, and even in thick lumps. At this step the nips have to be open so that damage to the elastic rolls can be avoided. Threading the lead-in strip of the web can be done with a rope carrier system known in the art and the start-up phase continues until an even and uninterrupted run of the web has been established, whereafter the nips can be closed and loaded to a required extent.
Removal of the elastic rolls 3 and 5 can be done e.g. with the aid of roll changing device disclosed in the FI-patent No. 65462 of the applicant. For removing the roll 4 a recess 18 in the foundation of the calender is provided.
In FIGS. 1-5 the continuous lines represent various courses of the web through the calender of the invention. A common feature in several of these is the relatively long path of the web W from the first nip to the second one between the first and the second hard roll. Such a long path is of importance e.g. in case the web is moisturized in the region of the first nip. This results in the tendency of the web to become broader, which has to be allowed to take place freely and if possible, completely before the next nip.
If the web W is not moistened during the calendering, guiding of the web W may be realized following the shortest-way -principle of which some examples have been illustrated by the dotted lines in FIGS. 1,2 and 4. The choice of solution for guiding the web W through the nips of the calender depends e.g. on the paper brand and/or its possible coating and among other things on the running speed of the calender and applied nip pressures.
The inventive concept is described above, and various details of the invention may vary within the scope thereof. | Method and apparatus for the finishing of a fiber web (W) by means of an on-machine calender connected to a paper machine or the like. The calendering apparatus includes a first hard roll (1) and a second hard roll (2) which is at a distance from the first one, and at substantially the same horizontal level, and in addition at least two elastic rolls (3,4,5) mounted on bearings borne by movable support (9,10,11,12). The elastic rolls (3,5) define in a working position calendering nips with the hard rolls (1,2). A number of paper guiding rolls (6,7,8,9,10,11) lead the course (W in →W out ) of the web (W) through the calendering nips. The elastic rolls (3,4,5) have been arranged with respect to the hard rolls (1,2) so that the calendering nips (N 1 , N 10 , N 11 ,N 2 , N 20 , N 21 ) can be defined against the upper quadrant of the hard rolls (1,2) at substantially the same horizontal level with each other. | 3 |
BACKGROUND OF THE INVENTION
The present invention relates to a new and distinct Impatiens plant botanically known as Impatiens walleriana×Impatiens auricoma and hereinafter referred to by the cultivar name ‘Balfusglo’.
The new cultivar was developed by the inventors in a controlled breeding program during September 1999 at Elburn, Ill. The objective of the breeding program was to develop Impatiens cultivars with numerous flowers, new and unique flower shape and colors, excellent basal branching, and upright compact to moderate growth habit.
The female (seed) parent of ‘Balfusglo’ was the proprietary Impatiens walleriana selection designated ‘9516-4’ (not patented) characterized by its upright growth habit, coral-colored flowers, and medium green-colored foliage. The male (pollen) parent of ‘Balfusglo’ was the proprietary Impatiens auricoma selection designated ‘193’ (not patented) characterized by its upright growth habit, yellow-colored flowers, and dark green-colored foliage. ‘Balfusglo’ was discovered and selected as a single flowering plant within the progeny of the above stated cross-pollination in August of 2000 at Elburn, Ill. and initially designated ‘PAS T31-08’.
Asexual reproduction of the new cultivar by shoot tip or stem cuttings since August 2000 at Elburn, Ill. and West Chicago, Ill., has demonstrated that the new cultivar reproduce true to type with all the characteristics, as herein described, firmly fixed and retained through successive generations of such asexual propagation.
SUMMARY OF THE INVENTION
The new cultivar has not been observed under all possible environmental conditions to date. Accordingly, it is possible that the phenotype may vary somewhat with variations in the environment, such as temperature, light intensity, and day length without, however, any variance in genotype.
It was repeatedly found that the cultivar of the present invention:
1. Exhibits single, cupped, yellow-colored flowers,
2. Forms medium green-colored foliage,
3. Exhibits a good basal branching character, and
4. Exhibits an upright mounded growth habit.
Plants of the new cultivar differ from plants of the female parent primarily in flower color, flower shape and leaf shape, and from plants of the male parent in flower color, flower shape, leaf size, and branching habit.
Plants of the new cultivar can be compared to plants of ‘96-009-7’ (U.S. Plant Pat. No. 10,972). However, in a side-by-side comparison conducted in West Chicago, Ill., plants of the new cultivar differed from plants of ‘96-009-7’ primarily in the following characteristics:
1. Plants of the new cultivar have a more compact growth habit than plants of ‘96-009-7’, and
2. Plants of the new cultivar have larger flowers than plants of ‘96-009-7’.
BRIEF DESCRIPTION OF THE PHOTOGRAPHS
The accompanying photographs show as nearly true as it is reasonably possible to make the same in color illustrations of this type, typical flower and foliage characteristics of the new cultivar. Colors in the photographs differ slightly from the color values cited in the detailed description, which accurately describe the colors of ‘Balfusglo’. The plants were grown for 13 weeks in a greenhouse at West Chicago, Ill.
FIG. 1 illustrates a side view of the overall growth and flowering habit of ‘Balfusglo’.
FIG. 2 illustrates a close-up view of a single flower of ‘Balfusglo’.
DETAILED DESCRIPTION
The chart used in the identification of colors described herein is The R.H.S. Colour Chart of The Royal Horticultural Society, London, England, 1995 edition, except where general color terms of ordinary significance are used. The color values were determined on Sep. 3, 2003 between 9:00 and 10:45 a.m. under natural light conditions.
The following measurements and comparisons describe plants produced from shoot tip or stem cuttings taken from stock plants and grown under greenhouse conditions comparable to those used in commercial practice. The plants were grown in 10 cm pots for 15 weeks utilizing a soilless growth medium. Greenhouse temperatures were maintained at approximately 72° F. during the day and approximately 65° F. during the night. Greenhouse light levels were maintained at approximately 4,000 to 6,000 footcandles during the day.
Botanical classification: Impatiens walleriana×Impatiens auricoma cultivar ‘Balfusglo’.
Parentage:
Female ( seed ) parent.— Proprietary Impatiens walleriana selection designated ‘9516-4’ (not patented).
Male ( pollen ) parent.— Proprietary Impatiens auricoma selection designated ‘193’ (not patented).
Propagation:
Type cutting.— Shoot tip or stem (with two nodes).
Time to initiate roots.— Approximately 7-14 days.
Time to develop a rooted cutting.— Approximately 21 days.
Root description.— Fine, fibrous.
Rooting habit.— Freely branching.
Plant description:
Habit of growth.— Moderately vigorous with good basal branching. A mature plant, 15 weeks after the planting of a rooted cutting, commonly measures approximately 25.8 cm in height and approximately 42.1 cm in width.
Plant form.— Upright and mounded.
Lateral branches.— Quantity: Approximately 4. Length: Approximately 19.9 cm. Diameter: Approximately 8 mm. Texture: Glabrous. Color: 146C with streaks of 187B especially at nodes. Internode length at center of branch: Approximately 3.3 cm.
Foliage.— Type: Simple. Arrangement of lower leaves: Alternate. Arrangement of upper leaves: Whorls. Shape: Elliptic. Apex: Acuminate/cuspidate. Base: Attenuate. Margin: Crenate with ciliation. Texture of upper and lower surface: Glabrous. Venation pattern: Pinnate, arcuate. Size of mature foliage: Length: Approximately 8 cm. Width: Approximately 3.7 cm. Color of mature foliage: Upper surface: 137A with veins and mid-vein of 146D. Lower surface: 147B with veins and mid-vein of 146D. Petiole: Diameter: Approximately 2 mm. Length: Approximately 2.3 cm with 2 mm stipules along edges. Texture: Upper and lower surface: Glabrous. Color: Upper and lower surface: 146D with overlay of 187D.
Flower description:
Flower type.— Single, not fragrant with self-cleaning petals.
Flowering habit.— Freely flowering with flowers positioned above the foliage and facing outward.
Natural flowering season.— Year round in greenhouse environment. Flowering is continuous from spring until fall in the garden.
Flower longevity on plant.— Approximately 5 days.
Quantity of flowers.— Approximately 5 flowers and 5 buds per stem at any one time.
Mature flower buds ( just before opening ).—Shape: Ovate. Length: Approximately 1.3 cm. Diameter: Approximately 9.4 mm. Texture: Glabrous. Color: 15D.
Flower shape.— Oval, cupped when first open, becoming more flat with age.
Flower size.— Length: Approximately 3.8 cm. Width: Approximately 3.3 cm. Depth: Approximately 1.2 cm.
Petals.— Number: Five per flower. Texture: Glabrous. Appearance: Iridescent.
Superior petal.— Length: Approximately 1.3 cm. Width: Approximately 1.2 cm. Shape: Cucullate. Margin: Entire. Apex: Emarginate. Base: Truncate. Color of upper surface: 9D. Color of lower surface: 9D.
Lateral petals.— Length: 1.6 cm. Width: 1.4 cm. Shape: Obovate. Margin: Entire. Apex: Obtuse. Base: Attenuate. Color of upper surface: 9D with faint spot of 32B and veins of 46A along inner edge. Color of lower surface: 9D.
Lower petals.— Length: 2.2 cm. Width: 1.2 cm. Shape: Obovate. Margin: Entire. Apex: Obtuse. Base: Attenuate. Color of upper surface: 9D with center of petal having a small area of 32B. Color of lower surface: 9D.
Peduncles.— Strength: Strong. Angle to stem: Acute. Length: Approximately 2.6 cm. Diameter: Approximately 1 mm. Texture: Glabrous. Color: 144B.
Calyx.— Consists of 3 sepals. Lateral sepals: Length: Approximately 8 mm. Width: Approximately 5 mm. Texture: Glabrous. Color of both surfaces: 1D with tip of 144C. Lower sepal: Length: Approximately 1.4 cm. Width: Approximately 9 mm. Texture: Glabrous. Color of both surfaces: 1D with tip of 144C. Base of lower sepal is modified to form spur.
Spur.— Quantity: One per flower. Double tipped. Length: Approximately 1.5 cm. Diameter at flower: Approximately 2 mm. Diameter of tips: Approximately 1 mm. Aspect: Moderately curved downward. Color: 1C.
Reproductive organs.— Androecium: Five stamens, anthers are fused together forming one organ that surrounds the pistil. Filament color: 1C. Anther shape: Oval. Anther length: Approximately 2 mm. Anther color: Lighter than 35D. Gynoecium: Pistil number: One per flower. Pistil length: 6 mm. Stigma shape: Five pointed star. Stigma length: 0.5 mm. Stigma color: Colorless, translucent. Style length: 1.5 mm. Style color: Colorless, translucent. Ovary length: 4 mm. Ovary diameter: 2 mm. Ovary texture: Glabrous. Ovary color: 149A.
Seed and fruit development: Neither seed nor fruit production has been observed.
Disease and pest resistance: Resistance to pathogens and pests common to Impatiens has not been observed. | A new and distinct cultivar of Impatiens plant named ‘Balfusglo’, characterized by its single, cupped, yellow-colored flowers, medium green-colored foliage, upright and mounded habit, and excellent basal branching. | 0 |
BACKGROUND OF THE INVENTION
The present invention relates to microencapsulated adhesives and processes for producing such microencapsulated adhesives. More particularly, the invention relates to a process for microencapsulating acrylate-based or methacrylate-based adhesives to produce an adhesive composition that is initially non-tacky but exhibits tacky properties upon application of external forces, such as shearing.
Adhesive compositions are generally tacky and gluey. However, there are numerous applications where it would be beneficial to mask the tacky nature of the adhesive prior to its use. Examples of such applications include adhesive materials for stamps or envelopes.
One potential way of rendering adhesives non-tacky is to microencapsulate the adhesive. Various attempts have been made to encapsulate adhesives such as hot melt ethylene/vinyl acetate copolymers and styrene/isoprene/styrene-type block copolymers. However, due to their high molecular weight and high viscosity, these copolymers tend to be solids at room temperature and precipitate when emulsified, and thus are very difficult to microencapsulate.
It is an object of the present invention to produce an adhesive composition that is initially non-tacky but can be made tacky when desired.
Another object of the present invention is to provide an adhesive compound that can be microencapsulated.
A further object of the present invention is to provide a monomer compound that is capable of being microencapsulated and is also capable of being polymerized inside the microcapsules to form a polymer adhesive.
The present inventor has found that acrylate or methacrylate monomers can be microencapsulated by well-known microencapsulation techniques, and then these monomers can be polymerized inside the microcapsules to form adhesives. These microencapsulated adhesives are initially non-tacky, but when external forces such as shearing are applied, the capsules break and the tacky adhesive is exposed.
SUMMARY OF THE INVENTION
To achieve the objects and in accordance with the purpose of the invention, as embodied and broadly described herein, the invention comprises a method of producing a microencapsulated adhesive by providing a mixture containing as a major component, an alkyl acrylate or alkyl methacrylate monomer, or a mixture thereof, along with a free radical initiator. This mixture of monomer and initiator is microencapsulated. The microencapsulated monomer and initiator is heated for a time and a temperature sufficient to cause the monomer to polymerize inside the microcapsules.
In another aspect of the present invention, there is provided a microencapsulated adhesive composition containing an adhesive produced from a monomer including as a major component an alkyl acrylate or methacrylate, or a mixture thereof, encapsulated in microcapsules. This composition functions as an adhesive that is initially non-tacky but exhibits tacky properties upon application of external forces, such as shearing. Specifically, upon application of an external force, such as shearing, at least some of the microcapsules are broken and the adhesive is exposed.
In a further aspect of the present invention, there is provided a microencapsulated adhesive composition produced by microencapsulating a mixture containing as a major component, an alkyl acrylate or methacrylate monomer having about 4 to about 12 carbon atoms, or a mixture thereof, along with a free radical initiator. The microencapsulated monomer and initiator are heated for a time and at a temperature sufficient to cause the monomer to polymerize inside the microcapsules. The adhesive that is formed is initially non-tacky but exhibits tacky properties upon the application of external forces, such as shearing.
Additional objects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objects and advantages of the invention will be realized and attained by means of the elements and combinations particularly pointed out in the appended claims.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with the present invention, microencapsulated adhesives are produced from monomers having as a major component an alkyl acrylate or methacrylate monomer, or a mixture thereof. The acrylate or methacrylate monomers used as a major component of the adhesives of the invention generally have very low viscosity and thus are capable of being encapsulated. Preferably, the monomer of the invention is a C 4 -C 12 alkyl acrylate or methacrylate. It is to be understood, however, that any acrylate-based or methacrylate-based monomer that is capable of being polymerized inside microcapsules and is useful as an adhesive is within the scope of the present invention. In addition, other monomers such as vinyl acetate, styrene, acrylonitrile, methacrylonitrile, and the like can be present in the invention as a minor component. Following encapsulation, the monomers can be polymerized in the microcapsules by heating.
Examples of the acrylate and methacrylate monomers that can be used as the major component in accordance with the invention include, but are not limited to: isobutyl acrylate, isobutyl methacrylate, isodecyl acrylate, isodecyl methacrylate, isooctyl acrylate, 2-ethyl hexyl acrylate, isobornyl acrylate, 4-methyl-2-pentyl acrylate, 2-methyl butyl acrylate, isoamyl acrylate, isononyl acrylate and the like. Preferred monomers are isodecyl methacrylate and a mixture of ethyl hexyl acrylate and isobornyl acrylate.
In accordance with the invention, the monomers may be polymerized in the microcapsule by heating to a temperature sufficient to cause a reaction exotherm to be observed. After the reaction exotherm is reached, the microcapsule solution is preferably further heated to a temperature of about 5 degrees greater than the exotherm temperature for a period preferably ranging from about 4 to about 6 hours to complete the free radical polymerization.
In accordance with the invention, the adhesive can be microencapsulated by those techniques known in the art, including interfacial polymerization, gelatin/gum arabic coacervation and melamine/formaldehyde encapsulation. A preferred encapsulation technique is interfacial polymerization. The walls of the microcapsules are preferably comprised of polyamide or polyurea.
The interfacial polymerization method that may be used in accordance with the invention involves mixing the adhesive monomer or monomers to be microencapsulated together with a free radical initiator and either an acid chloride or an isocyanate. The resultant mixture is emulsified in an emulsification agent to obtain an oil-in-water emulsion. A polyfunctional amino compound is then added into the emulsion, whereby microcapsule walls are formed around each microparticle of oil. In accordance with the invention, when an acid chloride is mixed with the monomer and initiator, a polyamide microcapsule is produced—when an isocyanate is mixed with the monomer and initiator, polyurea capsules are formed. After the monomer or monomers and initiator are microencapsulated, the entire composition is heated to thermally polymerize the monomer or monomers inside the microcapsules.
The gelatin/gum arabic coacervation encapsulation method that may be used in accordance with the present invention involves first emulsifying the core material into a gelatin solution to obtain an oil-in-water emulsion. The emulsion is mixed with a gum arabic solution. The system is then pH adjusted or diluted to cause the gelatin/gum arabic to coacervate. Thereafter, the capsules are post-treated with a crosslinking agent, such as formaldehyde, glutaldehyde, or other similar known compounds.
The melamine-formaldehyde encapsulation method that may be used in accordance with the present invention involves first emulsifying the core material into a carboxyl methyl cellulose solution or a poly(styrene-maleic anhydride) solution to obtain an oil-in-water emulsion. The emulsion is then mixed with a melamine-formaldehyde precondensate solution. The system is then pH adjusted, followed by heating to initiate polymerization of the precondensate to a high molecular weight compound. The presence of the carboxyl methyl cellulose or poly(styrene-maleic anhydride) solution helps the polymerized melamine-formaldehyde to deposit onto the core material surfaces, thereby encapsulating the core.
The free radical initiator that can be used in accordance with the invention is any oil-soluble, thermal activatable free radical initiator known in the art. Examples of such free radical initiators include, but are not limited to: benzoyl peroxide, t-amyl peroxyneodecanoate, t-amyl peroxypivalate, t-amyl peroxy-2-ethyl-hexanoate, t-butyl peroxyisobutyrate, t-amyl perbenzoate, di-t-butyl peroxide, 2,2′-azobis(2-methylbutyronitrile), 2,2′-azobis(2,4-dimethylvaleronitrile), 2,2′-azobis(2-methylpropanenitrile), and the like. A preferred initiator for use in the invention is benzoyl peroxide.
Acid chlorides that can be used in the invention to produce polyamide microcapsules include, but are not limited to: terephthaloyl chloride, isophthaloyl chloride, 1,3,5-benzenetricarboxylic acid chloride, sebacyl dichloride, 4,4-sulfonyldibenzoyl chloride, 1,3-benzenedisulfonyl chloride, 1,4-benzenedisulfonyl chloride, or mixtures thereof. A preferred acid chloride for use in the invention is a mixture of isophthaloyl chloride and terephthaloyl chloride.
Isocyanate compounds that can be used in the invention to produce polyurea microcapsules include, but are not limited to: 2,4- and 2,6-diisocyanatotoluene, 4,4′-diisocyanato-diphenyl methane, 1,3,5-trimethylbenzene-2,4-diisocyanate, 1,6-diisocyanato-hexane, polymethylene polyphenyl isocyanate, polyisocyanates which additionally contain biuret-, allophanate-, and carbodiimide groups, and the like. A preferred isocyanate for use in the invention is Desmodur N-100, a polyfunctional aliphatic isocyanate compound containing a biuret linkage commercially available from Mobay Chemicals.
Examples of polyfunctional amines that can be used in the invention include, but are not limited to: ethylene diamine, diethylene triamine, triethylene tetramine, tetraethylene pentamine 1,6 hexanediamine, polyethyleneimine, bis-hexamethylenetriamine, and the like. A preferred polyfunctional amine for use in the invention is diethylene triamine.
The emulsification agents that can be used in accordance with the invention include those compounds that contain both hydrophilic and hydrophobic groups in the same molecule. Examples include, but are not limited to: partially hydrolyzed polyvinyl alcohol, starch derivatives, cellulose derivatives, polyacrylamide, and the like. A preferred emulsification agent for use in the invention is partially hydrolyzed polyvinyl alcohol.
The following examples are illustrative of the invention embodied herein and are not to be considered limiting.
EXAMPLE 1
60 parts of ethyl hexyl acrylate/isobornyl acrylate (at a 7/3 ratio by weight) and 0.13 parts of benzoyl peroxide were mixed with 2.39 parts of isophthaloyl chloride/1.02 parts of terephthaloyl chloride. The resultant mixture was emulsified into 110 parts of 2% Vinol 523 solution in a Waring blender. Vinol 523 is a partially hydrolyzed polyvinyl alcohol, commercially available from Air Products and Chemicals. To this emulsion, 20 parts of an aqueous solution containing 1.38 parts of diethylenetriamine, 0.54 part of NaOH, and 0.71 part of sodium carbonate was added. The mixture was stirred at room temperature, under mild agitation, for 16 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 120 microns, with an average of about 40 microns.
The content was then heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for about 5 hours to complete the free radical polymerization.
EXAMPLE 2
60 parts of isodecyl methacrylate and 0.12 parts of benzoyl peroxide were mixed with 2.39 parts of isophthaloyl chloride/1.02 parts of terephthaloyl chloride. The resultant mixture was emulsified into 110 parts of 2% Vinol 523 solution in a Waring blender. To this emulsion, 20 parts of an aqueous solution containing 1.38 parts of diethylenetriamine, 0.54 part of NaOH, and 0.71 part of sodium carbonate was added. The mixture was stirred at room temperature, under mild agitation, for 16 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 140 microns, with an average of about 45 microns.
The content was heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for about 5 hours to complete the free radical polymerization.
EXAMPLE 3
60 parts of ethyl hexyl acrylate/isobornyl acrylate (at a 7/3 weight ratio) and 0.12 parts of benzoyl peroxide were mixed with 5.65 parts of Desmodur N-100. Desmodur N-100 is a polyfunctional aliphatic isocyanate compound containing a biuret linkage, commercially available from Mobay Chemicals. The resultant mixture was emulsified into 110 parts of 2% Vinol 523 solution in a Waring blender. To this emulsion, 20 parts of an aqueous solution containing 1.02 parts of diethylenetriamine was added. The mixture was stirred at 60° C. under mild agitation for 2 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 150 microns, with an average of about 48 microns.
The content was heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for 5 hours to complete the free radical polymerization.
EXAMPLE 4
60 parts of isodecyl methacrylate and 0.12 parts of benzoyl peroxide were mixed with 5.65 parts of Desmodur N-100. The resultant mixture was emulsified into 110 parts of a 2% Vinol 523 solution in a Waring blender. To this emulsion, 20 parts of an aqueous solution containing 1.02 parts of diethylenetriamine was added. The mixture was stirred at 60° C. under mild agitation for 2 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 145 microns, with an average of about 45 microns.
The content was then heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for 5 hours to complete the free radical polymerization.
EXAMPLE 5
60 parts of ethyl hexyl acrylate/isobornyl acrylate (at a 7/3 weight ratio) and 0.12 parts of benzoyl peroxide were mixed with 5.65 parts of Desmodur N-100. The resultant mixture was emulsified into 110 parts of a 1% Vinol 523 solution in a Waring blender. To this emulsion, 20 parts of an aqueous solution containing 1.02 parts of diethylenetriamine was added. The mixture was stirred at 60° C. under mild agitation for 2 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 135 microns, with an average of about 40 microns.
The content was then heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for 5 hours to complete the free radical polymerization.
EXAMPLE 6
60 parts of isodecyl methacrylate and 0.12 parts of benzoyl peroxide were mixed with 5.65 parts of Desmodur N-100. The resultant mixture was emulsified into 110 parts of a 1% Vinol 523 solution in a Waring blender. To this emulsion, 20 parts of an aqueous solution containing 1.02 parts of diethylenetriamine was added. The mixture was stirred at 60° C. under mild agitation for 2 hours to complete the microencapsulation reaction. Particle size varied from about 5 to about 145 microns, with an average of about 40 microns.
The content was then heated to about 85° C., when a reaction exotherm was observed. After the reaction exotherm, the mixture was further heated to 90° C. for 5 hours to complete the free radical polymerization.
Each of the microcapsule compositions in Examples 1-6 was coated onto a 24# bond paper substrate, at a coating weight of about 5 g/m2 and dried in a heated oven at 90° C. for 1 minute. The coatings were completely non-tacky, yet under some shearing pressure, the tacky properties of the adhesive were obtained.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and the practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only with a true scope and spirit of the invention being indicated by the following claims. | A microencapsulated adhesive and a method for producing that microencapsulated adhesive is disclosed. The adhesive is produced from an alkyl acrylate or methacrylate monomer having about 4 to about 12 carbon atoms, or a mixture thereof. The monomer is encapsulated by interfacial polymerization, gelatin/gum arabic coacervation or melamine/formaldehyde encapsulation. The microcapsules may be polyamide or polyurea. The monomer is polymerized in the microcapsules by heating to form an adhesive that is non-tacky, but becomes tacky upon application of external forces, such as shearing. The microencapsulated adhesive composition may be used, among other applications, as an adhesive for stamps or envelopes. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to industrial presence sensor systems and, more specifically, to cable motion detection systems.
2. Related Art
High volume manufacturing processes move large numbers of production units through manufacturing lines. One example of such a process is baked goods. High numbers of loaves of bread are processed in a manufacturing plant. These loaves are transported by conveyor belt from operation to operation. During transportation, for various reasons such as jamming an error will occur and the loaves will fall off the conveyor belt. Alternatively, empty bread pans may jam. Empty bread pans are cooled off on long conveyors before coming back to be reused. When these bread pans jam, the bread pans become damaged from falling off the conveyor or from hitting each other and must be replaced. Alternatively, the pans jam machinery (equipment), damaging the equipment such that it must be repaired or replaced. If the problem is not corrected quickly, or if the manufacturing line is not stopped quickly, a great number of loaves of bread and/or bread pans will fall on the floor or jam equipment. These loaves and damaged bread pans must then be discarded, while the equipment can require repair or replacement. This results in higher manufacturing costs.
Because these lost bread pans are considered pure waste and because a very large number of bread pans (and loaves) can be lost, it is critical that any falling bread pans be identified as quickly as possible. Accordingly, one means of identifying conditions when bread pans are falling is to add alarms at trouble points, instruct the existing employees to watch for the alarms in addition to their regular duties. However, any losses from the failure to recognize alarms are simply absorbed. Thus, it is a forgone conclusion that a loss will occur, and the major challenge is managing the extent of the loss.
Though the above example relates to the bakery process, the illustrated problem is common to many high volume manufacturing processes.
Accordingly, there is a need in the art to provide a system which will enable an automatic means for monitoring the status of the material involved in the manufacturing processes.
An optical emitter/detector pair system produces a long beam that is interrupted whenever an object moves between the emitter and the detector. These systems are difficult to align and keep aligned. In addition, once in place, the beams are not visually apparent and thus individuals who are moving may walk between the emitter and detector, setting off false alarms. Further, optical sensors have difficulty with wet, dusty, hot, corrosive or otherwise extreme conditions. An area of particular difficulty for optical sensors is transparent targets, many of which cannot be reliably detected using common light sources. Moreover, because optical sensors are practically limited to line-of-sight beams, an array of detectors and emitters must be utilized if it is desired to detect an object crossing anywhere through a plane in space. Theoretically, mirrors may be used to expand the area of coverage, but alignment, signal strength, environmental factors, and maintenance issues make the use of mirrors less attractive.
In certain instances, information regarding the status of the manufacturing process may be determined by obtaining information on the speed of the conveyor belt. If the conveyor belt is jammed, the speed may be zero, and a problem arises. U.S. Pat. No. 3,743,913 issued to Rebucci discloses a mechanism for electrically transmitting the speed of a conveyor belt. However, if a problem such a jamming occurs which may cause manufactured articles to fall off the conveyor belt the belt speed is not affected, and no information is developed. Vehicle speed detectors which provide an alarm for excessive speed generally are of course well known in the art, as in U.S. Pat. Nos. 3,648,267, and 3,859,629.
U.S. Pat. No. 3,838,341 issued to Gaines discloses a detection system for determining unacceptable deviations from a desired spacing pattern in the passage of articles past a station. This solution is limited to checking the status at only one point. If multiple points are needed, multiple devices are required. Also, an entire area cannot be checked, given the constraint that only the status of a particular point can be checked. In addition, the existence of a desired spacing pattern is a prerequisite of such a detection system, while such a spacing pattern in fact does not exist for many production lines.
Wire-type sensors and detectors for determining the presence of various articles are also known. For example, U.S. Pat. No. 4,367,459 discloses a taut wire intrusion detection system in which an actuator is connected to a group of tensioned wires. A force transducer outputs an electrical signal proportional to the force applied to the actuator; when the force exceeds a predetermined threshold, an alarm is activated.
In another example, U.S. Pat. No. 4,736,194 discloses a fence with security wires fastened to posts via sensors. An alarm signal is generated when only one or only a few security wires move slowly. However, these slow movements are ignored when caused by environmental factors such as changes in temperatures and wind forces because the signal amplitudes of the sensors are drawn up to a mean value and only threshold deviations from the mean value create an alarm situation. One mode compares the tension of one wire with the average tension of a group of wires to ignore slow noise sources. Another mode compares the time rate of change of wire tension to a threshold value. This reference does not teach or suggest the use of time rate of change of position.
In yet another example, U.S. Pat. No. 4,929,926 discloses an intrusion detection barrier utilizing a coiled wire fence and a sensor wire tensioned between a pair of ground wires. The sensor wire, which is connected to an intrusion detector, is free to move along its longitudinal axis, but is not free to move transversely. The intrusion detector may be of the force sensing type or of the pull switch type.
Similarly, U.S. Pat. No. 5,371,488 discloses a tension sensing security apparatus which senses variation in the longitudinal tension in taut wire and produces a tension signal which is transmitted to a central monitoring location. While in the general area of cable tension transducers, none of these references teach or suggest applications of the technology to the area of high volume manufacturing processes. The general class of cable pull switches (an industrial product often used to trigger manual safety alarms) suffer from significant limitations: they are not very sensitive; they are limited in cable length to around 100 feet; they do not move out of the way of an object; and they can be deactivated by mechanical failures.
U.S. Pat. No. 5,236,144 discloses a cable extension linear position transducer which has an integrated support structure, a potentiometer having a shaft, a drum affixed to the shaft and a tension spring. This type of transducer has been used in conjunction with industrial limit alarms to signal when an absolute limit has been reached. However, these applications rely on the inherent accuracy and repeatability of these precision instruments, and do not adaptively filter out the noise sources that more strongly affect longer, lower stiffness cables or lines. Precise measurement of the linear movement of an item is provided by this invention, but no other applications of this technology in other arts are either taught or suggested.
U.S. Pat. No. 3,882,474 discloses a system for monitoring the instantaneous velocity of a pipe string being tripped relative to a well bore. Specifically, the invention discloses a unit which derives an electrical signal as a function of instantaneous pipe speed, and a monitoring system which compares signals representative of instantaneous velocities and provides an alarm when predetermined velocity limits are exceeded. There is no automatic adaptation to changing conditions disclosed or suggested by this reference.
U.S. Pat. No. 4,128,888 discloses a velocity control system for an oil drilling rig which gathers information on certain indices and compares that information against certain predetermined threshold values. If certain values are exceeded, output signals or alarm signals are generated. The information gathered is of actual velocity and direction of travel, and the predetermined thresholds relate to minimum and maximum velocities, and direction of travel. Output signals are generated when the actual velocity is not within the minimum and maximum thresholds, or when the direction of travel deviates from the predetermined direction of travel.
SUMMARY OF THE INVENTION
It is in the view of the above problems that the present invention was developed. The invention is a system for monitoring cable motion that includes a cable-encoder combination to create an electrical signal indicating distance and a microprocessor monitoring system to provide time measurement in conjunction with distance information and to provide alarms whenever predetermined limits are exceeded. The system provides a teaching mode for teaching the predetermined limits, and provides a velocity-adaptive mode in which certain informational values may be adjusted over fixed time periods to provide for moving references. In the teaching mode, the microprocessor software learns a limit for that position value from an example the user gives it by moving the sensing line. In run mode, the microcontroller reads the encoder and keeps a current position output value after subtracting off any motions that occur below a user-specified speed. If this value exceeds the taught position value limit, an alarm is produced. Accordingly, slow length changes are rejected.
More specifically, the invention is a velocity-discriminating and position threshold cable transducer system which has a tensioned cable in contact with a spool. When the cable is moved, the spool is rotated. The spool communicates with a digital encoder. The encoder reads the distance traveled and communicates the information to a microprocessor.
In this invention, a position threshold may appear to be a moving value over time. A new relative value for the position threshold is obtained by subtracting up to one position unit from any displacement occurring within a selected time interval. Accordingly, the system can be very sensitive to the amount of motion produced by a slight lateral displacement of the sensing line because it rejects the kind of slow length changes in the sensing line that would require wide limits to be set if one were using pure displacement sensing. Slow length changes could be a result of many factors, including temperature expansion/contraction cycles, humidity shrink/stretch cycles, aging stretch, settling & temperature effects of the building and equipment to which the sensing line is mounted, weakening of springs used to keep sensing line tension, etc. In addition, the system of the present invention is advantageous in that it provides the ability to reject the presence of slow motion in either objects or mounting points for the sensing line.
Velocity is calculated by knowing the amount of time elapsed between two different cable positions. The low velocity rejection feature is implemented by subtracting up to one position unit from any motion that happens within a selected time interval. This produces a new virtual or relative output of the encoder/potentiometer that has any motion below the selected amount already subtracted off. This derived virtual output is basically in the form of a set of positions over time, just like the original outputs. Accordingly, anything that could be done to the original outputs can be done to this derived output. That is why a threshold for the alarm can be set for a position value, as in the preferred invention, or a velocity, as in the less preferred invention. Velocity can be calculated from this derived output as change in position over a time interval.
In another embodiment, the microprocessor determines the velocity and compares it against a preset velocity threshold. If the velocity threshold is exceeded, an output is generated in the form of an alarm signal.
In yet another embodiment, the system utilizes a constant velocity timer wheel connected to the cable such that one of two square wave edges is generated by the encoder periodically, and that creates an alarm signal output in the absence of square wave changes.
The system further comprises seven separate modes: an initialization module, a mode configuration module, a limit-learner module, a sensor reader module, a slow motion rejector module, a limit checker module, a health monitor module, and an alarm driver module. The limit-learner module implements a teaching mode in which the cable is displaced by a user to the minimum distance that detection is desired; the system will read the value and set it to the new position threshold.
A wide variety of materials can be selected for the sensing line to allow the sensor system to work in hot, corrosive, underwater, or other difficult environments. The line can then simply be run out of that environment using a mechanical coupling, to attach to the line position transducer component of the present invention. Moreover, dusty, wet environments and transparent target objects can be easily tolerated by the system of the present invention.
Further features and advantages of the present invention, as well as the structure and operation of various embodiments of the present invention, are described below in detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated in and form a part of the specification, illustrate the embodiments of the present invention and together with the description, serve to explain the principles of the invention. In the drawings:
FIG. 1 illustrates a multiple embodiment of a velocity-discriminating cable transducer system of the present invention which utilizes sacrificial link variants, netting variants, guide bushing variants, and stationary object variants;
FIG. 2 illustrates a side plan and partial cutaway view of an alternate embodiment of the encoder and spool shown in FIG. 1 of the present invention;
FIG. 3 illustrates a side plan and partial cutaway view of yet another alternate embodiment utilizing an encoder and spring reel combination with a flexible coupling;
FIG. 4 illustrates a slide potentiometer embodiment of a velocity-discriminating cable transducer system;
FIG. 5 illustrates an alternate cable attachment embodiment of the present invention;
FIG. 6a illustrates a side plan view of a gearmotor timer embodiment of the present invention;
FIG. 6b illustrates a front plan view of the gearmotor timer embodiment of FIG. 6a;
FIG. 7 illustrates a block diagram view of the functions performed by the microprocessor of the present invention;
FIG. 8 illustrates a software flow chart for an initialization module and portion of a mode configuration module for the microprocessor of the present invention;
FIG. 9 illustrates a software flow chart for the remainder of the mode configuration module and a portion of a limit learner module for the microprocessor of the present invention;
FIG. 10 illustrates a software flow chart for the remainder of the limit learner module, a sensor reader module, and a slow motion rejecter module for the microprocessor of the present invention;
FIG. 11 illustrates a software flow chart for a limit checker module, and a portion of a health monitor module of the present invention;
FIG. 12 illustrates a software flow chart for the remainder of the health monitor module and an alarm driver module for the microprocessor of the present invention; and
FIG. 13 illustrates an electrical schematic of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the accompanying drawings in which like reference numbers indicate like elements, FIG. 1 shows a multiple embodiment of a velocity-discriminating cable transducer system, shown generally at 10, of the present invention which utilizes sacrificial link variants, netting variants, guide bushing variants and stationary object variants. In particular, system 10 includes sensing cable 12 wrapped at first end, shown generally at 14, about first spring reel 16 and wrapped at second end, shown generally at 18, about second spring reel 20. First, second, third and fourth guide pins, 22-28 respectively, of first spring reel 16 are disposed in close proximity to spool 30 to prevent sensor cable 12 from disengaging laterally from spring reel 16.
Between first spring reel 16 and second spring reel 20, sensing cable 12 is wound around spool 30. First, second, third and fourth spool guide pins, 32-38 respectively, are disposed in close proximity to first spring reel 16 again to prevent sensor cable 12 from disengaging laterally. Spool 30 and shaft 40 rotate about a common axis. Shaft 40 is connected to encoder assembly shown generally at 42 which comprises encoder 44 having flange 46 equipped with mounting holes 48-52. Encoder assembly 42 is firmly anchored to its surrounding.
Thus, first spring reel 16 tensions sensing cable 12 with a few pounds of constant tension. Sensing cable 12 then wraps around spool 30 to rotate encoder 44. Sensing cable 12 continues through a series of elements until it is anchored by a second spring reel 20.
Referring again to FIG. 1, sensor cable 12 is also in contact with first pulley 54. First pulley 54 is preferably a ball bearing pulley anchored firmly to its surroundings. Sensor cable 12 has a first cable portion 13 connected to one end of sacrificial link shown generally at 56 and a second cable portion 15 connected to the other end of sacrificial link 56. Sensor cable 12 is preferably a low stiffness, low stretch material such as fine steel cable, nylon sheathed bronze cable, or nylon sheathed Kevlar cord. Sacrificial link 56 may be a fishing leader, a bent piece of wire, or any other material which is set to release or fail at a force a few pounds higher than that normally produced by either of the two spring reels, 16 and 20.
Second cable portion 15 then extends through net 58 suspended at four corners, first guide bushing 62, second pulley 64, second guide bushing 66, third guide bushing 68, and wraps around second spring reel 20.
One of many possible configurations is shown, where the sensing line passes near the center of the net, weaving under one web of the net to couple to the center of the net. It also passes through a hole in the net one time near where the sensing line first encounters net, and once near where the line later encounters the net. This is accomplished by installing sensing line so that it passes though the near and far edges of the net without touching the net, or as close to this as possible; then unthreading one side of the sensing line from the net, threading it under one net web near the net center, and rethreading the sensing line through the original far hole. This places as little of the weight of the net as possible on the sensing line, keeping the friction loading effects on the sensing line to a minimum.
Guide bushings, 62, 66 and 68, which are firmly anchored to their surroundings (i.e. mounted to rigid mounting posts) are preferably coated with a low friction material such as Teflon or nylon, or are made from polished metal. Guide bushing 62, 66 and 68 serve to support sensing cable 12 for a long, nearly straight run while amplifying the pulling effect of any object contacting the sensing line laterally.
First stationary object 72 is tethered to sensor cable 12 via first tether 74 and first connector 76 that is preferably a slidable ring connector. Similarly, second stationary object 78 is tethered to sensor cable 12 via second tether 80 and second connector 82.
In operation, a section of sensor cable 12, as in middle section 90, is placed adjacent a high-volume manufacturing process, preferably next to or under a conveyor belt (not shown). Middle section 90 spans the area occupied by net 58 and the area occupied by net 58 is preferably wider than the conveyor belt. When product (not shown) falls from a conveyor belt, it is caught by net 58. The momentum of the product encountering net 58 shakes net 58 and causes displacement of sensor cable 12.
However, sensor cable 12 is constrained to move in a generally linear fashion as constrained by first, second, and third bushings, 62, 66, 68, respectively, and by first and second pulleys 54 and 64 respectively. As sensor cable 12 moves linearly, spool 30 rotates because sensor cable 12 is wrapped about spool 30. As a result, shaft 40 also rotates, providing an input to encoder 44. As a result of the input, encoder 44 produces an output which is communicated to the microprocessor 100, shown generally in FIG. 7.
In a stationary object embodiment, here combined with the guide bushing embodiment, of FIG. 1, stationary objects 72, 78, and 84 respectively are monitored. Specifically, if stationary objects 72, 78, and 84 fall or are moved any appreciable distance, first, second and third tethers, 74, 80, and 86 respectively, will move sensor cable 12, and linear movement of sensor cable 12 will result in an output from encoder 44. Thus, there should be a minimum of tension on tethers 74, 80 and 86 to minimize the friction loading on sensing cable 12.
Second spring reel 20 and first spring reel 16 are provided with a sensing cable 12 having a total wraparound length greater than the maximum sensing cable 12 length change caused by the worst case object motion for the particular installation. However, it is noted that second spring reel 20 may not be needed if first spring reel 16 has enough length of sensing cable 12 wrapped therearound. Second spring reel 20 has a cable tension at least a few pounds above the value of the tension that first spring reel 16 can provide so that second spring reel 20 will not unwind unless first spring reel 16 has completely unwound.
Accordingly, encoder assembly 42 provides input to a circuit board with a microcontroller 100 on it that uses the motion of encoder 44 to determine when to drive lamps, buzzers, and/or relays based on algorithms in the program of the microcontroller.
FIG. 2 illustrates a side plan and partial cutaway view of an alternate embodiment of the encoder 44 and spool 30 shown in FIG. 1. The use and configuration of encoders 44 and spools 30 are well known in the art, and vary widely. Sensor cable 12 is shown wrapped around spool 30 in the same manner as in FIG. 1. Encoder 44 is bolted to a foundation 92 just as contemplated, but not shown, in FIG. 1. Foundation 92 may be an insulating material for providing insulation from liquids, gases, chemicals, or temperature differences. In FIG. 2, an environmental seal 94 is provided between spool 30 and foundation 92. Thus, FIG. 2 represents an alternate embodiment in which the invention may be utilized in harsh environments. By use of environmental seal 94, the encoder 44 and microprocessor 100 shown in FIG. 7 may be separated from the harsh environment in which spool 30 and cable 12 operate. The harsh environment may be a highly humid area, a liquid immersion, a chemically active environment, a highly hot or cold area, or the like. As in FIG. 1, the embodiment of FIG. 2 still provides an output (not shown) from encoder 44 which is communicated to microprocessor 100.
FIG. 3 illustrates a side plan and partial cutaway view of yet another alternate embodiment. In this embodiment, no spool is required. Instead, first spring reel 16 is provided with a first spring reel cap 102 and a flexible coupling 104 is attached at one end to spring reel cap 102. The other end of flexible coupling 104 is attached to encoder assembly 42. As in FIG. 1, the embodiment of FIG. 3 still provides an output (not shown) from encoder 44 which is communicated to microprocessor 100.
FIG. 4 illustrates a side plan view of a slide potentiometer embodiment of a velocity-discriminating cable transducer system. It should be noted that both the encoder approach of FIG. 1 and the slide potentiometer approach of FIG. 5 are based upon reading the cable position often. While the embodiment of FIG. 1 utilizes first spring reel 16 and second spring reel 20 as tension devices, a weight 108 may be alternately used as a tension device to provide tension in sensor cable 12.
Velocity is calculated by knowing the amount of time elapsed between two different cable positions. The low velocity rejection feature is implemented by subtracting up to one position unit from any motion that happens within a selected time interval. This produces a new virtual or relative output of the encoder/potentiometer (relative to a floating reference position) that has any motion (such as low velocity motion) below the selected amount already subtracted off. This new output is basically in the form of a set of positions over time, just like the original outputs. Accordingly, anything that could be done to the original outputs can be done to this. That is why a threshold for the alarm can be set for a position value, as in the preferred invention, or a velocity, as in the less preferred invention.
There are many ways to characterize a sequence of position values in time. A minimal definition of a motion requires that there be some change in position that occurs over an interval of time. Quantifying this motion with a motion value can be done by looking only at two or three position values at certain times, calculating instantaneous velocity or acceleration quantities, and then defining a motion value as the magnitude of these quantities. Alternatively, a graph of position against time can be treated as a waveform that can have circuit-type filtering function applied to it. Alternatively, a graph of position against time can form the basis for a two-dimensional image that can have machine-vision-type structuring elements applied to it. In the graphing cases, the modified graph would be input to an evaluation function that extracts a single number quantifying a motion value based on concepts such as fixed-width time windows, integration, or age-weighted averages. Accordingly, it would be accurate to describe, in a generic sense, the microprocessor 100 as calculating a motion value from an encoder 44 signal and that this motion value may be compared against a limit to change a binary output when the limit is exceeded.
There are various reasons why a position threshold is preferred over a velocity threshold in a high-volume manufacturing environment. For example, conveyor belts in high-volume manufacturing environments can move slowly or rapidly. This range of velocity makes a velocity threshold difficult to select. In contrast, selecting a cable deflection position for the alarm threshold is much less difficult. In addition, a velocity threshold could be very sensitive to small fast moves, such a vibration, creating more highly undesirable false alarms.
FIG. 5 illustrates a friction clip used to attach slide 109 of the slide potentiometer 110 embodiment of a velocity-discriminating cable transducer system to cable 12. Screw 112 is used to hold clip 111 to potentiometer slide 109. Screw 106 is used to adjust the amount of friction between clip 111 and cable 12.
In the first embodiment, spool 30 and encoder assembly 42 (including encoder 44) operate together to form a linear displacement sensing device. Thus, there is illustrated in FIGS. 4 and 5 an alternate linear displacement sensing device in the form of slide potentiometer 110 and friction clip 111.
FIG. 6a illustrates a side plan view of a gearmotor timer embodiment of the present invention and FIG. 6b illustrates a front plan view of the gearmotor timer embodiment of FIG. 6a. Gearmotor timer 113 is a repetitive motion device and preferably utilizes a 1 RPM timer wheel which can keep the encoder in continuous motion. In other words, gearmotor timer 113 applies a repetitive motion to sensing cable 12. As a result of the 1 RPM timer wheel, sensing cable 12 is in continuous motion and results in one of two square wave edges generated by encoder 44 approximately every 10 seconds. Encoder 44 is for example manufactured by Oak Grigsby 90Q128-00-00, and produces two square waves, WF1 (waveform 1) and WF2 (waveform 2), in quadrature to each other. As the encoder wheel (not shown) connected to encoder shaft 40 is rotated, two sensors in encoder 44 pick up the light (or transparent) and dark stripes that radiate from the center of the encoder wheel as high and low voltages, creating the two square wave signals that correspond directly to motion of encoder shaft 40. These signals are connected directly to the input of microcontroller 100 (the term "microprocessor" and "microcontroller" are synonymous and are used interchangeably). These quadrature signals are directly read by the program in microcontroller 100. The term "quadrature" refers to the four combinations of black-black, black-light, light-light, and light-black that may be sensed by encoder sensors. These four combinations enable direction of rotation to be determined. This program uses the quadrature signals to calculate the current position of sensing cable 12, then computes a virtual position after all motion below a selectable threshold is subtracted out. The program also compares this virtual position with a threshold to determine when to set outputs to LED's, a buzzer, and a relay. Two manual push-buttons are also read to allow the user to select the program's mode of operation.
The control program comprises eight modules that reside in the Read Only Memory of microcontroller 100. Preferably, microcontroller 100 is a Microchip Technologies PIC16F84. The program runs in an infinite loop, continuously calling the various program modules one after the other at a high rate of speed. Each program module may look at a timer value and determine not to run that time, or it can run for a very short time, less than 300 microseconds, before returning control to the infinite loop. At the beginning of the infinite loop, all program module variable are set to initial values to appear to the other program modules that the system has already been running smoothly.
Microprocessor 100 starts a timer that is reset whenever the square wave changes, but that times out after a predetermined value of no square wave changes. Preferably, the predetermined value is 10 seconds of no square wave changes. This allows an alarm to be sounded to indicate that the system is not operating reliably, yielding a system that is more reliable than the simple cable pull switch trip wire approach often used which can be deactivated by mechanical failures.
FIG. 7 illustrates a block diagram view of the eight software modules and their interactions provided within microprocessor 100 of the present invention. The modules are shown on circuit board 114. The software modules include initialization module 116, mode configurator module 118, limit learner module 120, a sensor reader module 122, a slow motion rejector module 124, a limit checker module 126, a health monitor module 128, and an alarm driver module 130. Outputs from the board include lamp 132, buzzer 134, and relay 136. It is contemplated that system 10 is a stand alone system. Thus, sensory outputs 132 and 134 are important. However, relay 136 may be used to provide an input to a network or network controller (not shown) to provide further coordination within the manufacturing area and to provide information to management information systems.
FIGS. 8-12 illustrate a software flow chart for initialization module 116, mode configurator module 118, limit learner module 120, sensor reader module 122, slow motion rejector module 124, limit checker module 126, health monitor module 128, and alarm driver module 130 for microprocessor 100 of the present invention.
As shown in FIG. 8, initialization module 116 is run only once when the power is initially turned on. The purpose of initialization module 116 is to set the value of various variables. Normally, selected variables are set to initial values. However, if the power had previously failed, certain key variables are assigned values from flash RAM with the remaining selected variable set to initial values.
Mode configuration module 118 shown in FIGS. 8-9 is run approximately 50 times per second. This module checks or polls for operator input at either push-button, ENABLE or TEACH. If ENABLE is detected as pushed, the variable ENABLED is toggled between TRUE and FALSE. The TEACH push-button is only checked if ENABLED is TRUE. If the TEACH push-button is pushed, then the LEARNING variable is set to TRUE, and a timeout timer for learning is started (LEARNING TIMER). When LEARNING TIMER has timed out in 1 to 5 minutes, LEARNING is set to FALSE and normal sensing operation resumes. If the ENABLE push-button is detected while LEARNING is TRUE, then the next of three decreasing precalculated constants is loaded in the variable SPEEDTHRESHOLD. If more than two button pushes are detected, the first constant is reloaded, and the selection process continues with decreasing values, as before. The three constants are chosen for a particular type of application, and can be customized for different specialized application. A generic model with constants around 4000 milliseconds, 400 milliseconds, and 4 milliseconds would cover most applications.
As shown in FIGS. 9-10, limit learner module 120 is run approximately 20 times per second. This module examines the LEARNING variable set by mode configurator module 118. The first run that the LEARNING variable becomes TRUE, POSNTHRESHOLD is set to the minimum allowable (most sensitive) position threshold value. From then on while the LEARNING variable is true, limit learner module 120 computes a variable NEWTHRESHOLD=absolute value of (CABLEPOSN-NOMINALPOSN). Slow motion rejector module 124 is also off during this period to avoid interference with the calibration. If this value is greater than POSNTHRESHOLD, then it sets POSNTHRESHOLD=NEWTHRESHOLD. The LEARNING value is typically true for 1 to 5 minutes, long enough to let the operator manipulate the sensing line to the least displaced position at which he wants an alarm to be declared. The farthest travel of sensing cable 12 will thus become the newly taught POSNTHRESHOLD value.
As shown in FIG. 10, sensor reader module 122 runs every time through the loop and reads the two quadrature square waves from encoder 44. It compares two binary inputs with the last two read and does nothing if the values have not changed. If the values have changed, the module updates the CABLEPOSN variable depending upon the direction of motion. Thus, the module 122 determines a motion value upon displacement of sensor cable 12.
Slow motion rejector module 124 shown in FIG. 10, runs once every SPEEDTHRESHOLD milliseconds. This time can be many seconds for a sensing cable 12 with very slowly changing length. Its operation is simple: if CABLEPOSN is greater than the initial value (NOMINALPOSN), then subtract 1 from CABLEPOSN; if CABLEPOSN is less than NOMINALPOSN, then add 1 to CABLEPOSN. This module 124 is always trying to drive CABLEPOSN to the value of NOMINALPOSN. Thus, the motion value is a linear displacement value (position value) having a virtual position output calculated relative to a floating reference position by subtracting off the effects of low velocity motion from an absolute cable position value.
As shown in FIG. 11, limit checker module 126 runs in each program loop. If the absolute value of (CABLEPOSN-NOMINALPOSN) is greater than POSNTHRESHOLD, then the module sets LIMITEXCEEDED=TRUE; otherwise, LIMITEXCEEDED is not changed. LIMITEXCEEDED may latch to a true state here, causing an alarm to sound until being cleared when the enable button is pushed. POSNTHRESHOLD is the length of change in sensing cable 12 permitted before an alarm is declared. Thus, a binary output signal is changed when the motion value (here a position value) exceeds the limit.
As shown in FIGS. 11-12, health monitor module 128 reads the Power Fail signal input, and sets the POWERFAIL variable equal to this level. When POWERFAIL becomes TRUE, key variables are saved to nonvolatile memory to be retrieved by the initialization module 116 when power returns. It also turns on the Green LED every 1/6 seconds and turns it back off 1/6 seconds later. This gives a visible "heartbeat" indication that the software is operating properly and the system is not in the DISABLED mode. Whenever the LEARNING variable is set, the green LED is left on. It is noted that an embodiment utilizing gearmotor timer is contemplated. For this embodiment, an additional feature may be provided in health monitor module 128. The module 128 checks the raw encoder input if the MAXIMUM RELIABILITY flag is configure to true. In this case, if the encoder signal does not a transition indicating motion for approximately 10 seconds, it sets the MOTIONSTOPPED variable to cause an alarm.
Alarm driver module 130 shown in FIG. 12 preferably is run approximately 1000 times per second. This module 130 looks to see whether the LIMITEXCEEDED or MOTIONSTOPPED variables are TRUE; if so, the relay and beeper outputs are asserted, and the red LED output is also asserted. A timer is started (FLASHING TIMER) for a period of about 1/6 seconds, and at the end of that time, the red LED output is toggled. This continues every 1/6 seconds while LIMITEXCEEDED is TRUE. When LIMITEXCEEDED and MOTIONSTOPPED are FALSE, the red LED output is cleared.
FIG. 13 illustrates an electrical schematic of the present invention. The watchdog timer circuit is built around two of the op amps, and drives the buzzer output. The flow chart requires that the software toggles that output at a high rate of speed to keep the buzzer from sounding. This function is to support high reliability applications that probably would also use the 1-rpm motor on the end of the sense line to reduce the risk of undetected failure. The watchdog timer allows any fatal fault in the microprocessor hardware or software to be quickly signaled, before the system has time to miss sensing an important event. This is in keeping with the general principle in automation that safety-related functions are hard-wired, and do not depend on software.
An interesting result of combining a velocity-rejecting module with a position threshold is that the reference location from which the position threshold is judged moves with respect to the absolute position of the cable at the encoder.
Operation of the System
Sensing cable 12 is installed in an area where the user wants object motion detected when an object crosses a straight line such as where sensing cable 12 is threaded through guide bushings (e.g. guide bushing 62, 66 and 68), and/or when an object crosses a plane such as where sensing cable 12 is threaded through net 58, and/or when an object moves away from sensing cable 12 such as when tether 74, which is attached to stationary object 72, is connected to a ring or connector 76 that sensing cable 12 runs through. After all the components of system 10 are physically in place, the user presses the LEARN push-button that places the system into a special learning mode signified by the constant illumination of the green LED and the absence of its usual heartbeat flashing. During the several minutes that the system is in this mode, the user identifies an important section of sensing cable 12 such as the location where finest motion is being monitored, or in the center of the longest unsupported run of cable 12, or some other user-specific location. The user then physically displaces cable 12 the minimum distance that detection is desired at that selected location. In other words, the user teaches the system the desired position threshold (alternatively referred to as a "limit") by physically displacing sensing cable 12 to the desired position threshold or limit. Limit learner module 120 will read the value of displacement and will store this value as the new position threshold if the new value is larger than the last motion during the learning mode. After exiting from the calibration mode via timeout or via the user pressing the LEARN push-button again, the system 10 will set the present cable position to the nominal value and begin looking for motion using the new parameters.
The result of movement of sensing cable 12 in any of the applications discussed above is that sensing cable 12 wound around spring reel is pulled and unwinds from spring reel under approximately constant force. The spring reel cable, being wrapped around the spool, causes the spool to rotate, which then causes encoder shaft 40 to rotate.
When encoder shaft 40 rotates, a quadrature signal is produced and read by sensor reader module 122 of microprocessor 100. The signal is converted into a change in the sensing line position variable (motion value). This is resisted by slow motion rejector module 124 which tries to drive the position variable back to its nominal value at a rate equivalent to the speed rejection threshold. If the motion is fast enough, the sensing line position variable will change. When limit checker module 120 sees this change, it compares it against the position threshold. If the position threshold or limit is exceeded, limit checker module 120 signals alarm driver module 130 to change the hardware outputs of the system. In this implementation, this includes flashing the red LED, supplying 12 volt power to sound the buzzer, and supplying 12 volt power to energize the relay coil. The hardware outputs continue to be asserted until manually silenced by the user pressing the enable button. Optionally, a timeout occurs after a period of minutes or hours. Either reset method causes the system to redefine the current sensing line position as the nominal value, and resume monitoring for motion using all the previous parameters.
In view of the foregoing, it will be seen that the several objects of the invention are achieved and other advantages are attained. The embodiments were chosen and described in order to best explain the principles of the invention and its practical application to thereby enable others skilled in the art to best utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated. As various modifications could be made in the constructions and methods herein described and illustrated without departing from the scope of the invention, 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. For example, the parameter output after velocity subtraction need not be position, but could be velocity or acceleration. Another modification falling within the scope of the present invention involves the amount of velocity subtracted. The amount of velocity subtracted could be learned, like the position threshold, from an example of line motion, and not simply selected. In another modification, a lower cost progressive force spring could replace the constant force spring reel. In yet another modification, nonvolatile memory could be used to allow the system to remember its setup through power failures or shutdowns. In addition, other types of computing engines could be used besides a microcontroller, such as a digital signal processor, a custom digital circuit, or a neural network chip. Rotary encoder 44 could be replaced by a rotary potentiometer or resolver. Linear potentiometer 110 could be replaced by a magnetostrictive or inductive coil type linear position sensor. A further modification could be that sensing cable 12 could be highly visible, larger diameter plastic sheathing a core of Kevlar, bronze, or steel; alternatively, its length could be maximized by using fine steel cable. Yet another modification is that the control buttons can be mounted remotely for user convenience when the transducer is not in an easily accessible place. A further modification is that encoder 44 may be integrated with spring reel 16. Another modification is using a repetitive motion device other than gearmotor timer 113 that provides a predictable repetitive motion. Thus, the breadth and scope of the present invention should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims appended hereto and their equivalents. | A system for monitoring motion includes a cable-encoder combination to create an electrical signal indicating distance and a microprocessor monitoring system to provide time measurement in conjunction with distance information and to provide alarms whenever predetermined limits are exceeded. The system provides a teaching mode for teaching the predetermined limits, and provides a velocity adaptive mode in which a certain informational values may be adjusted over fixed time periods to provide for moving references. | 6 |
FIELD OF THE INVENTION
The present invention is directed to tamper-evident closures. More specifically, the present invention is directed to such closures which include a frangible portion which fractures when the closure is removed from the container thereby evidencing the fact that the container has been opened. Still more particularly, the present invention is directed to such closures which are useful in connection with various containers, including soda bottles and other such containers which are maintained under significant pressures.
BACKGROUND OF THE INVENTION
Both plastic and metal closures for various bottles and containers which include a tamper-evident feature have been known for many years. In most cases, this tamper-evident feature comprises a lower shoulder or skirt portion of the closure which is in some way intended to fracture or break upon removal of the closure from the container, so that it then becomes evident that the container has been opened. While a large number of these closures have been known in the past, on a commercial basis, and particularly in connection with soda bottles and other such containers maintained under significant pressures, up until quite recently metal closures have predominated. These include closures such as those shown in U.S. Pat. No. 3,812,991 which issued on May 28, 1974 to the Coca Cola Company, and many others.
The many problems encountered in connection with the use of metal closures however, have been significant. They primarily relate to the fact that in an unacceptably large proportion of cases, removal of the closure does not result in a clean and efficient fracture of the lower skirt portion, therefore making removal of the closure quite difficult and/or eliminating the tamper-evident feature completely. In addition, the cost of metal closures has recently increased dramatically, and the search for efficient plastic closures has therefore intensified.
In connection with plastic closures of this type, again a large number have been known in the past, but no commercial closure has been found which can be applied in a single step to the container or bottle, (i.e., they generally require a two-step application procedure), and can at the same time result in efficient breaking or fracturing upon its removal. One recent commercial closure which is now widely utilized is that of U.S. Pat. No. 4,033,472 to Albert Obrist AG, which issued on July 5, 1977. This closure, however, again suffers from both of these infirmities. In the first place, it requires a two-step application procedure, i.e., initial application of the closure to the bottle followed by a heating process whereby the lower depending bead 4 is deformed against the surface of the bead or collar on the bottle itself, as shown in FIG. 4 thereof. In addition, it has again been found that these closures, although used commercially, do not fracture properly in an unacceptable proportion of cases. Several other issued patents which include such two-step application procedures include U.S. Pat. No. 3,673,761 assigned to Ciba-Geigy AG, and U.S. Pat. No. 3,788,509 to Keeler, which includes a separate heating step for producing the weakened zones themselves.
Among those patents which do show a one-piece plastic closure, which does not require such a heat sealing step are those to Hamberger, namely U.S. Pat. Nos. 2,162,711 and 2,162,712. These patents, however, are directed to closures which include a weakened portion defined by corresponding grooves on the shoulder portion (see FIG. 1 thereof) of the depending skirt 23. In these closures fracture thus occurs in a vertical direction with respect to the closure, and tangentially with respect to the lugs 18 to which the skirt is attached. In addition, the skirt portion in this patent appears to be constructed so as to be thinner than the upper walls thereof. Additional such closures are also shown in the Schauer patents, namely U.S. Pat. Nos. 2,162,752 and 2,162,754. None of these patents thus teach the structure of a commercially acceptable product.
There are yet another group of patents directed to such closures which rely upon interlocking teeth or serrations in order to effect the fracture of the closure. For example, French Pat. No. 1,347,895 includes a ratchet or lug means on the breakaway skirt portion 2 thereof as well as on the bottle bead, and German Pat. No. 2,349,265 also includes lugs 16 which extend inwardly from depending skirt 13 to aid in fracturing at the point of weakness thereon. Reference in this regard is also made to U.S. Pat. Nos. 3,980,195, 3,924,769 and 4,126,240.
SUMMARY OF THE INVENTION
In accordance with the present invention, a one-piece tamper-evident closure has now been discovered which not only can be applied to containers in a one-step operation, but which also result in highly efficient fracturing of the depending lower skirt portion upon removal of the closure from a container. In particular, these tamper-evident closures comprise one-piece closure bodies including an end wall, an internally threaded upper portion, and a depending lower skirt portion. The depending lower skirt portion includes an inwardly projecting bead which is adapted to engage the annular collar portion of a container when the closure is completely threaded onto the container, and the depending lower skirt portion has a substantially uniform thickness throughout its entire area intended to engage that annular collar. These closures further include an area of weakness located above the depending lower skirt portion and designed to fracture in a substantially horizontal plane across the closure itself when the closure is unthreaded from the container, thereby leaving the depending lower skirt portion engaged to the annular collar of the container after the upper portion of the closure has been removed from that container.
In another embodiment of this closure, however, the depending lower skirt portion includes an outwardly extending shoulder portion having a substantially L-shaped outer surface, and the closure includes an area of weakness designed to fracture in a plane which does not pass through and is not tangential to the annular collar portion of the container when the closure is unthreaded therefrom.
In yet another embodiment of this closure, however, the depending lower skirt portion includes an inwardly projecting bead adapted to engage the lower end of the annular collar portion of the container when the closure is completely threaded onto the container, and the closure includes an area of weakness located above the inwardly projecting bead, and the entire portion of the depending lower skirt portion of the closure located below the area of weakness has a substantially uniform thickness.
In a preferred embodiment of the closures of the present invention, the area of weakness is formed by a circumferential groove formed on the outer surface of the closure, preferably a V-shaped groove, which can include a slot or a plurality of slots whereby at least a portion of the groove passes entirely through the closure, in effect forming a pre-cut area of weakness.
In another preferred embodiment of the present invention, the inwardly projecting bead at the end of the depending lower skirt portion includes a gradually tapered lower surface to assist in effecting the gradual outward bending of the skirt when the closure is initially threaded onto the container without fracturing the closure at the area of weakness, and a substantially planar upper portion for engagement with the annular collar portion of the container when the closure is completely threaded onto the container, so that the skirt portion cannot gradually bend outward when the closure is unthreaded from the container thereby causing fracture to occur at the area of weakness.
In yet another embodiment of the present invention, the outer surface of the internally threaded upper portion of the closure includes a plurality of vertical serrations, which preferably terminate a predetermined distance above the area of weakness discussed above.
In a preferred embodiment of the present invention, the closure includes sealing means located on the inner face of the end wall so as to form a seal between the closure and the container when the closure is completely threaded onto the container. In one embodiment, the sealing means comprises a yieldable sealing disc maintained against the inner face of the end wall. In another such embodiment, however, the sealing means comprises a ridge or ridges projecting from the inner face of the end wall at a location corresponding to the position where the neck portion of the container is intended to contact the end wall when the closure is completely threaded onto the container. Preferably these ridge means thus comprise a number of concentric annular projections or ridges, and preferably three such ridges, which most preferably have a substantially V-shaped configuration.
In another embodiment of the sealing means of the present invention, the end wall of the closure includes an annular sealing membrane corresponding with the intended location of the neck portion of the container and having a thickness substantially less than that of the remainder of the end wall so that the sealing membrane is substantially more flexible than the remainder of the end wall, and can therefore conform to the shape of the neck portion of the container when the closure is completely threaded onto the container. Preferably, hinge means are located on the inner and outer annular surfaces of the sealing membrane in order to increase the flexibility of the membrane, and these hinge means will preferably be annular V-shaped grooves located on the inner face of the end wall at the inner and outer annular surfaces of the sealing membrane.
In another embodiment of the sealing means of the present invention, an annular sealing ring is provided projecting from the inner face of the end wall at a location directly adjacent to the intended location of the inner surface of the neck portion of the container upon closure, and preferably including an outwardly projecting annular bead for engagement with the inner surface of the neck portion of the container.
BRIEF DESCRIPTION OF THE DRAWINGS
The tamper-evident closure of the present invention can be further understood with reference to the drawings herein wherein:
FIG. 1 is a side, elevational view of two embodiments of a tamper-evident closure of the present invention;
FIG. 2 is a top elevational view of the tamper-evident device of FIG. 1;
FIG. 3 is a side, elevational, cross-sectional view of a tamper-evident closure of the present invention completely threaed onto a container;
FIG. 4 is a side elevational, cross-sectional view of the circled portion of FIG. 3;
FIG. 5 is a side elevational, cross-sectional view of another tamper-evident closure of the present invention completely threaded onto a container;
FIG. 5a is a side, elevational, cross-sectional view of another tamper-evident closure of the present invention completely threaded onto a container;
FIG. 6 is a side, elevational, cross-sectional view of another tamper-evident closure of the present invention completely threaded onto a container;
FIG. 7 is a side, elevational, cross-sectional view of another tamper-evident closure of the present invention completely threaded onto a container;
FIG. 8 is a side, elevational, cross-sectional view of another tamper-evident closure of the present invention completely threaded onto a container; and
FIG. 9 is an exploded, cross-sectional view of the circled section of the tamper-evident closure of FIG. 8.
DETAILED DESCRIPTION
Referring to the figures, in which like numerals refer to like portions thereof, FIG. 3 shows a tamper-evident closure 1 in accordance with this invention, preferably made of a thermoplastic material, completely threaded onto a bottle or container 3. The bottle itself includes a threaded neck portion 5 and an annular collar 7 therebelow. This annular collar 7 may in some cases be referred to as a transfer bead, since in the past it has been formed in connection with the manufacture of certain types of bottles (generally glass bottles) in order to assist in the transfer or movement of the bottle during its formation. On the other hand, annular collar 7 may also be referred to as a more pronounced elongated raised surface 25 of the container, such as is shown in FIG. 7. It is this collar 7 to which the present tamper-evident closure will be firmly engaged or affixed both before and after fracture of the tamper-evident portion of the closure, and furthermore which will assist in the fracturing process itself.
The closure 1 includes an upper end wall 9, and an internally threaded upper portion 11, which of course corresponds to the threaded neck portion 5 of the container to which is to be applied. The portion of closure 1 which is affixed to the collar of bead 7 when the closure is completely threaded onto the container 3 includes a depending lower skirt portion 12. As shown in FIGS. 1 and 3, this depending lower skirt portion 12 has a substantially L-shaped outer surface, including an upper horizontal shoulder surface 14 and a depending side wall surface 15. The inner surface of this depending side wall surface 15 includes an annular bead 16, which can best be seen in FIG. 4, and which itself includes an upper surface 18 and a lower surface 19. The lower surface 19 of bead 16 has a gradual inclined or tapered surface, so that as the closure is threaded onto the container and the surface 19 comes in contact with the upper surface of bead 7 on container 3, the entire skirt portion 12 is gradually forced outward until it snaps over bead 16, and the closure is thus completely threaded onto the container into the configuration shown in FIG. 3. On the other hand, however, when one attempts to remove closure 1 from the container 3, the substantially planar or horizontal upper surface 18 of bead 16, which is firmly engaged with the corresponding lower surface of collar 7 of container 3 now prevents any such gradual outward motion of skirt portion 12, causing an efficient fracture of the closure 1 as is more fully discussed below.
As can be seen in FIGS. 1 and 3 through 8, an area of weakness is located above the annular bead portion 16 of the depending lower skirt portion 12. In particular, as shown in FIGS. 1 and 3 through 8, a groove 21 is located on the outer surface of closure 1. The depth of groove 21 should be such that a distance X (see FIG. 4) is established between the bottom of groove 21 and the inner wall of the closure 1, with X generally being from about 0.003 inches to 0.005 inches, and preferably from about 0.002 inches to about 0.003 inches, and most preferably less than about 0.002 inches. It is also possible, however, and in many applications preferred, for at least a portion or several intermittent portions 23 of groove 21 to pass completely through the wall of closure 1 as also shown in the partial view in FIG. 1, so long as enough of a connection still remains between the internally threaded upper portion 11 and the depending lower skirt portion 12 of closure 1 so that the closure can be applied to the container without causing premature fracture to occur at this time.
Referring again to FIGS. 1 and 4 through 8, groove 21 is formed in the outer wall of closure 1 in a manner such that when fracture occurs it will occur in a horizontal plane across the closure 1, i.e., generally along line 22 formed at the bottom of the generally V-shaped groove 21. Furthermore, fracture will thus occur at a location above lower depending skirt portion 12 such that the entire lower depending skirt portion 12 will then remain (after fracture) affixed to or engaged with container 3, even after internally threaded upper portion 11 is completely removed from the container. As can thus be seen, no part of the depending lower skirt portion 12 includes any weakened area therein, and in fact fracture does not occur in proximity to bead 7 on container 3. More particularly, fracture does not occur either in a plane which passes through bead 7 or in a plane which is tangential to bead 7. On the other hand, where the annular collar 7 to which the annular bead 16 is intended to be affixed comprises the elongated raised surface 25 shown in FIG. 5, the entire portion of the lower skirt portion of the closure which is located below the area of weakness will have a substantially uniform thickness (preferably the same thickness as that of the rest of the closure). It has been found that in this manner the improved results of the present invention can be obtained, and a one-piece closure which results in a clean and efficient fracture of the weakened area upon attempting to remove the closure, results therefrom. This result is unlike any of the results which can be obtained in accordance with any such devices in the prior art.
Referring again to FIG. 1, the outer surface of closure 1 can be seen, and it includes groove 21 located between internally threaded upper portion 11 and the lower depending skirt portion 12 thereof. As can also be seen in FIG. 1, the outer surface of internally threaded upper portion 11 also includes an area which contains a plurality of vertical serrations 24 forming a linear-roughened surface thereon. This surface has been found to be not only aesthetically appealing, but it also aids in assisting one to grip the closure and twisting it in order to effect fracture and remove the internally threaded upper portion 11 therefrom.
As noted above, the closure 1 of the present invention is preferably made of a thermoplastic material, and can be manufactured in an injection molding process. Thus, the internal threads of the closure 1 can be formed by the action of an unscrewing mold. That is, after the part has been formed, during opening of the mold, the cores of the mold rotate and unscrew from the closure, thus forming the threads. The closure itself is kept from turning during this unscrewing phase by means of steel teeth, which engage the bottom of the closure and hold it in place as the core rotates.
After the unscrewing cycle is completed, a stripper plate, which is part of the mold itself, ejects the finished closure form the mold. As the mold initally opens, and before the unscrewing cycle occurs, the closure is released from an undercut position in the mold by means of angle pins which cause cam bars to separate from around the closure. This undercut position was created because protruding portions of the mold (cams) were required in order to mold the annular groove, i.e., the weak portion of the closure which is intended to fracture.
The relationship of the internal diameter of this protruding groove in the cams to the outside diameter of the mold core determines the dimension "X" shown in FIG. 4 at the point of the groove. Thus, it is possible to change that dimension in the closure by merely replacing these cam sections.
The remainder of the molding process is the same as in conventional thermoplastic molding processes.
The closure of the present invention can also be adapted to be used with a variety of containers and bottles, i.e. where for example the annular collar or bead on the bottle has different dimensions from that shown in FIG. 3, or is located at different positions relative to the end of the neck 5 of the bottle, as is shown in the embodiments of FIGS. 1 through 8. Reference is specifically made to the embodiments of FIGS. 5a and 6, which relate to other containers which, in the case of FIG. 5a includes a different neck finish and transfer head configuration, and in the case of FIG. 6 not only includes bead 7, but which also includes an elongated raised surface 25, which is sometimes found in connection with certain containers, including certain wine bottles, etc. This elongated raised surface 25, which can have a width up to about one-half inch or so, is located between threaded neck portion 5 and bead 7, and is of a height which projects above the surface of the bottle less than that of bead 7, in the embodiment shown in FIG. 7. In this embodiment, it is merely required that the overall length of the closure be extended so that the lower depending skirt portion 12 now include an added portion 13. However, it is also possible that the closures of the present invention can be adapted to a container which is similar to that of FIG. 7, but which does not include bead 7. In that case the annular bead portion of the lower depending skirt portion 12 would be adapted to engage the lower end of elongated raised surface 25 itself. In this case, it would be essential that the entire lower depending skirt portion located below groove 21 have a substantially uniform thickness, compared for example to the tapered surface of the band 5 of U.S. Pat. No. 4,033,472, in order to attain the improved results of this invention. In that event, if the elongated raised surface 25 did not extend outwardly beyond the height of the threads 5 on the container itself, it might be necessary to soften and bend the lower end of skirt portion 12 to some degree after application of the closure to the container, but this would not be necessary if the elongated raised surface 25 were raised to a sufficient extent.
Referring to FIGS. 3, 5, 6 and 8, a number of embodiments of the closure 1 which include various sealing means are shown. Thus, in FIG. 3, a yieldable sealing disc 28, made of a material such as cork or other commercial lining materials, which will yield to a degree to absorb the pressure of the upper end of neck portion 5 when the closure 1 is completely threaded onto the container, is maintained against the inner face of end wall 9, such as by means of glue, etc. In FIG. 8, on the other hand, end wall 9 includes a circular central recessed portion 27 and an annular outer elevated portion 29. These portions are connected by means of an annular sealing membrane 30 which connects the recessed portion 27 and the elevated portion 29, and is interposed therebetween at an angle θ (see FIG. 9) of between about 25 and 45 degrees. Sealing membrane 30 comprises the same plastic material from which the entire closure is manufactured, except that whereas the remainder of the end wall 9, i.e., both the recessed portion 27 and the elevated portion 29 generally have a thickness of between about 0.040 inches and 0.060 inches, membrane portion 30 is much thinner, and will generally have a thickness of between about 0.015 inches and 0.025 inches and preferably between about 0.010 inches and 0.015 inches, such as less than about 0.025 inches. In this manner, sealing membrane portion 30 has increased flexibility so that upon threading of closure 1 onto the container, 3, the upper end wall of the neck portion of the container is pressed into contact with membrane portion 30 of end wall 9, and the membrane becomes deformed thereagainst. This produces a seal between the interior of the container and the inner wall of the internally threaded upper portion 11 of the closure 1. In addition, hinges comprising V-shaped, annular grooves 32 and 33 on the inner and outer surfaces of annular membrane portion 30 are also provided in order to further increase the flexibility of the membrane portion 30.
Referring next to FIGS. 5 and 5a, in these cases 4 the inner surface of end wall 9 includes one or more closely spaced annular ridges 34, preferably two or three such ridges, which project downwardly therefrom. These ridges, 34, which are preferably V-shaped in configuration, are located at the precise location where the upper end of the neck portion 5 of container 3 is intended to come into contact with the inner face of end wall 9 when the closure is completely threaded onto the container. In this manner, a seal is once again formed between the inner surface of the container and the inner surface of the internally threaded upper portion 11 of closure 1.
Finally, reference is made to FIG. 6, in which yet another type of seal is shown. In this case, a seal such as that which is shown in U.S. Pat. No. 4,033,472 to Obrist. This seal includes an inner annular sealing rail 36, which again projects from the inner face of end wall 9. In this case, however, the seal is intended to be located within the upper end of the neck portion of the container when the closure is completely threaded onto the container. Projecting outwardly from annular sealing rail 36 is an annular bead portion 38, so as to ensure firm contact between the bead 38 and the inner wall of the container 3. | Tamper-evident closures which are useful in conjunction with various bottles and containers are disclosed. The closures are intended to be used in connection with containers having threaded necks above an annular collar, and they comprise one-piece closures including an end wall, an internally threaded upper portion and a depending lower skirt portion which includes an inwardly projecting bead adapted to engage the annular collar on the container. The depending lower skirt portion has a substantially uniform thickness throughout its entire area intended to contact the annular collar on the container, and theclosure includes an area of weakness which is designed to fracture in a substantially horizontal plane across the closure or, in another embodiment, in a plane which neither passes through nor is tangential to the annular collar on the container. Fracture thus occurs when the closure is unthreaded from the container, thereby leaving the lower skirt portion engaged to the annular collar on the container after the end wall and internally threaded upper portion of the closure have been removed. | 1 |
RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional Patent Application Ser. No. 62/141,223, entitled Systems and Methods for In-Operating-Theatre Imaging of Fresh Tissue Resected During Surgery for Pathology Assessment by Rachet et al., the content of which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] Solid epithelial cancers account for over 10% of all deaths each year world-wide. This figure is expected to increase. Early-stage cancer diagnosis and subsequent complete surgical removal of the tumor offers the best chance for complete cancer cure. With early-stage tumor screening and diagnostics becoming more efficient, the bottleneck lies in efficient surgical management. Current surgical technology cannot precisely define the margins of a tumor, resulting in missed opportunities for life-saving treatment. Tumor residues may remain undetected and untreated until they grow to advanced stages, at which point both patient death rate and overall treatment costs can dramatically increase.
[0003] The diagnosis of a solid tumor typically involves (i) a screen via a blood test or mucosal smear (molecular diagnostics assays); (ii) gross tumor localization in the body typically by means of radiological imaging (e.g., PET, CT, MRI and ultrasound); and (iii) a visual inspection (e.g., endoscopy), and if necessary, the excision of a tissue sample (e.g., biopsy), and a subsequent pathologic examination.
[0004] The pathology laboratory analysis is crucial in the diagnostic process as it is often the basis for the final diagnosis at which the stage of the tumor is confirmed. The pathologist typically prepares thin tissue sections of a frozen or otherwise fixed tissue sample (e.g., a sample processed with formalin or paraffin) obtained during a diagnostic biopsy, then the pathologist examines the thin tissue sections under a microscope. The morphology of the tissue (e.g., cell size and cell arrangement) is the principal basis for distinguishing between healthy and cancer tissue, and for distinguishing between malignant and benign cancer tissue.
[0005] Because diagnostic techniques and cancer screens are improving, cancers are more frequently detected in the earlier stages. This gives oncology surgeons the opportunity to apply the most efficient and least invasive cancer treatment—complete surgical removal of the tumor.
[0006] If no metastases are present, minimally invasive surgical procedures can be used to remove the solid tumor. Typically, chemotherapy is not necessary for patients who undergo a complete resection of the tumor. However, a complete resection requires “tumor-free margins” of the resected tissue, meaning that no tumor cells are left behind in the patient.
[0007] Currently, there is no reliable means available to guide the resection of solid tumors. For certain indications, this results in the need to re-operate on many patients days after the initial operation when an analysis is obtained from the histo-pathology laboratory. Such follow-up surgical procedures usually lead to less favorable outcomes for the patient, psychological stress, and can roughly double treatment and hospitalization costs.
[0008] Healthcare institutions sometimes perform intra-operative frozen-section analysis (FSA) during certain tumor surgeries. Intra-operative FSA is a pathologic assessment of the resected tissue during ongoing surgeries. In spite of inherent problems, such as inferior sample quality when compared to standard paraffin-embedded histology, possible wrong diagnosis due to freezing artifacts (e.g., fatty tissue, like breast or brain tissue, is not suitable for rapid freezing), and tedious sample preparation (e.g., FSA needs to be planned ahead of surgery), long term studies show that intraoperative FSA can reduce the reoperation rate to 10% in the case of breast tumor resections.
[0009] However, intra-operative FSA requires the prolongation of operation time by at least 30 minutes, which, in addition to inconvenience for the patient and the clinical personnel, results in increased cost of the surgery and complications for operating theatre planning and management. Further, many tumor surgeries today do not include pathologic margin assessment, primarily due to the inconvenience and cost of a frozen section analysis. Thus, there is a need for a system for more efficient in-operating-theatre imaging of tissue.
SUMMARY OF THE INVENTION
[0010] The disclosed technology brings histopathology into the operating theatre, to enable real-time intra-operative digital pathology. The disclosed technology utilizes a confocal imaging device that can analyze, in the operating theatre, “optical slices” of fresh tissue without having to fix the resected tissue by freezing and/or processing with formalin or paraffin. This greatly reduces the time necessary for preparing and analyzing a sample and facilitates in-operating-theater analysis of tissue samples obtained during surgery.
[0011] For example, a tissue sample is obtained during surgery and the fresh tissue sample is analyzed by a confocal imaging device located in the operating theatre (e.g., where “operating theatre” includes the area in the operating room, adjacent to the operating room, and/or sufficiently near the operating room such that transport of the sample can be quick and/or does not involve taking the tissue sample out of a sterile environment). The sample is analyzed as a fresh tissue sample (without freezing or other fixation processing that kills cells in the sample), and results are obtained in a timely manner so that feedback is provided to the surgeon while the surgery is still proceeding. For example, images and/or other data obtained from the confocal imaging device can be analyzed remotely by a pathologist (and/or by automated analysis) such that results can be communicated to the surgeon in near real-time. In certain embodiments, the fresh tissue sample is analyzed and results provided to the surgeon within 1 minute of obtaining the sample, within 5 minutes of obtaining the sample, within 10 minutes of obtaining the sample, or within 15 minutes of obtaining the sample. In certain embodiments, the fresh tissue sample has a thickness within a range of 0.5-20 mm, 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm or is no less than 0.2 mm, no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0012] The disclosed technology, in certain embodiments, includes a simple, operating table-side digital histology scanner, with the capability of rapidly scanning all outer margins of a tissue sample (e.g., resection lump, removed tissue mass). Using point-scanning microscopy technology, the disclosed system, in certain embodiments, precisely scans an “optical section” of the resected tissue, and sends the digital image to a pathologist rather than the real tissue, thereby providing the pathologist with the opportunity to analyze the tissue intra-operatively. Thus, the disclosed technology provides digital images with the same information content as FSA, but faster and without destroying the tissue sample itself (e.g., without killing cells).
[0013] For example, a resection lump may be placed into the disclosed histology scanner by an operating theatre nurse and the scanner will rapidly (e.g., in less than 10 minutes) acquire pathology information necessary for an intra-operative pathology consultation. A pathologist can receive and view the digital images remotely and communicate his/her analysis digitally back into the operating theatre to guide the next surgical steps. Further, since the tissue is imaged outside of the patient, it can be stained with one or more of a wide range of fluorescent dyes (e.g., Proflavin, Acridin Orange, and eosin stain).
[0014] The disclosed technology, in some implementations, includes a medical device to assist a surgery group in obtaining a digital image at the microscopy level of a patient sample, for example, a tumorous tissue resected during cancer surgery. The captured image can be used by a pathologist to provide assistance, for example, from a remote location, to the surgery group. For example, the pathologist may evaluate the quality of the surgery from a remote location to ensure that the tumor has been completely removed. In certain embodiments, this review by the pathologist is performed quickly (e.g., in less than 5, 10, 15, or 20 minutes) such that if further removal of the tumor is necessary, the remaining portions of the tumor can be removed during the same operation.
[0015] In some implementations, the device includes a holder to carry the sample and position it on the reader and an imaging system (e.g., a reader) capable of fluorescence microscopy imaging on thick fresh tissue. In some implementations, a computer interface displays the images from the reader to the surgery group. In some implementations, sharing software is used to share images and comments with the pathology group (e.g., outside of the operating theatre).
[0016] In one aspect, the invention is directed to a system for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the system comprising: a light source for providing (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm) an illumination beam that illuminates a fluorescent stained, fresh sample (e.g., a fluorescent-stained fresh sample) (e.g., an unsliced sample preserved for definitive assessment in follow-up testing), wherein the fresh sample is held by a sample holder located in an operating theatre; a beam expander (e.g., collimating lens (e.g., for use with a monomode fibered laser) or a telecentric afocal magnification relay (e.g., for use with a collimated laser)) for expanding the waist of the illumination beam to a size comparable to the field of view to be illuminated, thereby providing a collimated illumination beam; a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)) located between the sample and a detector array, for directing the collimated illumination beam toward a micro optical element array; the micro optical element array (e.g., comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array) for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein the micro optical element array is configured such that: the micro optical element array collects back-emitted light from the sample, and the collected back-emitted light propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array; and a gap (e.g., an airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; a scanning stage for moving a position of the micro optical element array relative to the transparent window and the detector array such that back-emitted light collected by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein: the position of the transparent window relative to the detector array is fixed (e.g., during imaging of the sample by the system), and the scanning stage and micro optical element array are confined (e.g., fully confined) within the system such that the scanning stage and micro optical element array are protected from the sample (e.g., and the outside environment) by the transparent window; an aperture stop for spatially filtering the back-emitted light (e.g., fluorescent light between 510-520 nm, or light with a wavelength greater than or equal to 490 nm and, in some implementations, less than 530 nm; between 491 nm and 520 nm), thereby rejecting out-of-focus light (e.g., filtering out collected sample information that does not originate from the foci of the micro optical elements prior to detection by the detector array), wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and a computing device comprising a processor and a memory storing instructions thereon that, when executed by the processor, cause the processor to construct an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0017] In another aspect, the invention is directed to a system for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the system comprising: a light source for providing (e.g., laser) an illumination beam that illuminates a fluorescent stained, fresh sample (e.g., a preserved sample—i.e., unsliced thereby preserving the sample for definitive assessment) held by a sample holder in an operating theatre; a beam expander (e.g., collimating lens) for expanding a waist of the illumination beam, thereby providing a collimated illumination beam; a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, for directing the collimated illumination beam toward a micro optical element array (e.g., using refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array); the micro optical element array for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce back-emitted light, wherein: the micro optical element array collects back-emitted light from the sample, and the collected back-emitted light propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array; and a gap (e.g., an airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; a scanning stage for moving a position of the transparent window relative to the micro optical element array and the detector array such that back-emitted light collected by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein the position of the micro optical element array relative to the detector array is fixed (e.g., during imaging of the sample by the system); an aperture stop for spatially filtering the back-emitted light (e.g., fluorescent light between 510-520 nm, or light with a wavelength greater than or equal to 490 nm and, in some implementations, less than 530 nm, or between 491 nm and 520 nm), thereby rejecting out-of-focus light (e.g., filtering out collected sample information that is not originating from the foci of the micro optical elements prior to detection by the detector array), wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and a computing device comprising a processor and a memory storing instructions thereon that, when executed by the processor, cause the processor to construct an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0018] In certain embodiments, the memory stores instructions thereon that, when executed by the processor, cause the processor to send, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0019] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample. In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0020] In certain embodiments, the system comprises a kinematic support structure having at least three feet of adjustable height, the support structure supporting the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array and the corresponding optical path are adjustable.
[0021] In certain embodiments, the system comprises a first flat mirror for reflecting the collimated illumination beam onto the beam splitter. In certain embodiments, the system comprises a second flat mirror for reflecting the collimated illumination beam from the beam splitter to the micro optical element array. In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0022] In certain embodiments, the system comprises a field lens for focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0023] In certain embodiments, the beam expander is a collimating lens.
[0024] In certain embodiments, the ratio of detectors to micro optical elements is from 1:1 to 1:12 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0025] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0026] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0027] In certain embodiments, the system is configured for in-operating-theatre imaging of tissue (e.g., fresh) resected during surgery (e.g., cancer surgery) in less than 10 minutes (e.g., less than 5 minutes).
[0028] In certain embodiments, the system comprises a first computing device for sending information regarding the detected back-emitted light (e.g., an image captured by the camera) to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre).
[0029] In certain embodiments, the sample holder is screwed onto the scanning stage.
[0030] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., a high precision positioning stage, e.g., with precision equal or better than one micrometer; in other embodiments, the stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0031] In certain embodiments, the sample holder comprises the transparent window.
[0032] In certain embodiments, the transparent window is a thin transparent window (e.g., 25-50 μm, or 50-100 μm thick; e.g., thin glass with a thickness from 25-50 μm or 50-100 μm).
[0033] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0034] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat between the sample and the micro optical element array.
[0035] In certain embodiments, the scanning stage is configured to bring the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0036] In certain embodiments, the sample holder comprises a metallic body.
[0037] In certain embodiments, the sample holder comprises an opening window (e.g., 40×20 mm, 10-50 mm by 10-50 mm; e.g., covered/filled by the transparent window).
[0038] In certain embodiments, the scanning stage comprises a translation mechanism which is configured for establishing a relative motion between said sample and said micro optical element array.
[0039] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample toward the detector.
[0040] In certain embodiments, the sample holder is configured (e.g. is sized and shaped) to accommodate a sample having a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0041] In another aspect, the invention is directed to a method for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the method comprising: providing, by a light source (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm), an illumination beam for illuminating a fluorescent stained, fresh sample (e.g., a fluorescent-stained fresh sample) (e.g., an unsliced sample preserved for definitive assessment in follow-up testing) held by a sample holder located in an operating theatre; directing a collimated light beam via illumination optics onto the fresh sample (e.g., the fresh fluorescent stained sample) held by the sample holder in the operating theatre, wherein the illumination optics comprise: a beam expander expanding a waist of the illumination beam, thereby providing the collimated illumination beam, a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, directing the collimated illumination beam toward a micro optical element array (e.g., the micro optical element array comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array), and the micro optical element array for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein: each micro optical element focuses a portion of the collimated illumination beam onto the sample, and a gap (e.g., airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; directing the back-emitted light from the sample to the detector array via detecting optics, the detecting optics comprising: the micro optical element array, which collects the back-emitted light from the sample, which propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to the detector array, and an aperture stop spatially filtering the back-emitted light, thereby rejecting out-of-focus light; moving, by a scanning stage, a position of the micro optical element array relative to the transparent window and the detector array such that back-emitted light focused by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein: the position of the transparent window relative to the detector array is fixed (e.g., during imaging of the sample by the system), and the scanning stage and micro optical element array are confined (e.g., fully confined) within the system such that the scanning stage and micro optical element array are protected from the sample (e.g., and the outside environment) by the transparent window; detecting, by the detector array, the back-emitted light filtered by the aperture stop, wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and constructing, by a processor of a computing device, an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0042] In another aspect, the invention is directed to a method for in-operating-theatre imaging of fresh tissue resected during surgery (e.g., cancer surgery) for pathology assessment, the method comprising: providing, by a light source (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm), an illumination beam for illuminating a fluorescent stained, fresh sample (e.g., a preserved sample—i.e., unsliced thereby preserving the sample for definitive assessment) held by a sample holder in an operating theatre; directing a collimated light beam via illumination optics onto a fresh (e.g., fluorescent-stained) sample held by a sample holder in an operating theatre, wherein the illumination optics comprise: a beam expander expanding a waist of the illumination beam, thereby providing the collimated illumination beam, a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, directing the collimated illumination beam toward a micro optical element array (e.g., the micro optical element array comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array), and the micro optical element array focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein: each micro optical element in the micro optical element array focuses a portion of the collimated illumination beam onto the sample, and a gap (e.g., airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; directing the back-emitted light from the sample to the detector array via detecting optics, the detecting optics comprising: the micro optical element array, which collects the back-emitted light that propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array, and an aperture stop spatially filtering the back-emitted light, thereby rejecting out-of-focus light; moving, by a scanning stage, a position of the transparent window relative to the micro optical element array and the detector array such that back-emitted light focused by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample, wherein the position of the micro optical element array relative to the detector array is fixed (e.g., during imaging of the sample by the system); detecting, by the detector array, the back-emitted light filtered by the aperture stop, wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and constructing, by a processor of a computing device, an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0043] In certain embodiments, the method comprises sending, by the processor, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0044] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample.
[0045] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0046] In certain embodiments, a kinematic support structure having at least three feet of adjustable height supports the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array (e.g., and the corresponding optical path) are adjustable.
[0047] In certain embodiments, the illumination optics comprises: a first flat mirror reflecting the collimated illumination beam onto the beam splitter. In certain embodiments, the illumination optics comprises: a second flat mirror reflecting the collimated illumination beam from the beam splitter to the micro optical element array. In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0048] In certain embodiments, the detection optics comprises: a field lens focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0049] In certain embodiments, the beam expander is a collimating lens.
[0050] In certain embodiments, the ratio of detectors to micro optical elements is from 1:1 to 1:12 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0051] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0052] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0053] In certain embodiments, the method is performed in less than 10 minutes (e.g., less than 5 minutes).
[0054] In certain embodiments, the method comprises sending, by a processor of a first computing device, to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre) information regarding the detected back-emitted light (e.g., an image captured by the camera).
[0055] In certain embodiments, the method comprises, prior to providing an illumination beam for illuminating the sample: staining the sample with a fluorescent stain; and placing the sample in/on the sampler holder.
[0056] In certain embodiments, the sample holder is screwed onto the scanning stage.
[0057] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., high precision positioning stage; e.g., in other embodiments, the scanning stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0058] In certain embodiments, the sample holder comprises the transparent window.
[0059] In certain embodiments, the transparent window is a thin transparent window (e.g., 25-50 μm, or 50-100 μm thick).
[0060] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0061] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat) between the sample and the micro optical element array.
[0062] In certain embodiments, the scanning stage brings the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0063] In certain embodiments, the sample holder comprises a metallic body.
[0064] In certain embodiments, the sample holder comprises an opening (e.g., 40×20 mm, 10-50 mm by 10-50 mm) covered/filled by the transparent window.
[0065] In certain embodiments, the scanning stage comprises a translation system for establishing a relative motion between the sample and the micro optical element array.
[0066] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample towards the detector.
[0067] In certain embodiments, the sample has a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0068] In another aspect, the invention is directed to a method for in-operating-theatre imaging of tissue (e.g., fresh tissue) resected during surgery (e.g., cancer surgery) for pathology assessment, the method comprising: intraoperatively resecting tissue to obtain a fresh tissue sample; procuring an image of the fresh tissue sample (e.g., using an embodiment of the system described herein); and sending, by a processor of a first computing device, to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre) the image of the fresh tissue sample.
[0069] In various embodiments, elements or features described with respect to one aspect of the invention can be used with respect to another aspect of the invention (e.g., any limitation described with respect to a system embodiment of the invention can apply to a method embodiment of the invention, and vice versa).
[0070] In another aspect, the disclosed technology includes a system for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the system including: a light source for providing (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm) an illumination beam that illuminates a fluorescent stained, fresh sample (e.g., a fluorescent-stained fresh sample) (e.g., an unsliced sample preserved for definitive assessment in follow-up testing), wherein the fresh sample is held by a sample holder located in an operating theatre; a beam expander (e.g., collimating lens (e.g., for use with a monomode fibered laser) or a telecentric afocal magnification relay (e.g., for use with a collimated laser)) for expanding the waist of the illumination beam to a size comparable to the field of view to be illuminated, thereby providing a collimated illumination beam; a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)) located between the sample and a detector array, for directing the collimated illumination beam toward a micro optical element array; the micro optical element array (e.g., comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array) for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein the micro optical element array is configured such that: the micro optical element array collects back-emitted light from the sample, and the collected back-emitted light propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array; and a gap (e.g., an airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a window (e.g., a transparent window, e.g., made of glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; a scanning stage for moving a position of the micro optical element array relative to the transparent window and the detector array such that back-emitted light collected by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein: the position of the transparent window relative to the detector array is fixed (e.g., during imaging of the sample by the system), and the scanning stage and micro optical element array are confined (e.g., fully confined) within the system such that the scanning stage and micro optical element array are protected from the sample (e.g., and the outside environment) by the transparent window; an aperture stop for spatially filtering the back-emitted light (e.g., fluorescent light between 510-520 nm, or light with a wavelength greater than or equal to 490 nm and, in some implementations, less than 530 nm; between 491 nm and 520 nm), thereby rejecting out-of-focus light (e.g., filtering out collected sample information that does not originate from the foci of the micro optical elements prior to detection by the detector array), wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and a computing device comprising a processor and a memory storing instructions thereon that, when executed by the processor, cause the processor to construct an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0071] In certain embodiments, the memory stores instructions thereon that, when executed by the processor, cause the processor to send, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0072] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample.
[0073] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0074] In certain embodiments, the curved surface of each micro optical element has a conical shaped surface.
[0075] In certain embodiments, the curved surface of each micro optical element has a hyperbolic shaped surface.
[0076] In certain embodiments, the curved surface of each micro optical element has a conic constant from −1.8 to −2.2 (e.g., −2).
[0077] In certain embodiments, each micro optical element has a Strehl ratio greater than or equal to 0.8.
[0078] In certain embodiments, each micro optical element has a spot size from 0.2 μm to 5 μm, 0.2 μm to 1 μm, 0.3 μm to 0.6 μm, and 0.4 μm to 0.5 μm.
[0079] In certain embodiments, a free working distance (i.e., a distance from the tip of the micro optical elements to a focal plane of the micro optical element array) is from 80 μm to 450 μm, 150 μm to 350 μm, or 250 μm to 300 μm.
[0080] In certain embodiments, the micro optical element array has a focal plane from 10 μm to 200 μm, 20 μm to 150 μm, or 50 μm to 100 μm above the transparent window.
[0081] In certain embodiments, the system includes a kinematic support structure having at least three feet (e.g., four) of adjustable height, the support structure supporting the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array and the corresponding optical path are adjustable.
[0082] In certain embodiments, the system includes a first flat mirror for reflecting the collimated illumination beam onto the beam splitter.
[0083] In certain embodiments, the system includes a second flat mirror for reflecting the collimated illumination beam from the beam splitter to the micro optical element array.
[0084] In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0085] In certain embodiments, the system includes a field lens for focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0086] In certain embodiments, the beam expander is a collimating lens.
[0087] In certain embodiments, the ratio of micro optical elements to detectors is from 1:1 to 1:100, 1:5 to 1:80, 1:20 to 1:70, 1:30 to 1:60, or 1:40 to 1:50 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0088] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0089] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0090] In certain embodiments, the system is configured for in-operating-theatre imaging of tissue (e.g., fresh) resected during surgery (e.g., cancer surgery) in less than 10 minutes (e.g., less than 5 minutes).
[0091] In certain embodiments, the system includes a first computing device for sending information regarding the detected back-emitted light (e.g., an image captured by the camera) to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre).
[0092] In certain embodiments, the system includes the sample holder is screwed onto the scanning stage.
[0093] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., a high precision positioning stage, e.g., with precision equal or better than one micrometer; in other embodiments, the stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0094] In certain embodiments, the sample holder comprises the transparent window.
[0095] In certain embodiments, the transparent window is a thin transparent window (e.g., 50-100 μm, or 100-500 μm thick; e.g., thin glass with a thickness from 50-100 μm or 100-500 μm).
[0096] In certain embodiments, the system includes an optical interface clamp (e.g., ring-shaped) that maintains the transparent window in place.
[0097] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0098] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat between the sample and the micro optical element array.
[0099] In certain embodiments, the scanning stage is configured to bring the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0100] In certain embodiments, the sample holder comprises a metallic body.
[0101] In certain embodiments, the sample holder comprises an opening window (e.g., 40×20 mm, 10-50 mm by 10-50 mm; e.g., covered/filled by the transparent window).
[0102] In certain embodiments, the scanning stage comprises a translation mechanism which is configured for establishing a relative motion between said sample and said micro optical element array.
[0103] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample toward the detector.
[0104] In certain embodiments, the sample holder is configured (e.g. is sized and shaped) to accommodate a sample having a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0105] In certain embodiments, the system includes a mobile cart.
[0106] In certain embodiments, the system includes an attachment system for attaching a removable sample holder to the scanning stage.
[0107] In certain embodiments, the attachment system comprises a support base mounted on the scanning stage, the support base having a mount with one or more protrusions extending from the mount, wherein the mount is hollow on the inside and the support base has a corresponding opening therein such that an optical chip can scan a sample through the support base.
[0108] In another aspect, the disclosed technology includes a system for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the system including: a light source for providing (e.g., laser) an illumination beam that illuminates a fluorescent stained, fresh sample (e.g., a preserved sample—i.e., unsliced thereby preserving the sample for definitive assessment) held by a sample holder in an operating theatre; a beam expander (e.g., collimating lens) for expanding a waist of the illumination beam, thereby providing a collimated illumination beam; a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, for directing the collimated illumination beam toward a micro optical element array (e.g., using refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array); the micro optical element array for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce back-emitted light, wherein: the micro optical element array collects back-emitted light from the sample, and the collected back-emitted light propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array; and a gap (e.g., an airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; a scanning stage for moving a position of the transparent window relative to the micro optical element array and the detector array such that back-emitted light collected by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein the position of the micro optical element array relative to the detector array is fixed (e.g., during imaging of the sample by the system); an aperture stop for spatially filtering the back-emitted light (e.g., fluorescent light between 510-520 nm, or light with a wavelength greater than or equal to 490 nm and, in some implementations, less than 530 nm, or between 491 nm and 520 nm), thereby rejecting out-of-focus light (e.g., filtering out collected sample information that is not originating from the foci of the micro optical elements prior to detection by the detector array), wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and a computing device comprising a processor and a memory storing instructions thereon that, when executed by the processor, cause the processor to construct an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0109] In certain embodiments, the memory stores instructions thereon that, when executed by the processor, cause the processor to send, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0110] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample.
[0111] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0112] In certain embodiments, the curved surface of each micro optical element has a conical shaped surface.
[0113] In certain embodiments, the curved surface of each micro optical element has a hyperbolic shaped surface.
[0114] In certain embodiments, the curved surface of each micro optical element has a conic constant from −1.8 to −2.2 (e.g., −2).
[0115] In certain embodiments, each micro optical element has a Strehl ratio greater than or equal to 0.8.
[0116] In certain embodiments, each micro optical element has a spot size from 0.2 μm to 5 μm, 0.2 μm to 1 μm, 0.3 μm to 0.6 μm, and 0.4 μm to 0.5 μm.
[0117] In certain embodiments, a free working distance (i.e., a distance from the tip of the micro optical elements to a focal plane of the micro optical element array) is from 80 μm to 450 μm, 150 μm to 350 μm, or 250 μm to 300 μm.
[0118] In certain embodiments, the micro optical element array has a focal plane from 10 μm to 200 μm, 20 μm to 150 μm, or 50 μm to 100 μm above the transparent window.
[0119] In certain embodiments, the system includes a kinematic support structure having at least three feet (e.g., four) of adjustable height, the support structure supporting the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array and the corresponding optical path are adjustable.
[0120] In certain embodiments, the system includes a first flat mirror for reflecting the collimated illumination beam onto the beam splitter.
[0121] In certain embodiments, the system includes a second flat mirror for reflecting the collimated illumination beam from the beam splitter to the micro optical element array.
[0122] In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0123] In certain embodiments, the system includes a field lens for focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0124] In certain embodiments, the beam expander is a collimating lens.
[0125] In certain embodiments, the ratio of micro optical elements to detectors is from 1:1 to 1:100, 1:5 to 1:80, 1:20 to 1:70, 1:30 to 1:60, or 1:40 to 1:50 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0126] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0127] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0128] In certain embodiments, the system is configured for in-operating-theatre imaging of tissue (e.g., fresh) resected during surgery (e.g., cancer surgery) in less than 10 minutes (e.g., less than 5 minutes).
[0129] In certain embodiments, the system includes a first computing device for sending information regarding the detected back-emitted light (e.g., an image captured by the camera) to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre).
[0130] In certain embodiments, the system includes the sample holder is screwed onto the scanning stage.
[0131] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., a high precision positioning stage, e.g., with precision equal or better than one micrometer; in other embodiments, the stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0132] In certain embodiments, the sample holder comprises the transparent window.
[0133] In certain embodiments, the transparent window is a thin transparent window (e.g., 50-100 μm, or 100-500 μm thick; e.g., thin glass with a thickness from 50-100 μm or 100-500 μm).
[0134] In certain embodiments, the system includes an optical interface clamp (e.g., ring-shaped) that maintains the transparent window in place.
[0135] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0136] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat between the sample and the micro optical element array.
[0137] In certain embodiments, the scanning stage is configured to bring the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0138] In certain embodiments, the sample holder comprises a metallic body.
[0139] In certain embodiments, the sample holder comprises an opening window (e.g., 40×20 mm, 10-50 mm by 10-50 mm; e.g., covered/filled by the transparent window).
[0140] In certain embodiments, the scanning stage comprises a translation mechanism which is configured for establishing a relative motion between said sample and said micro optical element array.
[0141] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample toward the detector.
[0142] In certain embodiments, the sample holder is configured (e.g. is sized and shaped) to accommodate a sample having a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0143] In certain embodiments, the system includes a mobile cart.
[0144] In certain embodiments, the system includes an attachment system for attaching a removable sample holder to the scanning stage.
[0145] In certain embodiments, the attachment system comprises a support base mounted on the scanning stage, the support base having a mount with one or more protrusions extending from the mount, wherein the mount is hollow on the inside and the support base has a corresponding opening therein such that an optical chip can scan a sample through the support base.
[0146] In another aspect, the disclosed technology includes a method for in-operating-theatre imaging of fresh tissue samples resected during surgery (e.g., cancer surgery) for pathology assessment, the method including: providing, by a light source (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm), an illumination beam for illuminating a fluorescent stained, fresh sample (e.g., a fluorescent-stained fresh sample) (e.g., an unsliced sample preserved for definitive assessment in follow-up testing) held by a sample holder located in an operating theatre; directing a collimated light beam via illumination optics onto the fresh sample (e.g., the fresh fluorescent stained sample) held by the sample holder in the operating theatre, wherein the illumination optics comprise: a beam expander expanding a waist of the illumination beam, thereby providing the collimated illumination beam, a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, directing the collimated illumination beam toward a micro optical element array (e.g., the micro optical element array comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array), and the micro optical element array for focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein: each micro optical element focuses a portion of the collimated illumination beam onto the sample, and a gap (e.g., airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; directing the back-emitted light from the sample to the detector array via detecting optics, the detecting optics comprising: the micro optical element array, which collects the back-emitted light from the sample, which propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to the detector array, and an aperture stop spatially filtering the back-emitted light, thereby rejecting out-of-focus light; moving, by a scanning stage, a position of the micro optical element array relative to the transparent window and the detector array such that back-emitted light focused by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample), wherein: the position of the transparent window relative to the detector array is fixed (e.g., during imaging of the sample by the system), and the scanning stage and micro optical element array are confined (e.g., fully confined) within the system such that the scanning stage and micro optical element array are protected from the sample (e.g., and the outside environment) by the transparent window; detecting, by the detector array, the back-emitted light filtered by the aperture stop, wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and constructing, by a processor of a computing device, an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0147] In certain embodiments, the method includes sending, by the processor, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0148] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample.
[0149] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0150] In certain embodiments, the curved surface of each micro optical element has a conical shaped surface.
[0151] In certain embodiments, the curved surface of each micro optical element has a hyperbolic shaped surface.
[0152] In certain embodiments, the curved surface of each micro optical element has a conic constant from −1.8 to −2.2 (e.g., −2).
[0153] In certain embodiments, each micro optical element has a Strehl ratio greater than or equal to 0.8.
[0154] In certain embodiments, each micro optical element has a spot size of 0.1 μm to 2 μm, 0.2 μm to 1 μm, 0.3 μm to 0.6 μm, or 0.4 μm to 0.5 μm.
[0155] In certain embodiments, a free working distance (i.e., a distance from the tip of the micro optical elements to a focal plane of the micro optical element array) is from 80 μm to 450 μm, 150 μm to 350 μm, or 250 μm to 300 μm.
[0156] In certain embodiments, the micro optical element array has a focal plane from 10 μm to 200 μm, 20 μm to 150 μm, or 50 μm to 100 μm above the transparent window.
[0157] In certain embodiments, a kinematic support structure having at least three feet (e.g., four) of adjustable height supports the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array (e.g., and the corresponding optical path) are adjustable.
[0158] In certain embodiments, the illumination optics includes: a first flat mirror reflecting the collimated illumination beam onto the beam splitter.
[0159] In certain embodiments, the illumination optics includes a second flat mirror reflecting the collimated illumination beam from the beam splitter to the micro optical element array.
[0160] In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0161] In certain embodiments, the detection optics comprises: a field lens focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0162] In certain embodiments, the beam expander is a collimating lens.
[0163] In certain embodiments, the ratio of detectors to micro optical elements is from 1:1 to 1:100, 1:5 to 1:80, 1:20 to 1:70, 1:30 to 1:60, or 1:40 to 1:50 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0164] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0165] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0166] In certain embodiments, the method is performed in less than 10 minutes (e.g., less than 5 minutes).
[0167] In certain embodiments, the method includes sending, by a processor of a first computing device, to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre) information regarding the detected back-emitted light (e.g., an image captured by the camera).
[0168] In certain embodiments, the method includes, prior to providing an illumination beam for illuminating the sample: staining the sample with a fluorescent stain; and placing the sample in/on the sampler holder.
[0169] In certain embodiments, the sample holder is screwed onto the scanning stage.
[0170] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., high precision positioning stage; e.g., in other embodiments, the scanning stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0171] In certain embodiments, the sample holder comprises the transparent window.
[0172] In certain embodiments, the transparent window is a thin transparent window (e.g., 50-100 μm, or 100-500 μm thick; e.g., thin glass with a thickness from 50-100 μm or 100-500 μm).
[0173] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0174] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat) between the sample and the micro optical element array.
[0175] In certain embodiments, the scanning stage brings the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0176] In certain embodiments, the sample holder comprises a metallic body.
[0177] In certain embodiments, the sample holder comprises an opening (e.g., 40×20 mm, 10-50 mm by 10-50 mm) covered/filled by the transparent window.
[0178] In certain embodiments, the scanning stage comprises a translation system for establishing a relative motion between the sample and the micro optical element array.
[0179] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample towards the detector.
[0180] In certain embodiments, the sample has a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0181] In another aspect, the disclosed technology includes the disclosed technology includes a method for in-operating-theatre imaging of fresh tissue resected during surgery (e.g., cancer surgery) for pathology assessment, the method including: providing, by a light source (e.g., laser or other light source providing light with a wavelength of 488 nm or between 450-490 nm), an illumination beam for illuminating a fluorescent stained, fresh sample (e.g., a preserved sample—i.e., unsliced thereby preserving the sample for definitive assessment) held by a sample holder in an operating theatre; directing a collimated light beam via illumination optics onto a fresh (e.g., fluorescent-stained) sample held by a sample holder in an operating theatre, wherein the illumination optics comprise: a beam expander expanding a waist of the illumination beam, thereby providing the collimated illumination beam, a beam splitter (e.g., dichroic mirror/filter, prism, or grating(s)), located between the sample and a detector array, directing the collimated illumination beam toward a micro optical element array (e.g., the micro optical element array comprising refractive lenses, Fresnel zone plates, micro reflective objectives, and/or GRIN lenses; e.g., a micro lens array), and the micro optical element array focusing the collimated illumination beam from the beam splitter onto the sample, thereby forming an array of tight foci for exciting the fluorescence in the sample to produce the back-emitted light, wherein: each micro optical element in the micro optical element array focuses a portion of the collimated illumination beam onto the sample, and a gap (e.g., airgap) of less than 500 μm (e.g., 50-150 μm, 80-120 μm) is maintained between the micro optical element array and a transparent window (e.g., glass, quartz, sapphire, plastic) onto which (e.g., above which) the sample is placed for imaging; directing the back-emitted light from the sample to the detector array via detecting optics, the detecting optics comprising: the micro optical element array, which collects the back-emitted light that propagates (e.g., as individual collimated beams) and is directed (e.g., by a set of optics) to a detector array, and an aperture stop spatially filtering the back-emitted light, thereby rejecting out-of-focus light; moving, by a scanning stage, a position of the transparent window relative to the micro optical element array and the detector array such that back-emitted light focused by the micro optical element array is detected by the detector array to form a scanned confocal image (e.g., to construct an optical slice of the sample, wherein the position of the micro optical element array relative to the detector array is fixed (e.g., during imaging of the sample by the system); detecting, by the detector array, the back-emitted light filtered by the aperture stop, wherein the detector array comprises a plurality of detectors, each detector independently detecting a portion of the back-emitted light originating from a micro optical element in the micro optical element array; and constructing, by a processor of a computing device, an image representing an optical slice of the fresh tissue sample based on the back-emitted light detected by the detector array.
[0182] In certain embodiments, the method includes sending, by the processor, via a network, the image to a second computing device such that a pathologist in a remote location (e.g., outside of the operating theatre) can perform the pathology assessment.
[0183] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the sample.
[0184] In certain embodiments, the micro optical element array comprises a plurality of micro optical elements having curved surfaces facing the collimated illumination beam.
[0185] In certain embodiments, the curved surface of each micro optical element has a conical shaped surface.
[0186] In certain embodiments, the curved surface of each micro optical element has a hyperbolic shaped surface.
[0187] In certain embodiments, the curved surface of each micro optical element has a conic constant from −1.8 to −2.2 (e.g., −2).
[0188] In certain embodiments, each micro optical element has a Strehl ratio greater than or equal to 0.8.
[0189] In certain embodiments, each micro optical element has a spot size of 0.1 μm to 2 μm, 0.2 μm to 1 μm, 0.3 μm to 0.6 μm, or 0.4 μm to 0.5 μm.
[0190] In certain embodiments, a free working distance (i.e., a distance from the tip of the micro optical elements to a focal plane of the micro optical element array) is from 80 μm to 450 μm, 150 μm to 350 μm, or 250 μm to 300 μm.
[0191] In certain embodiments, the micro optical element array has a focal plane from 10 μm to 200 μm, 20 μm to 150 μm, or 50 μm to 100 μm above the transparent window.
[0192] In certain embodiments, a kinematic support structure having at least three feet (e.g., four) of adjustable height supports the scanning stage such that the height and tilt of the transparent window relative to the micro optical element array (e.g., and the corresponding optical path) are adjustable.
[0193] In certain embodiments, the illumination optics includes: a first flat mirror reflecting the collimated illumination beam onto the beam splitter.
[0194] In certain embodiments, the illumination optics includes a second flat mirror reflecting the collimated illumination beam from the beam splitter to the micro optical element array.
[0195] In certain embodiments, the second flat mirror reflects the back-emitted light passed through the micro optical element array from the sample through the beam splitter.
[0196] In certain embodiments, the detection optics comprises: a field lens focusing the back-emitted light prior to spatially filtering the back-emitted light.
[0197] In certain embodiments, the beam expander is a collimating lens.
[0198] In certain embodiments, the ratio of detectors to micro optical elements is from 1:1 to 1:100, 1:5 to 1:80, 1:20 to 1:70, 1:30 to 1:60, or 1:40 to 1:50 (e.g., about 1:1, 1:2, 1:3, 1:4, 1:6, 1:8, or 1:12, e.g., to the nearest whole number, or within a range of any two of these values).
[0199] In certain embodiments, the micro optical element array comprises from 1000 to 100,000 micro optical elements (e.g., 1600 micro optical elements for a 10 mm field of view; 6400 micro optical elements for a 20 mm field of view, etc.).
[0200] In certain embodiments, the sample is stained with a fluorescent stain (e.g., proflavine, acridine orange, hematoxylin or eosin).
[0201] In certain embodiments, the method is performed in less than 10 minutes (e.g., less than 5 minutes).
[0202] In certain embodiments, the method includes sending, by a processor of a first computing device, to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre) information regarding the detected back-emitted light (e.g., an image captured by the camera).
[0203] In certain embodiments, the method includes, prior to providing an illumination beam for illuminating the sample: staining the sample with a fluorescent stain; and placing the sample in/on the sampler holder.
[0204] In certain embodiments, the sample holder is screwed onto the scanning stage.
[0205] In certain embodiments, the scanning stage is a three axis positioning stage (e.g., high precision positioning stage; e.g., in other embodiments, the scanning stage is a two-axis positioning stage, e.g., high precision positioning stage).
[0206] In certain embodiments, the sample holder comprises the transparent window.
[0207] In certain embodiments, the transparent window is a thin transparent window (e.g., 50-100 μm, or 100-500 μm thick; e.g., thin glass with a thickness from 50-100 μm or 100-500 μm).
[0208] In certain embodiments, the sample holder comprises a seal at the bottom of the transparent window to protect the system from sample liquid.
[0209] In certain embodiments, the transparent window provides an optical interface (e.g., transparent and flat) between the sample and the micro optical element array.
[0210] In certain embodiments, the scanning stage brings the transparent window in close proximity to the micro optical element array (e.g., within 100 μm).
[0211] In certain embodiments, the sample holder comprises a metallic body.
[0212] In certain embodiments, the sample holder comprises an opening (e.g., 40×20 mm, 10-50 mm by 10-50 mm) covered/filled by the transparent window.
[0213] In certain embodiments, the scanning stage comprises a translation system for establishing a relative motion between the sample and the micro optical element array.
[0214] In certain embodiments, the sample is located in the focus area of the micro optical element array; and each micro optical element is configured to collect and direct sample information from the sample towards the detector.
[0215] In certain embodiments, the sample has a thickness that is within a range of 0.5-20 mm (e.g., that is within a range of 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm, and/or that is no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm).
[0216] In another aspect, the disclosed technology includes a method for in-operating-theatre imaging of tissue (e.g., fresh tissue) resected during surgery (e.g., cancer surgery) for pathology assessment, the method including: intraoperatively resecting tissue to obtain a fresh tissue sample; procuring an image of the fresh tissue sample (e.g., using the system of any one of claims 1 to 39 ); and sending, by a processor of a first computing device, to a second computing device (e.g., remote from the first computer device—i.e., outside the operating theatre) the image of the fresh tissue sample.
[0217] In another aspect, the disclosed technology includes a sample holding device, including: a support base that can be mounted on a pathology system, the support base comprising a mount having one or more protrusions extending from the mount, wherein the mount is hollow on the inside and the support base has a corresponding opening therein such that an optical chip can scan a sample through the support base; and a removable sample holder that is removably attachable to the support base, the removable sample holder comprising: a housing having an opening therethrough with one or more (e.g., two) interior protrusions extending into the opening, wherein the size and shape (e.g., round, cylindrical, circular) of the opening in the housing is such that the removable sample holder can be attached over the support base and twisted such that the one or more interior protrusions of the removable sample holder engage the one or more protrusions of the support base, thereby securing the removable sample holder to the support base; and a transparent window on which the sample can be placed and through which the optical chip can image the sample.
BRIEF DESCRIPTION OF THE FIGURES
[0218] The foregoing and other objects, aspects, features, and advantages of the present disclosure will become more apparent and better understood by referring to the following description taken in conjunction with the accompanying drawings, in which:
[0219] FIG. 1A is a side view of an example system for in-operating-theatre of fresh thick tissue resected during surgery, in accordance with an embodiment of the invention;
[0220] FIG. 1B is a top view of an example system for in-operating-theatre of fresh thick tissue resected during surgery, in accordance with an embodiment of the invention;
[0221] FIGS. 2A-C are photographs of an example system for in-operating-theatre of fresh thick tissue resected during surgery, in accordance with an embodiment of the invention;
[0222] FIG. 3 is a flowchart of an example method for imaging a sample, in accordance with an embodiment of the invention;
[0223] FIGS. 4A-G are illustrations of an example system for in-operating-theatre of fresh thick tissue resected during surgery, in accordance with an embodiment of the invention;
[0224] FIG. 5 is an illustration of an example sample holder, in accordance with an embodiment of the invention;
[0225] FIGS. 6A-6J is an illustration of an example sample holder, in accordance with an embodiment of the invention;
[0226] FIG. 7 is an illustration of an example structure for adjusting both height and tilt of the glass window (e.g., by moving the scanning stage) relative to the optical chip and corresponding optical path with an embodiment of the invention;
[0227] FIG. 8 is an illustration of an example camera and pinhole assembly, in accordance with an embodiment of the invention;
[0228] FIG. 9 is an illustration of an example optical chip scanning system, in accordance with an embodiment of the invention;
[0229] FIGS. 10A-G are illustrations of example systems for in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment, in accordance with embodiments of the invention;
[0230] FIGS. 11A through 11C illustrate an example implementation of a specimen imaging area, in accordance with an embodiment of the invention;
[0231] FIG. 11D is an illustration of example optical interface clamps, in accordance with embodiments of the invention;
[0232] FIGS. 11E through 11G are illustrations of an example optical interface mount, in accordance with an embodiment of the invention;
[0233] FIG. 12A is an illustration of an example mobile cart in accordance with an embodiment of the invention;
[0234] FIG. 12B is a photograph of an example mobile cart in accordance with an embodiment of the invention;
[0235] FIG. 13 is a screenshot of a microscopy image acquired on fresh tissue using the disclosed technology.
[0236] FIG. 14 is an image acquired on fresh mice kidney tissue using the disclosed technology.
[0237] FIG. 15 shows a block diagram of an exemplary cloud computing environment; and
[0238] FIG. 16 is a block diagram of a computing device and a mobile computing device.
[0239] The features and advantages of the present disclosure will become more apparent from the detailed description set forth below when taken in conjunction with the drawings, in which like reference characters identify corresponding elements throughout. In the drawings, like reference numbers generally indicate identical, functionally similar, and/or structurally similar elements.
DETAILED DESCRIPTION OF THE INVENTION
[0240] In the present text the expression “micro optical element” is used to describe a miniaturized focusing element with a cross sectional diameter of less than 1 mm (e.g., between 10 micrometers and 500 micrometers) that focuses light. In some implementations, the micro optical element is a micro lens having a paraxial radius of curvature that is in the order of magnitude of its diameter. In some implementations, the micro optical element is a refractive lens, Fresnel zone plate, GRIN lens, or micro reflective objective. The term “micro optical element array” is used to describe a structure composed of a plurality of micro optical elements positioned in a grid which may be, but is not necessarily, periodic. While the description may describe embodiments of the disclosed technology implemented with a micro lens array, similar embodiments may be implemented with micro optical elements.
[0241] The expression “fresh tissue” is generally used herein to describe tissue resected or otherwise obtained during surgery that is not fixed tissue. For example, fresh tissue has not been frozen or processed with formalin, paraffin. In some implementations, the fresh tissue sample is in the same or similar state that it was in when it was removed from the patient. Fresh tissue is a living tissue that has not yet been fixed, in the histology terminology understanding. In the fields of histology and pathology, fixation is a critical step in the preparation of histological sections by which biological tissues are preserved from decay, thereby preventing autolysis or putrefaction. The broad objective of tissue fixation is to preserve cells and tissue components and to do this in such a way as to allow for the preparation of thin, stained sections.
[0242] Even though the microscopy system described herein may be used to image fixed thin tissue sections, an advantage that is achieved, in certain embodiments, is to provide a solution for fresh tissue imaging that does not necessitate a fixation procedure and thin slicing of the sample. In consequence, embodiments described herein allow microscopic imaging on fresh thick tissue, in contrast to standard preparation of fixed thin tissue in histology.
[0243] In the present text the expression “operating theatre” is used to describe a facility within a hospital where surgical operations are carried out in a sterile environment, including an operating room and operating suite. It also refers to an operating room with an on-site laboratory (e.g., adjacent to the operating room). In some implementations, the operating theatre is an operating room.
[0244] The disclosed technology may be used for the observation of thick fresh tissue samples (e.g., having a thickness within a range of 0.5-20 mm, 3-5 mm, 5-10 mm, 7-15 mm, 10-25 mm, 15-30 mm, or 25-35 mm or is no less than 0.2 mm, no less than 0.5 mm, no less than 1 mm, no less than 3 mm, or no less than 5 mm)) at a cellular level during surgery in order to provide pathology assistance to ongoing surgery. The sample may be processed using the disclosed technology in less than 10 minutes (e.g., less than 5 mins) because, for example, the sample does not need to be mechanically sliced as the disclosed microscopy may be used directly on fresh thick tissue (e.g., using optical slicing, a non-destructive method). Further, the technical speed of reading the sample is improved, and this approach preserves the sample such that it is available for definitive assessment (contrary of FSA). Additionally, images can be shared electronically which allows direct connection between the pathologist and the surgical team.
[0245] FIG. 1A illustrates a top view of an example in-operating-theatre pathology system for imaging fresh, thick tissue. FIG. 1B illustrates a side view of the same example system. The disclosed technology uses a micro lens array 104 for performing large-field high resolution microscopy and/or micro-projection of in-operating-theatre imaging for fresh, thick tissue for pathology assessment. Fresh thick tissue is typically difficult to image as the illumination light is passed through the sample 101 , such as a biopsy or a tumor resection, and the collected emission light collected also travels through the sample 101 . The disclosed technology overcomes this challenge by using, among other things, transmitting optics to limit the part of the light path that has to propagate into the sample 101 , thereby allowing imaging of fresh thick tissue. Examples of transmitting optics that can be used include refractive lens, Fresnel zone plate and the micro reflective objective described in U.S. patent application Ser. No. 14/415,106, filed January 2015, entitled Reflective Optical Objective, which is hereby incorporated by reference in its entirety and attached hereto as an Appendix.
[0246] The illumination light is provided by a light source 109 and is directed onto a beam splitter 112 that transmits the collected light. In some implementations, the illumination light is projected directly onto the beam splitter 112 . In other implementations, a flat mirror 111 redirects the illumination light onto the beam splitter 112 .
[0247] In some implementations, a beam expander 110 (e.g., collimating lens) expands the waist of the illumination beam prior to the light reaching the beam splitter 112 , thereby providing an expanded illumination beam. In some implementations, the expanded illumination beam is projected directly onto the beam splitter 112 . In other implementations, a flat mirror 111 redirects the expanded illumination beam onto the beam splitter 112 .
[0248] The beam splitter 112 reflects the illumination beam (i.e., the unexpanded illumination beam or expanded illumination beam depending on whether a beam expander is used) to a micro lens array 104 . In some implementations, the beam splitter 112 transmits the illumination beam to a micro lens array 104 via a flat mirror 105 .
[0249] In some implementations, the beam splitter 112 separates light (e.g., reflects the illumination beams and allows the back-emitted light to pass therethrough) according to its wavelength, its polarization or without such distinctions. For example, a dichroic mirror or a polarizing cube associated with a quarter-wave, half-wave plate or a partially reflecting mirror can be used to achieve the desired effect.
[0250] In some implementations, the system includes a micro lens array 104 that focuses the illumination beam onto a sample 101 . The illumination beam is focused by each of the micro lens, producing an array of foci in the sample 101 . The micro lens array 104 focuses the collimated light into the sample 101 , forming an array of tight foci in which fluorescence will be excited (e.g., fluorescence from the fluorescence stained sample 101 ).
[0251] In some implementations, the micro lens array 104 includes plano-convex spherical lenses that focus the collimated beam of light. The plano-convex spherical lenses, in some implementations, are used with their curved surface facing the collimated beam in order to minimize aberrations (e.g., spherical aberrations).
[0252] The same micro lens array 104 allows the light emitted from the sample 101 (i.e., back-emitted light) as a result of the illumination to pass ultimately towards a detector array 108 . The light emitted by the sample 101 in response to the illumination, in some implementations, is collected by each of the micro lens. In this example, the collected light then propagates as individual collimated beams. In some implementations, the flat mirror 105 reflects the back-emitted light to the beam splitter 112 . In contrast to the illumination beam which the beam splitter 112 reflects, the beam splitter 112 transmits the back-emitted light.
[0253] After the back-emitted light passes through the beam splitter 112 , imaging optics 106 (e.g., field lens) focus the back-emitted light from the beam splitter 112 onto the detector 108 , thereby imaging the micro lens plane onto the detector plane. In some implementations, the back-emitted light from the beam splitter 112 is focused onto the detector 108 via an aperture stop 107 (e.g., pinhole). The aperture stop 107 spatially filters the light, thereby rejecting out-of-focus light.
[0254] In some implementations, the light originating from each individual micro lens is independently detected by dedicated sensors element of the detector array 108 . The sensitive elements of the detector array 108 can be any type of sensor sensitive to the light collected by the micromirrors, such as CMOS or CCD photodetectors, photodiodes, phototransistors, avalanche photodiodes, photoresistors, Golay cells, bolometer thermopiles or pyroelectric detectors.
[0255] Distances a and b as shown in FIG. 1B and the focal length of the relay optics can be chosen to arrange the magnification, therefore adapting the field of view such that the micro lens array 104 area maps onto the detector array 108 surface appropriately. This optical relay simultaneously allows spatial filtering for confocal detection when an aperture stop 107 is positioned in the Fourier plane of imaging optics 106 . In the example shown in FIG. 2B , the focal length of the relay optics is 100 mm, distance a is 32 mm, and distance b is 100 mm. Other focal lengths and distances may be used as well. For example, the focal length may be between 70-130 mm, distance a may be between 20-50 mm and distance b may be between 80-102 mm.
[0256] The relative motion between the sample 101 and the micro lens array 104 is achieved, in some implementations, with a scanning stage 103 that translates either the glass window on which the sample 101 sits or the micro lens array 104 (or both) in order to record variations of the sample signal with the changing position and to reconstruct an image therefrom. The camera 108 is recording the image plane situated at the back side of the micro lens array 104 . Therefore, every single micro lens signal is recorded simultaneously for a given position of the stage 103 . At a given position during the scanning process, multi-point information is recorded from the sample 101 and the relative position of all these point on the sample 101 is precisely known. By repeating this multi-point acquisition along the controlled scan pattern, the relative intensity variations recorded from each micromirror in the array in relation with their respective position on the sample 101 can be reconstructed by a computing device (e.g., a computing device integrated in the reader or separate from the reader). This provides the image of the sample 101 situated in the focal plane of the micro lens array 104 .
[0257] If the sample 101 is situated partially outside of the focal plane of the micro lens array 104 , the signal intensity will drop in the corresponding region of the array. It gives topographic information of the distance separating the sample 101 from the focal plane of the micro lens array 104 . A particularly valuable use of this topographic information is the compensation of a tilt angle between the sample plane and the micro lens plane. A computer may be used to control the reading instrument, including image reconstruction and/or displaying the image. In some implementations, control and reconstruction is embedded in the reading device.
[0258] In some implementations, the sample 101 is stained prior to processing using colored or fluorescent stains. For example, Proflavine, Acridine Orange, or other stains may be used. The staining procedure should remain simple to be executed in OR. For example, the staining procedure may comprise the steps: dip the tissue in a staining liquid, dip in a rinsing liquid, and then place the sample 101 on the glass above the micro lens array 104 for imaging. In certain embodiments, the sample 101 is placed in a sample holder 102 positioned above the micro lens array 104 .
[0259] FIGS. 2A through 2C are photographs of an example in-operating-theatre pathology system in accordance with an embodiment of the disclosed technology. This example system uses a micro lens array to perform large-field high resolution microscopy and/or micro-projection of fresh, thick tissue in an operating theatre for pathology assessment. The illumination light is provided by a light source 209 (e.g., laser) and expanded by a collimating lens 210 (e.g., a beam expander). The collimated light is then directed onto a beam splitter 212 by a flat mirror 211 .
[0260] The beam splitter 212 reflects the illumination beam (i.e., the unexpanded illumination beam or expanded illumination beam depending on whether a beam expander is used) to a micro lens array via a flat mirror 205 . In this example, the beam splitter 212 is a dichroic mirror that separates light according to its wavelength (e.g., reflects the illumination beams and allows the collected fluorescence light to pass therethrough).
[0261] A micro lens array (underneath the scanning stage 103 in this example) focuses the illumination beam onto a sample (not shown) on the sample holder 220 . The illumination beam is focused by each of the micro lens, producing an array of foci in the sample. The same micro lens array allows the light emitted from the sample (i.e., back-emitted light) as a result of the illumination to pass ultimately towards a detector array 208 (e.g., camera). The light emitted by the sample in response to the illumination is collected by each of the micro lens. In this example, the collected light then propagates as individual collimated beams.
[0262] In some implementations, the flat mirror 205 reflects the back-emitted light to the beam splitter 212 . In contrast to the illumination beam which the beam splitter 212 reflects, the beam splitter 212 transmits the back-emitted light. After the back-emitted light passes through the beam splitter 212 , a field lens 206 focuses the back-emitted light from the beam splitter 212 onto the detector 208 via an aperture stop 207 , thereby imaging the micro lens plane onto the detector plane. The aperture stop 207 spatially filters the light, thereby rejecting out-of-focus light.
[0263] In this example, the relative motion between the sample and the micro lens array is achieved with a scanning stage 203 (e.g., 3×20×20 cm) that translates in order to record variations of the sample signal with the changing position and to reconstruct an image therefrom. At a given position during the scanning process, the global surface topography of the sample can be reconstructed by comparing the relative intensity variations recorded from each micromirror in array. A particularly valuable use of this topographic information is the compensation of a tilt angle between the sample plane and the micromirror plane. In this example, a computer (not shown) is used to control the reading instrument, including image reconstruction and/or displaying the image.
[0264] The system described in this example may be used for the observation of thick fresh tissue at a cellular level during surgery in order to provide pathology assistance to ongoing surgery. The sample may be processed using the disclosed technology in less than 10 minutes (e.g., less than 5 mins) using the system shown in FIGS. 2A-C in part because the sample does not need to be mechanically sliced as the disclosed microscopy may be used directly on fresh thick tissue (e.g., using optical slicing, a non-destructive method). Further, the pure technical speed of reading is improved and this approach preserves the sample such that it is available for definitive assessment (contrary of FSA). Additionally, images can be shared electronically which allows direct connection between the pathology and the surgery.
[0265] In this example, the sample holder 220 includes a sample holder frame 222 that is attached to the scanning stage 203 . Specifically, in this example, the sample holder frame 222 is screwed to the scanning stage 203 , although other attachment systems may be used. The sample holder frame 222 has a this transparent window 224 onto which the tissue sample is deposited for imaging. In this example, the transparent window 224 is glass.
[0266] FIG. 3 is an illustration of a method 300 for imaging thick fresh tissue in the operating theatre. A fresh tissue sample (e.g., 101 ) is positioned on the glass window from the sample holder (e.g., 102 ) (e.g., after fluorescent labeling process is applied to the sample 101 ) ( 302 ). In some implementations, the holder (e.g., 102 ) is a metallic body (for cleaning or disinfection) with an opening window (e.g., 40×20 mm). The holder may be sealed at the bottom by a glass window for the instrument to be protected from liquid. In some implementations, the thin glass window secures an optical interface (transparent and flat) between the sample and the micro-optics chip. An example holder 220 , window, and scanning stage 203 is shown in FIG. 2C .
[0267] The holder, in some implementations, is designed specifically for this application. The tissue may be put in contact with a thin glass slide (e.g., 50-100 μm thick) and gently pressed against the glass slide to secure the contact over the area to be imaged. In some implementations, the holder is sealed for specific cases where the tissue needs to be immersed in a liquid for clinical reasons. In some implementations, the holder is used for the staining procedure. In other implementations, the holder is a metallic plate with a hole in its center and a glued thin glass slide on the bottom.
[0268] In some implementations, the holder (e.g., 102 ) is screwed on the scanning stage (e.g., 103 ) ( 304 ). The stage, in some implementations, is a three-axis high precision positioning stage. The stage is used to bring the glass window in close proximity (e.g., <100 um) to the chip (e.g., 104 ). Then, the sample scan be imaged using the disclosed technology ( 306 ).
[0269] The disclosed scanning microscopy allows for fast confocal imaging over large area. For example, the disclosed scanning microscopy can be designed with a larger micro lens array to increase the field of view. In comparison, confocal microscope traditionally uses a configuration with a microscope objective and beam scanning. The field of view is limited (500 μm-1 mm) by the objective and highly dependent on the chosen magnification. The beam scanning increases the acquisition time for each image compare to standard microscopy. Consequently, to cover a 20 mm field of view for instance, a standard motorized confocal microscope would need to aggregate 400 to 1600 images in this example. The disclosed technology increases the speed, flexibility of use, robustness, ergonomics and compactness thereby achieving an in-operating—room scanning microscopy for imaging thick fresh tissue. The parallel approach described herein allows the disclosed technology to cover the field of view (e.g., of 20 mm) with a scan range corresponding to the pitch of the array (e.g., of 0.25 mm) while a sequential approach forces the scan to cover the entire field of view ( 2 orders of magnitude larger) which limits the speed, flexibility of use robustness, ergonomics and compactness.
[0270] In some implementations, the position of components in the system are fixed while only the sample is displaced (e.g., and in some implementations the scanning stage 103 ) by a translation fixture such that the sample may be scanned. In other implementations, the position of the sample relative to the system is fixed during scanning and the optical chip (e.g., micro lens array) is moved such that the sample is scanned. In this implementation, the image onto the detector will be moving, therefore the detected signal is processed to compensate for this movement. Further, in some implementations, the movement of the system during scanning is monitored to adjust the detected signal appropriately. Utilizing a moving optical chip rather than moving the sample itself while scanning eliminates any mobile component for the user to interact with and allows for a more robust external casing for cleaning and sterilization.
[0271] FIGS. 4A-G are illustrations of an example system for holding a sample. In this implementation, the sample holder is fixed and a mechanical translation stage moves the optical chip (e.g., micro lens array) relative to the rest of the system. In the example shown in FIGS. 4A-G , the main structure is supported by a base 402 (e.g., 300 mm×300 mm) and additional pillars 404 a - c (collectively 404 , post 404 d not shown) (e.g., 100 mm tall). The global volume in this example is therefore 300 mm×300 mm×100 mm. Height may vary considering the height of the holding structure 406 for the sample (in purple here). Length may be increased (e.g., such that the camera is within the dimensions of the translation stage). Various dimensions may be used for the base 402 (e.g., width of 50 mm, 100 mm, 150 mm, 200 mm, or 250 mm, and lengths of 50 mm, 100 mm, 150 mm, 200 mm, or 250 mm, all values+/−50 mm) and the pillars 404 (e.g., 25 mm, 50 mm, or 75 mm, all values+/−25 mm).
[0272] The optical path is below the base 402 , the scanning stage 408 is fixed on top of the base 402 . The mechanical structure (e.g., 408 and 406 ) to hold the sample allows adjusting height and tilt of the sample relative to the stage and optical path. An optical window 410 (e.g., glass window) is located in the holding structure 406 such that a sample may be placed on the optical window 410 and a micro lens array positioned below the optical window 410 can focus light onto the sample and collect back-emitted light (e.g., fluorescence excited by the focused light) as described above. In some implementations, metal bars as shown in FIGS. 4A-G are provided such that the components of the system may be adjusted. In some implementations, the components are adjusted during manufacturing such that no further adjustments are necessary in the field. In other implementation, most of the adjustments are set during manufacturing, however, select fine adjustments may be made in the field.
[0273] This example system uses a micro lens arrays to perform large-field high resolution microscopy and/or micro-projection of fresh, thick tissue in an operating theatre for pathology assessment. The illumination light is provided by a light source and expanded by a collimating lens (e.g., a beam expander).
[0274] The beam splitter 414 reflects the illumination beam (i.e., the unexpanded illumination beam or expanded illumination beam depending on whether a beam expander is used) to a micro lens array via a flat mirror 416 . In this example, the beam splitter 414 is dichroic mirror that separates light according to its wavelength (e.g., reflects the illumination beams and allows the collected fluorescence light to pass therethrough).
[0275] A micro lens array focuses the illumination beam onto a sample (not shown) on the sample holder. The illumination beam is focused by each of the micro lens, producing an array of foci in the sample. The same micro lens array allows the light emitted from the sample (i.e., back-emitted light) as a result of the illumination to pass ultimately towards a detector array 412 . The light emitted by the sample in response to the illumination is collected by each of the micro lens. In this example, the collected light then propagates as individual collimated beams.
[0276] In some implementations, the flat mirror 416 reflects the back-emitted light to the beam splitter 414 . In contrast to the illumination beam which the beam splitter 414 reflects, the beam splitter 414 transmits the back-emitted light. After the back-emitted light passes through the beam splitter 414 , a field lens focuses the back-emitted light from the beam splitter 414 onto the detector 412 via an aperture stop, thereby imaging the micro lens plane onto the detector plane. The aperture stop spatially filters the light, thereby rejecting out-of-focus light.
[0277] FIG. 5 is an illustration of an example sample holder system 500 . In this example, the sample holder 406 is a metallic part including a thin optical window 410 , which can be fixed on the system 500 . This illustrates an “all combined” solution where the glass window tilt and height relative to the scanning stage/optical chip (not shown) can be adjusted as a manufacturing setup, assuring that any sample deposited on the optical window 410 will be correctly positioned regarding the microscopy system to be imaged.
[0278] For sterility constraints due to dedicated application in clinical use (e.g., operating theater), it may be preferable to include a single use element (e.g., a disposable element). FIG. 6A shows an example of such a single use element 600 that can be inserted in the system for each use. The sample holder may be used as an adaptive element to secure the single use element 600 on the system at the right position for imaging. The single use element 600 , in some implementations, includes a thin glass window 602 through which the imaging takes place. In some implementations, the element 600 includes a cover/lid 604 to protect the glass window 402 and enclose the sample once inserted into the body 606 . The element 600 provides axial positioning repeatability (e.g., mechanical tolerancing, in some implementations, is better than 10 μm (e.g., 1 to 10 μm)). In some implementations, the element 600 is stackable with other similar elements. For example, the body 606 can include feet 608 a - c (foot 608 d not shown). Additionally, the body 606 can include storage guides 610 a - d that allow elements 600 to stack on top of each other easily. The storage guides 610 a - d are spaced inside of corresponding feet 608 a - d from another element 600 such that the guides 610 a - d laterally secure elements 600 when they are stacked on one another. In some implementations, the element 600 includes prominent feet 608 a - c (foot 608 d not shown) to preserve optical interface when, for example, putting the element 600 on a dirty or damaging surface.
[0279] FIGS. 6B and 6C illustrate an additional sample holder 660 that can be used with an in-operating-theatre pathology system 662 (e.g., such as a system described herein). This example shows a system protected from environment (dust, liquid) by an external enclosure offering an opening window for imaging protected by a transparent material (such as glass). Such a system can be used for imaging without the sample holder 660 (e.g., disposable part), by directly placing the sample on the transparent window 654 .
[0280] In the example shown in FIGS. 6B and 6C , the system 662 is a closed system and the sample holder 660 rests/sits on top of a plate 654 (e.g., transparent; e.g., made of glass or a polymer) that itself is attached to the body 650 of the system. The optical array 652 is housed within the body 650 . For the purpose of this illustration, the entire body and system is not shown. As shown in FIG. 6C , even when the sample holder 660 is removed the system 662 is closed and the optical array 652 is protected from the environment. However, such a system requires multiple, stacked up interfaces (e.g., 654 and 660 ) and thus these interfaces must be thin and/or be optically transparent. In certain embodiments, the sample holder 660 is rigid, such as a polymer or glass. In other embodiments, the sample holder is flexible, such as a pellicle or film.
[0281] FIGS. 6D and 6E illustrate an additional sample holder 670 that can be use with an in-operating-theatre pathology system 672 (e.g., such as a system described herein). In this example, the system 672 is an open system as shown in FIG. 6E and the sample holder 670 (e.g., holder) rests, sits, or is attached to the body 650 of the system. The system is closed by a removable part 670 . The optical array 652 is housed within the body 650 . For the purpose of this illustration, the entire body and system is not shown. As shown in FIG. 6E , even when the sample holder 670 is removed the system 672 is open and the optical array 652 is not protected from the environment. However, the optical interface is thinner and/or has improved optical transparency as the only interface is on the removable part 670 —there is no additional plate 654 as shown in FIGS. 6B and 6C .
[0282] The system shown in FIGS. 6D and 6E can includes a mounting system suited to accommodate the sample holder 670 (e.g., disposable sample holder) during an operation. In a surgical operation, for example, the tissue sample is placed on the sample holder 670 remotely from the system and then is brought to the system using the sample holder. In this example, the sample holder act as sample handler as well. The mounting system, in certain embodiments, has its own optical interface which is rigid to support tissue sample/specimen.
[0283] The mounting system for the sample holder (e.g., such as the sample holder shown in FIGS. 6A through 6E ) can be one of a variety of systems. For example, the mounting system for the sample holder can require no fixation—instead, the sample holder is simply deposited (e.g., placed) on the top side of the instrument in the appropriate position such that the sample holder sits or rests on top of the instrument. In other embodiments, the sample holder can be secured using an adhesive, mechanical fixation (e.g., screws, clamp or any locking device), or one or more magnets to hold the disposable in position.
[0284] FIGS. 6F through 6J illustrates one example for mounting a sample holder 690 to a pathology system. In this example, only the optical chip 652 portion of the pathology system is shown. In certain embodiments, a support base 680 can be mounted on the pathology system. The support base can include a mount 682 with one or more protrusions 684 extending from the mount 682 . In the example shown in FIG. 6F , the support base 680 includes two protrusions 684 . The mount 682 is hollow on the inside and the support base 680 has a corresponding opening therein such that an optical chip 652 can scan a sample through the support base 680 . This embodiment includes a second piece, referred to as a removable sample holder 690 . The removable sample holder 690 includes a transparent window 692 through which the optical chip 652 can image a sample (e.g., the optical sensor is on one side of the transparent window 692 and the sample is on the opposite side of the transparent window 692 ). The removable sample holder 690 includes one or more interior protrusions 694 . In this example, the removable sample holder 690 includes two interior protrusions 694 . The width (labeled as 696 in FIG. 61 ) of the vertical walls of the removable sample holder (excluding the interior protrusion(s) 694 ) is such that it can slide over the mount 682 when the protrusion(s) 684 and interior protrusion ( 694 ) are not aligned. Once the removable sample holder 694 is fully applied to the mount 682 , the removable sample holder 694 can be twisted (e.g., clockwise in this example) such that the protrusion(s) 684 and the interior protrusion(s) 694 are engaged with each other. This securely mates the removable sample holder 694 to the support base 680 such that the optical sensor 652 can image a sample placed on the transparent window 692 in the removable sample holder 694 .
[0285] FIG. 7 is an illustration of an example kinematic structure that is used, in some implementations, for adjusting both height and tilt of the glass window (e.g., by moving the scanning stage) relative to the optical chip and corresponding optical path. In certain embodiments, the kinematic structure has three feet (although different numbers of feet may be used such as 2, 4, or 5) with adjustable height (micrometric screw—see FIG. 7 kinematic base 700 holding the frame on which can be screwed the sample holder). The purpose of this kinematic base 700 is to adjust both height and tilt of the glass window (e.g., glass window 604 in FIG. 6 or optical window 410 in FIG. 4A ) relative to the optical chip (e.g., optical chip 902 in FIG. 9 or micro lens array 104 in FIG. 1A ) and corresponding optical path. The two surfaces (e.g., the glass window and the optical chip), in some implementations, have an area of about 20 mm by 20 mm (other dimensions may be used, such as a width of 10-60 mm and a length of 10-60 mm) and will be positioned at a close distance less than 500 μm (e.g., less than 400 μm, less than 300 μm, less than 200 μm, and/or greater than 100 μm, greater than 200, and/or between 100-200 μm, 200-300 μm, 300-400 μm, or 400-500 μm), which may require adjustment of these settings (e.g., during manufacturing). Additionally, the microscope performances are increased when all surfaces are positioned normal to the optical axis of the system. In the example shown in FIG. 7 , the kinematic base 700 includes a magnet 706 (e.g., a pair of magnets may be used—a magnet in the seat 704 that is magnetically attracted to a magnet in the head 702 ) that exerts a force that aligns and maintains the head 702 in position on the seat 704 . The height and tilt is defined by the distance between head 702 and seat 704 , which is controlled with the adjuster screw 708 (e.g., ¼″-100). In an example that uses three kinematic feet, one kinematic foot may be screwed in to increase the distance between the respective seat 704 and head 702 and modify the global tilt and height of the platform standing on these feet. In this example, if all three kinematic feet are screwed with the same number of rotations, all feet height change the same way, which gives a pure platform height change. Otherwise, if the kinematic feet are not all screwed with the same number of rotations, the tilt is modified.
[0286] FIG. 8 is an illustration of a camera 802 and pinhole 804 (e.g., aperture) assembly. The axial distance between the pinhole disk 804 (i.e., aperture stop) and the detector 802 (e.g., camera sensor) is determined from optics equations and is not extremely sensitive in terms of tolerances so it can be determined and mechanically set without the need for fine adjustment. Fine position, however, in certain embodiments, is required for the lateral position of the pinhole in the disk 804 . In certain embodiments, this requirement is provided using the system shown in FIG. 8 . In FIG. 8 , the position of the aperture stop relative to the optical axis is adjusted with an XY translating stage 806 , while the camera 802 has a fixed position relative to the optical axis. The aperture stop 804 (pinhole) is used to filter the collected light on a confocal manner before the light signal reaches the camera 802 sensor. The position of this aperture 804 is of importance as it selects the points of origin of the light collected in the sample. Adjusting this pinhole (i.e., small hole in the disk 804 ) position corresponds to adjusting the position of the grid of collected focal points in the sample. For maximizing the performance of the confocal microscope this collection grid must be aligned (match) with the illumination grid. This aperture 804 positioning is critical for correctly setting up the system.
[0287] Also illustrated in FIG. 8 is the optical interface clamp 808 (e.g., 1108 shown in FIG. 11D ). The optical interface clamp 808 is a ring-shaped part (although other shapes can be used) that maintains the optical interface 810 (e.g., transparent window) in place against the optical interface mount (e.g., 1106 in FIG. 11B ) and that seals the device with O-ring gaskets 812 . In certain embodiments, the optical interface clamp 1108 is designed to be in contact with the specimen while preventing the optical interface mount 1106 from contacting the specimen during use.
[0288] FIG. 9 is an illustration of an example optical chip scanning system 900 that may be used with the optical system described above. In this example, the optical chip 902 is moved by a scanning system 904 . In the example shown in FIG. 9 , the scanning system 904 and optical chip 902 are in an interior environment 950 of the instrument (e.g., fully or partially enclosed in the instrument) such that the optical chip 902 is protected from both the sample 906 and, in some implementations, outside environment 960 (i.e., outside of housing 910 ) by an optical (e.g., glass) window 908 . In some implementations, this allows for faster scan rates since the mass in motion is very small—in some implementations, the optical chip 902 weights from 0.5 to 2 grams (e.g., 0.9 to 1.1 grams, or 1 gram).
[0289] FIGS. 10A-D illustrate of an example system 1000 for in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment. In this example, a laser fiber 1002 (e.g., single mode optical fiber) provides laser light via a laser fiber output 1004 . The laser light is collimated by a collimating lens 1006 and then reflected off a dichroic beam splitter 1008 toward a beam steering mirror 1010 (e.g., at 45 degrees relative to the path of the collimated light). The beam steering mirror 1010 reflects the collimated laser beam upwards towards the optical chip 1012 . The optical chip (e.g., micro lens array) focuses the collimated light into the sample, forming an array of tight foci in which fluorescence will be excited (e.g., fluorescence from the fluorescence stained sample).
[0290] In some implementations, as illustrated in FIG. 10C , the micro lens array includes plano-convex spherical lenses that focus the collimated beam of light. The plano-convex spherical lenses, in some implementations, are used with their curved surface facing the collimated beam in order to minimize aberrations (e.g., spherical aberrations). However, in this implementation, the focal plane may not penetrate deep into the sample (e.g., only a 10-40 microns) since the focused light goes through the entire micro lens array substrate thickness, the separating medium (e.g., air), and the coverslip 1052 (e.g., glass).
[0291] In some implementations, the plano-convex spherical lenses are used with their curved surface facing the sample as shown in FIG. 10E . This allows the focal plane 1056 to penetrate much deeper into the sample (e.g., 100-500 microns). The optical elements (e.g., micro lenses 1014 a - 1014 k ) also collect and collimate fluorescence emission from the sample. The beam steering mirror 1010 reflects the collimated fluorescence emission horizontally toward the imaging lens 1016 . The imaging lens 1016 focuses the collimated fluorescence emission from each micro lens in the micro lens array 1012 through the common pinhole 1018 and forms an image of the micro lens array on the camera sensor 1020 . In terms of imaging, the camera sensor 1020 and the micro lens array 1012 form a pair of conjugate planes—the micro lens array 1012 is imaged on the camera sensor 1020 by the imaging lens 1016 .
[0292] FIG. 10E illustrates an example hyperbolic shape of the micro lenses 1014 . FIG. 10F illustrates an example system exciting the fluorescence in the sample with lens 1014 a - k facing the sample. FIG. 10G illustrates the back-emitted light emitted by the excited fluorescence.
[0293] FIG. 10E illustrates an inverted configuration compared to FIG. 10C . This configuration can provide a longer working distance at a cost of poorer optical performance. This drawback can be overcome by using optical elements with non-spherical curvature, such as conical curvature. In certain embodiments, the curvature of the optical elements is conical, hyperbolic, or parabolic, rather than spherical. The curvature can be described by the factor of conic constant k.
[0294] In geometry, the conic constant k is a quantity describing conic sections. For negative k, the conic constant is given by the following equation:
[0000] k=−e 2 ,
[0295] where e is the eccentricity of the conic section. The equation for a conic section with apex at the origin and tangent to the y axis is:
[0000] y 2 −2 Rx +( k+ 1) x 2 =0
[0296] where k is the conic constant and R is the radius of curvature at x=0. This formulation is used in geometric optics to specify oblate elliptical (k>0), spherical (k=0), prolate elliptical (0>k>−1), parabolic (k=−1), and hyperbolic (k<−1) lens and mirror surfaces. When the paraxial approximation is valid, the optical surface can be treated as a spherical surface with the same radius.
[0297] In certain embodiments, the conic constant k is a negative value with absolute value greater or equal to 0.5. A typical range for k is −10<k<−0.8. In certain embodiments, the range for k is −3<k<−0.9.
[0298] For example, an optical elements having radius of curvature of 195 um plus or minus 5 μm can be used. For example, optical elements having a radius of curvature from 190 μm to 200 μm, with a conicity k=−2.0 provides the following desired range of property values: Strehl ratio: 0.9<S<1, glass thickness for the sample interface 1052 : 300 um+/−100 um; air gap 1057 between optical chip 1051 and glass interface 1052 from 150+/−50 um; and/or depth of imaging plane 1056 inside the sample 1055 of 50 um+/−50 um. Other combinations of radius of curvature and/or conicities can be chosen to produce optical elements providing properties within these desired ranges for performing the functions described herein.
[0299] The shape of the optical elements may vary. For example, in certain embodiments, each micro optical element has a conical shaped surface. In certain embodiments, each micro optical element has a hyperbolic shaped surface. In certain embodiments, the curved surface of each micro optical element has a conic constant k from −1.8 to −2.2 (e.g., −2). In certain embodiments, each micro optical element has a Strehl ratio greater than or equal to 0.8. Furthermore, in certain embodiments, each micro optical element has a spot size from 0.2 μm to 5 μm, 0.2 μm to 1 μm, 0.3 μm to 0.6 μm, 0.4 μm to 0.5 μm, greater than or equal to 0.2, and less than or equal to 5 μm. The system can have a free working distance (i.e., a distance from the tip of the micro optical elements to a focal plane of the micro optical element array) from 80 μm to 450 μm, 150 μm to 350 μm, or 250 μm to 300 μm. Additionally, the resulting focal plane of the micro optical element array can be from 10 μm to 200 μm, 20 μm to 150 μm, or 50 μm to 100 μm above the transparent window (i.e., the depth of the focal plane into a sample being imaged).
[0300] As shown in FIG. 10E , the curved surfaces of the lenses 1014 are facing the glass interface 1052 with the sample 1055 thereon. The curvature is chosen to optimize optical performance and working distance. The quality criteria for optical performance is to minimize optical aberration at the focal plane. A way of evaluating this quality is the Strehl ratio. The Strehl ration has a value between zero and one, an unaberrated optical system attaining the value of unity. Compared to FIG. 10C , the inverted configuration of FIG. 10E increases the working distance which allows the use of a thicker glass interface 1052 and improves safety in the operating room.
[0301] In certain embodiments, as shown in FIG. 10E , the areas (e.g., flat areas) in between micro-lenses 1014 are covered by an absorptive and/or reflective layer 1054 . This layer 1054 can be, for example, a chromium layer, aluminum layer, or dielectric mirror layer. The purpose of this layer is to prevent or minimize the amount of illumination light transmitted by the optical chip that would travel outside of the system and possibly reach the eye of the operator. This can improve the safety of the system. The flat surface is covered because the illumination beam is collimated and therefore can travel long distance if not deviated by the curved surface. For the part of the beam focused by the curved surface, the beam is highly diverging at the distance of operator eyes which, when correctly designed, drastically diminishes the power received to a safe level.
[0302] The system disclosed herein provides several benefits. For example, alignment of the micro lens array axis with the scanning stage axis is robust. The micro lens array may be aligned by hand within approximately 5 degrees and a small rotation can be compensated for by software with a proper calibration routine for allocation of camera pixels to the optical element, offsetting, and/or rotating tiles during image reconstruction.
[0303] Misalignment between the micro lens array axis with camera axis can be compensated for by software, with a pixel allocation layer for arbitrary attribution of the camera pixels to the optical element. Similarly, alignment of the scanning stage axis with the camera axis in the embodiment in which the micro lens array is moved for scanning can be compensated for by software with a proper calibration routine and subsequent allocation of camera pixels to optical element.
[0304] Lateral alignment of confocal pinhole with the imaging lens must be precise. The pinhole will be relatively small (e.g., 75-400 μm) and must be precisely aligned in the imaging lens focal plane. This may be accomplished, for example, using an XY micrometer. The axial alignment of the confocal pinhole with the imaging lens is also important. For relatively long focal length of the imaging lens (e.g., f>50 mm), alignment in Z direction is not as critical and can be accomplished within 1 mm or better without precise positioning system.
[0305] The axial positioning of the imaging lens from the micro lens array plane determines the magnification of the imaging system. In some implementations, this does not need to be precisely adjusted.
[0306] The axial positioning of the imaging lens from the camera sensor plane determines how well focused the image of the micro lens array is on the camera sensor. In some implementations, considering the effective resolution of the imaging system through the confocal pinhole, manual adjustment of the lens position (e.g., to within 1 mm) on the cage system is sufficient for the long focal length of the imaging lens (e.g., f>50 mm). Further, for a long focal length imaging lens (e.g., f>50 mm), the axial positioning of pinhole from camera sensor plane, in some implementations, must be within less than or equal to a millimeter. For long focal length of the collimating lens (e.g., f>50 mm), which are needed to generate large beam diameter to illuminate the full micro lens array, manual adjustment of the axial positioning of the fiber collimation lens (e.g., to 1 mm) on the cage system is sufficient.
[0307] For a collimation of fibered light source, the lateral position of the fiber collimation lens is critical. A XY micrometer, for example, may be used to center optical fiber on collimating lens optical axis.
[0308] In scanning microscopy, the resolution of the image may depend on the position of the reader while scanning the sample. In some implementations, the image is reconstructed based on the relation between the position of the reader relative to the sample and the corresponding signal measured by the detector. Image quality may be deteriorated by imprecise position measurement. In some implementations, positioning feedback is accomplished using a closed loop positioning system to compensate for non-linearity, hysteresis and drift issues.
[0309] In some implementations, focusing elements may be used for positioning feedback. For example, one or more micro lenses can be used to record the image of a local known pattern, thereby providing a two or three-dimensional position feedback. In some implementations, the achromatic property of the lens allows for using a different wavelength for the feedback than the one used to image the sample. This allows image information to be easily separated from the positioning information with a dichroic beam splitter.
[0310] As described above in relation to FIG. 4 and FIG. 5 , the disclosed technology, in certain embodiments, includes a sample holder. In some embodiments, the disclosed technology also includes a kinematic support. In certain embodiments, the specimen imaging interface designates the part of the assembly on which the specimen is imaged.
[0311] FIGS. 11A through 11G illustrate an example implementation of a specimen imaging area in accordance with an embodiment of the disclosed technology. In this example, the design is optimized to take into account requirements for use in hospital and ergonomic integration in the operating room workflow. The system is designed to be robust to fluid leakage. In particular, it includes a containment ring sealed on the glass window to prevent liquid related to the sample from being in contact with the rest of the device (e.g., for safety—hygiene). Additionally, the design minimizes the risk of liquid flowing inside the device during the cleaning of the device (efficacy).
[0312] FIGS. 11A and 11B illustrate an example specimen imaging interface on the microscopy instrument. FIG. 11A illustrates the specimen imaging interface 1100 connected to the rest of the imaging system 1190 whereas FIG. 11B illustrates the specimen imaging interface 1100 alone. The optical interface 1102 is the surface on which the specimen lies. It protects the optical chip 1104 and the rest of the instrument from the environment (dust, liquids, etc. including the specimen itself). It is compatible with the imaging process (transparency, planarity, etc.).
[0313] The optical interface mount 1106 is the mechanical support for the optical interface 1102 . The optical interface clamp 1108 is the ring-shaped part (although other shapes can be used) that maintains the optical interface 1102 (e.g., transparent window) in place against the optical interface mount 1106 . The optical interface clamp 1108 seals the device with O-ring gaskets (not shown). In certain embodiments, the optical interface clamp 1108 is designed to be in contact with the specimen while preventing the optical interface mount 1106 from contacting the specimen during use.
[0314] The kinematic blocks 1112 serve to mount the precision adjusters 1114 which form the basis of the kinematic system. In certain embodiments, the kinematic system is a three-point kinematic system that uses only three adjusters for kinematic positioning of the optical interface mount 1106 . In other embodiments, the kinematic system is a four-point kinematic system that uses four adjusters. Other variations are possible as well. Additionally, the kinematic blocks 1112 serve to mount the protective plates that delimit the perimeter of the specimen imaging interface, and protect sensitive components located under the optical interface mount 1106 from the outside environment. The top of the adjusters 1114 on each kinematic block 1112 contact at least a portion of a respective groove 1154 a - d (collectively 1154 ) on the bottom side of the optical interface mount 1106 such that the grooves 1154 on the bottom side of the optical interface mount 1106 each sit on a respective kinematic block 1112 as shown in FIGS. 11E and 11F .
[0315] The base plate/frame refers to the mechanical backbone of the instrument on which all the components and modules are fixed. The baseplate is not part of the specimen imaging interface.
[0316] As illustrated in FIG. 11C , the entire optical interface mount assembly (with optical interface 1102 , optical interface clamp 1108 , etc.) can be magnetically maintained in position on the kinematic system and can be removed easily. Removing the optical interface mount 1106 exposes sensitive components (notably the optical chip 1104 and the scanning stage) to the “outside” environment (dust, liquid spill, mechanical impact, etc.) and allows removal of the optical interface 1102 itself. In this example, as shown in FIG. 11C , the optical interface clamp 1108 is fastened by five screws and can thus be removed relatively easily to allow replacement of the optical interface 1102 or the O-ring seals. Other attachment systems or numbers of screws can be used to fasten the optical interface clamp 1108 to the system.
[0317] The optical interface mount 1106 sits on the precision adjusters 1114 (e.g., three precision adjusters 1114 ) of the kinematic system. The position of the optical interface mount 1106 can be maintained by magnets. The optical interface mount 1106 can thus be easily removed from the microscopy instrument. In the example shown in FIG. 11A through 11C , the optical interface mount 1106 is machined from a 200 mm×200 mm×8 mm aluminum plate and has a anodized finish.
[0318] In certain embodiments, the optical interface clamp 1108 has two hidden grooves that accommodate O-rings to seal off the device by (i) preventing liquids inside the ring 1108 from flowing into the device, and (ii) preventing liquid spilled outside the ring 1108 from flowing into the device. FIG. 11D illustrates two examples of optical interface clamps 1108 . In both of these examples, the optical interface clamp 1108 is fastened to the optical interface mount 1106 by hardware 1010 , such as countersunk flat head screws. In this example, the optical interface clamp 1108 and optical interface 1102 can be disposable or sterilizable. The optical interface clamp 1108 can secure the optical interface 1102 onto the system and seal against the optical interface 1102 and/or optical interface mount 1106 to prevent liquid leakage from the sample into the system.
[0319] FIGS. 11E through 11G illustrate an example of a spill-proof optical interface mount 1106 . Specifically, FIG. 11E is a top view of the optical interface mount 1106 showing the groove 1152 a - d (collectively groove 1152 ) in the bottom of the optical interface mount 1106 . FIG. 11F is a bottom view of the example spill-proof optical interface mount 1106 and FIG. 11G is a cross-sectional view of the example spill-proof optical interface mount 1106 along section A-A as shown in FIG. 11F . It is important, in certain embodiments, to prevent liquid spilled on the optical interface mount 1106 from flowing into the device. In this example, the bottom surface of the optical interface mount 1106 near the perimeter of the optical interface mount 1006 is has a groove 1152 (e.g., a groove with a rectangular, circular, oval, triangular, or square cross-section) that prevents droplets on the bottom surface from migrating inwards). If liquid drains off the edge of the top surface of the interface mount 1106 , it will fall down when it reaches the groove 1152 . This prevents or reduces the likelihood that the liquid enters the system under the optical interface mount 1106 .
[0320] FIG. 12A is an illustration of an example mobile cart with an imaging device thereon for providing in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment and FIG. 12B is a photograph of an example of such a mobile cart.
[0321] As shown in FIG. 12A , an example mobile cart 1200 may include a plurality (e.g., three or four) wheels 1209 on which the cart can be rolled. Other transportation systems may be used as well, such as tracks. The cart 1200 can be motorized or can be pulled/pushed by a user. The mobile cart includes a microscopy instrument 1210 , such as the instrument described herein, with a specimen imaging interface 1212 . In certain embodiments, the mobile cart 1200 includes a display monitor 1205 , a keyboard, 1206 , and a user interaction device 1207 (e.g., touch pad, touch screen on the display monitor 1205 , and/or computer mouse). The microscopy instrument 1210 can be connected to the display monitor 1205 such that scans/images of the specimen in the imaging area 1213 can be shown on the display monitor 1206 .
[0322] In certain embodiments, the cart includes handles, such as a front side handle 1211 and backside handles 1210 . The mobile cart 1200 can be equipped with a power switch 1201 (e.g., on/off switch) that is used to control power to equipment on the mobile cart 1200 . A power cable 1203 can be used to connect the mobile cart 1200 to a power source. In certain embodiments, the cart 1200 has a battery for self-sufficient use. The mobile cart 1200 can also include an equipotential bonding cable 1204 . The mobile cart 1200 can include one or more drawers 1208 (e.g., two drawers as shown in FIG. 12A ). The mobile cart 1200 can also include a cable winder 1202 around which one or more cables can be wound for storage during, before, or after use.
[0323] Experiments
[0324] Several experiments were performed to identify sufficient optical chip designs. In these experiments, optical chip designs were tested using different curvature lenses and different lens orientations. Specifically, the lens orientation varied from facing the illumination beam and facing the sample. The shape of the lenses varied from spherical to conical. Table 1 summarizes the test results by showing the main quality criteria evaluated along with the tested optical chip configurations and curvature shapes.
[0000]
TABLE 1
Optical Chip Design
1
2
3
Configuration
A
B
Curvature shape
Spherical
Conical (k = −2.0)
Performance criteria
fWD (um)
110
420
400
Spot size
2.1
11.6
0.34
RMS radius (um)
Performance for
Lower
Poor
High
microscopy
performance;
Performance;
Performance;
lower
out of
best
specification
specification
specification
Strehl ratio
<0.8
<0.8
0.91
level of
aberrated
aberrated
diffraction
aberration
optics
optics
limited
[0325] In these experiments, three optical chips designs were tested. The optical chip design of configuration A utilized lenses having a curvature facing the illumination beam. In contrast, the optical chip designs of configuration B utilized lenses having a curvature facing the sample. Optical chip designs 1 and 2 utilized spherical lenses as described above while chip design 3 utilized conical lenses as described above. The optimization aims to maximize the free working distance (fWD) while minimizing the spot radius and maintaining high performance microscopy. The spot radius is representative of the smallest detail that can be distinguished by the optical system, hence it relates to resolution. Thus, optimization aims at minimizing the spot radius value. The Strehl ratio is a way of quantifying the level of aberration. Being diffraction limited means that the system reaches the physical limits and can therefore be considered as a non-aberrated optical system.
[0326] FIG. 13 is a screenshot of a microscopy image of fresh tissue acquired using the disclosed technology, specifically using optical chip design 3 from Table 1. The screenshot shows the Graphical User Interface (GUI), the alignment marks (e.g. square, triangle and round) to recognize tissue orientation, and the image obtained with a fresh porcine eyelid tissue deposited on the scanner instrument. The disclosed technology was used to capture an image that represents a digital slice of the fresh tissue—thus, allowing an image of a cross section of the tissue to be taken without actually slicing the tissue.
[0327] FIG. 14 is an image acquired on fresh mice kidney tissue (i.e., the piece of tissue has been deposited on the instrument). The insert in the image shows a zoomed adipose tissue region and illustrates that the whole image is not showed at full resolution and can be zoomed to reveal further details with appropriate software display tool. Again, the disclosed technology was used to capture an image that represents a digital slice of the fresh tissue—thus, allowing an image of a cross section of the tissue to be taken without actually slicing the tissue.
[0328] As shown in FIG. 15 , an implementation of a network environment 1500 for use providing in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment is shown and described. In brief overview, referring now to FIG. 15 , a block diagram of an exemplary cloud computing environment 1500 is shown and described. The cloud computing environment 1500 may include one or more resource providers 1502 a , 1502 b , 1502 c (collectively, 1502 ). Each resource provider 1502 may include computing resources. In some implementations, computing resources may include any hardware and/or software used to process data. For example, computing resources may include hardware and/or software capable of executing algorithms, computer programs, and/or computer applications. In some implementations, exemplary computing resources may include application servers and/or databases with storage and retrieval capabilities. Each resource provider 1502 may be connected to any other resource provider 1502 in the cloud computing environment 1500 . In some implementations, the resource providers 1502 may be connected over a computer network 1508 . Each resource provider 1502 may be connected to one or more computing device 1504 a , 1504 b , 1504 c (collectively, 1504 ), over the computer network 1508 .
[0329] The cloud computing environment 1500 may include a resource manager 1506 . The resource manager 1506 may be connected to the resource providers 1502 and the computing devices 1504 over the computer network 1508 . In some implementations, the resource manager 1506 may facilitate the provision of computing resources by one or more resource providers 1502 to one or more computing devices 1504 . The resource manager 1506 may receive a request for a computing resource from a particular computing device 1504 . The resource manager 1506 may identify one or more resource providers 1502 capable of providing the computing resource requested by the computing device 1504 . The resource manager 1506 may select a resource provider 1502 to provide the computing resource. The resource manager 1506 may facilitate a connection between the resource provider 1502 and a particular computing device 1504 . In some implementations, the resource manager 1506 may establish a connection between a particular resource provider 1502 and a particular computing device 1504 . In some implementations, the resource manager 1506 may redirect a particular computing device 1104 to a particular resource provider 1102 with the requested computing resource.
[0330] FIG. 16 shows an example of a computing device 1600 and a mobile computing device 1650 that can be used to implement the techniques described in this disclosure. The computing device 1600 is intended to represent various forms of digital computers, such as laptops, desktops, workstations, personal digital assistants, servers, blade servers, mainframes, and other appropriate computers. The mobile computing device 1650 is intended to represent various forms of mobile devices, such as personal digital assistants, cellular telephones, smart-phones, and other similar computing devices. The components shown here, their connections and relationships, and their functions, are meant to be examples only, and are not meant to be limiting.
[0331] The computing device 1600 includes a processor 1602 , a memory 1604 , a storage device 1606 , a high-speed interface 1608 connecting to the memory 1604 and multiple high-speed expansion ports 1610 , and a low-speed interface 1612 connecting to a low-speed expansion port 1614 and the storage device 1606 . Each of the processor 1602 , the memory 1604 , the storage device 1606 , the high-speed interface 1608 , the high-speed expansion ports 1610 , and the low-speed interface 1612 , are interconnected using various busses, and may be mounted on a common motherboard or in other manners as appropriate. The processor 1602 can process instructions for execution within the computing device 1600 , including instructions stored in the memory 1604 or on the storage device 1606 to display graphical information for a GUI on an external input/output device, such as a display 1616 coupled to the high-speed interface 1608 . In other implementations, multiple processors and/or multiple buses may be used, as appropriate, along with multiple memories and types of memory. Also, multiple computing devices may be connected, with each device providing portions of the necessary operations (e.g., as a server bank, a group of blade servers, or a multi-processor system).
[0332] The memory 1604 stores information within the computing device 1600 . In some implementations, the memory 1604 is a volatile memory unit or units. In some implementations, the memory 1604 is a non-volatile memory unit or units. The memory 1604 may also be another form of computer-readable medium, such as a magnetic or optical disk.
[0333] The storage device 1606 is capable of providing mass storage for the computing device 1600 . In some implementations, the storage device 1606 may be or contain a computer-readable medium, such as a floppy disk device, a hard disk device, an optical disk device, or a tape device, a flash memory or other similar solid state memory device, or an array of devices, including devices in a storage area network or other configurations. Instructions can be stored in an information carrier. The instructions, when executed by one or more processing devices (for example, processor 1602 ), perform one or more methods, such as those described above. The instructions can also be stored by one or more storage devices such as computer- or machine-readable mediums (for example, the memory 1604 , the storage device 1606 , or memory on the processor 1602 ).
[0334] The high-speed interface 1608 manages bandwidth-intensive operations for the computing device 1600 , while the low-speed interface 1612 manages lower bandwidth-intensive operations. Such allocation of functions is an example only. In some implementations, the high-speed interface 1608 is coupled to the memory 1604 , the display 1616 (e.g., through a graphics processor or accelerator), and to the high-speed expansion ports 1610 , which may accept various expansion cards (not shown). In the implementation, the low-speed interface 1612 is coupled to the storage device 1606 and the low-speed expansion port 1614 . The low-speed expansion port 1614 , which may include various communication ports (e.g., USB, Bluetooth®, Ethernet, wireless Ethernet) may be coupled to one or more input/output devices, such as a keyboard, a pointing device, a scanner, or a networking device such as a switch or router, e.g., through a network adapter.
[0335] The computing device 1600 may be implemented in a number of different forms, as shown in the figure. For example, it may be implemented as a standard server 1620 , or multiple times in a group of such servers. In addition, it may be implemented in a personal computer such as a laptop computer 1622 . It may also be implemented as part of a rack server system 1624 . Alternatively, components from the computing device 1600 may be combined with other components in a mobile device (not shown), such as a mobile computing device 1650 . Each of such devices may contain one or more of the computing device 1600 and the mobile computing device 1650 , and an entire system may be made up of multiple computing devices communicating with each other.
[0336] The mobile computing device 1650 includes a processor 1652 , a memory 1664 , an input/output device such as a display 1654 , a communication interface 1666 , and a transceiver 1668 , among other components. The mobile computing device 1650 may also be provided with a storage device, such as a micro-drive or other device, to provide additional storage. Each of the processor 1652 , the memory 1664 , the display 1654 , the communication interface 1666 , and the transceiver 1668 , are interconnected using various buses, and several of the components may be mounted on a common motherboard or in other manners as appropriate.
[0337] The processor 1652 can execute instructions within the mobile computing device 1650 , including instructions stored in the memory 1664 . The processor 1652 may be implemented as a chipset of chips that include separate and multiple analog and digital processors. The processor 1652 may provide, for example, for coordination of the other components of the mobile computing device 1650 , such as control of user interfaces, applications run by the mobile computing device 1650 , and wireless communication by the mobile computing device 1650 .
[0338] The processor 1652 may communicate with a user through a control interface 1658 and a display interface 1656 coupled to the display 1654 . The display 1654 may be, for example, a TFT (Thin-Film-Transistor Liquid Crystal Display) display or an OLED (Organic Light Emitting Diode) display, or other appropriate display technology. The display interface 1656 may comprise appropriate circuitry for driving the display 1654 to present graphical and other information to a user. The control interface 1658 may receive commands from a user and convert them for submission to the processor 1652 . In addition, an external interface 1662 may provide communication with the processor 1652 , so as to enable near area communication of the mobile computing device 1650 with other devices. The external interface 1662 may provide, for example, for wired communication in some implementations, or for wireless communication in other implementations, and multiple interfaces may also be used.
[0339] The memory 1664 stores information within the mobile computing device 1650 . The memory 1664 can be implemented as one or more of a computer-readable medium or media, a volatile memory unit or units, or a non-volatile memory unit or units. An expansion memory 1674 may also be provided and connected to the mobile computing device 1650 through an expansion interface 1672 , which may include, for example, a SIMM (Single In Line Memory Module) card interface. The expansion memory 1674 may provide extra storage space for the mobile computing device 1650 , or may also store applications or other information for the mobile computing device 1650 . Specifically, the expansion memory 1674 may include instructions to carry out or supplement the processes described above, and may include secure information also. Thus, for example, the expansion memory 1674 may be provide as a security module for the mobile computing device 1650 , and may be programmed with instructions that permit secure use of the mobile computing device 1650 . In addition, secure applications may be provided via the SIMM cards, along with additional information, such as placing identifying information on the SIMM card in a non-hackable manner.
[0340] The memory may include, for example, flash memory and/or NVRAM memory (non-volatile random access memory), as discussed below. In some implementations, instructions are stored in an information carrier. that the instructions, when executed by one or more processing devices (for example, processor 1652 ), perform one or more methods, such as those described above. The instructions can also be stored by one or more storage devices, such as one or more computer- or machine-readable mediums (for example, the memory 1664 , the expansion memory 1674 , or memory on the processor 1652 ). In some implementations, the instructions can be received in a propagated signal, for example, over the transceiver 1668 or the external interface 1662 .
[0341] The mobile computing device 1650 may communicate wirelessly through the communication interface 1666 , which may include digital signal processing circuitry where necessary. The communication interface 1666 may provide for communications under various modes or protocols, such as GSM voice calls (Global System for Mobile communications), SMS (Short Message Service), EMS (Enhanced Messaging Service), or MMS messaging (Multimedia Messaging Service), CDMA (code division multiple access), TDMA (time division multiple access), PDC (Personal Digital Cellular), WCDMA (Wideband Code Division Multiple Access), CDMA2000, or GPRS (General Packet Radio Service), among others. Such communication may occur, for example, through the transceiver 1668 using a radio-frequency. In addition, short-range communication may occur, such as using a Bluetooth®, Wi-Fi™, or other such transceiver (not shown). In addition, a GPS (Global Positioning System) receiver module 1670 may provide additional navigation- and location-related wireless data to the mobile computing device 1650 , which may be used as appropriate by applications running on the mobile computing device 1650 .
[0342] The mobile computing device 1650 may also communicate audibly using an audio codec 1660 , which may receive spoken information from a user and convert it to usable digital information. The audio codec 1660 may likewise generate audible sound for a user, such as through a speaker, e.g., in a handset of the mobile computing device 1650 . Such sound may include sound from voice telephone calls, may include recorded sound (e.g., voice messages, music files, etc.) and may also include sound generated by applications operating on the mobile computing device 1650 .
[0343] The mobile computing device 1650 may be implemented in a number of different forms, as shown in the figure. For example, it may be implemented as a cellular telephone 1680 . It may also be implemented as part of a smart-phone 1682 , personal digital assistant, or other similar mobile device.
[0344] Various implementations of the systems and techniques described here can be realized in digital electronic circuitry, integrated circuitry, specially designed ASICs (application specific integrated circuits), computer hardware, firmware, software, and/or combinations thereof. These various implementations can include implementation in one or more computer programs that are executable and/or interpretable on a programmable system including at least one programmable processor, which may be special or general purpose, coupled to receive data and instructions from, and to transmit data and instructions to, a storage system, at least one input device, and at least one output device.
[0345] These computer programs (also known as programs, software, software applications or code) include machine instructions for a programmable processor, and can be implemented in a high-level procedural and/or object-oriented programming language, and/or in assembly/machine language. As used herein, the terms machine-readable medium and computer-readable medium refer to any computer program product, apparatus and/or device (e.g., magnetic discs, optical disks, memory, Programmable Logic Devices (PLDs)) used to provide machine instructions and/or data to a programmable processor, including a machine-readable medium that receives machine instructions as a machine-readable signal. The term machine-readable signal refers to any signal used to provide machine instructions and/or data to a programmable processor.
[0346] To provide for interaction with a user, the systems and techniques described here can be implemented on a computer having a display device (e.g., a CRT (cathode ray tube) or LCD (liquid crystal display) monitor) for displaying information to the user and a keyboard and a pointing device (e.g., a mouse or a trackball) by which the user can provide input to the computer. Other kinds of devices can be used to provide for interaction with a user as well; for example, feedback provided to the user can be any form of sensory feedback (e.g., visual feedback, auditory feedback, or tactile feedback); and input from the user can be received in any form, including acoustic, speech, or tactile input.
[0347] The systems and techniques described here can be implemented in a computing system that includes a back end component (e.g., as a data server), or that includes a middleware component (e.g., an application server), or that includes a front end component (e.g., a client computer having a graphical user interface or a Web browser through which a user can interact with an implementation of the systems and techniques described here), or any combination of such back end, middleware, or front end components. The components of the system can be interconnected by any form or medium of digital data communication (e.g., a communication network). Examples of communication networks include a local area network (LAN), a wide area network (WAN), and the Internet.
[0348] The computing system can include clients and servers. A client and server are generally remote from each other and typically interact through a communication network. The relationship of client and server arises by virtue of computer programs running on the respective computers and having a client-server relationship to each other.
[0349] Components described herein may be made of polymer, metal, metalloid, glass, ceramic, or other materials, or composites thereof. In certain embodiments, components are made of surgical grade materials. Components may be sterilizable, autoclavable, reusable, and/or disposable. Disposable components may be designed for single use or limited multi-use (e.g., between 2 and 10 uses).
[0350] In view of the structure, functions and apparatus of the systems and methods described here, in some implementations, a system and method for providing in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment are provided. Having described certain implementations of methods and apparatus for supporting in-operating-theatre imaging of fresh thick tissue resected during surgery for pathology assessment, it will now become apparent to one of skill in the art that other implementations incorporating the concepts of the disclosure may be used. Therefore, the disclosure should not be limited to certain implementations, but rather should be limited only by the spirit and scope of the following claims.
[0351] Having described certain implementations of methods and apparatus for supporting transfer printing capacitors, it will now become apparent to one of skill in the art that other implementations incorporating the concepts of the disclosure may be used. Therefore, the disclosure should not be limited to certain implementations, but rather should be limited only by the spirit and scope of the following claims.
[0352] Throughout the description, where apparatus and systems are described as having, including, or comprising specific components, or where processes and methods are described as having, including, or comprising specific steps, it is contemplated that, additionally, there are apparatus, and systems of the disclosed technology that consist essentially of, or consist of, the recited components, and that there are processes and methods according to the disclosed technology that consist essentially of, or consist of, the recited processing steps.
[0353] It should be understood that the order of steps or order for performing certain action is immaterial so long as the disclosed technology remains operable. Moreover, two or more steps or actions may be conducted simultaneously. | The disclosed technology brings histopathology into the operating theatre, to enable real-time intra-operative digital pathology. The disclosed technology utilizes confocal imaging devices image, in the operating theatre, “optical slices” of fresh tissue—without the need to physically slice and otherwise process the resected tissue as required by frozen section analysis (FSA). The disclosed technology, in certain embodiments, includes a simple, operating-table-side digital histology scanner, with the capability of rapidly scanning all outer margins of a tissue sample (e.g., resection lump, removed tissue mass). Using point-scanning microscopy technology, the disclosed technology, in certain embodiments, precisely scans a thin “optical section” of the resected tissue, and sends the digital image to a pathologist rather than the real tissue, thereby providing the pathologist with the opportunity to analyze the tissue intra-operatively. Thus, the disclosed technology provides digital images with similar information content as FSA, but faster and without destroying the tissue sample itself. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention:
The present invention relates generally to apparatus and methodology for discharging static electricity from a vehicle and, more particularly, to avoiding wear and tear on the electrical conductor which discharges the static electricity to ground.
2. Description of Prior Art:
Static electricity buildup is a fundamental phenomenon of nature, and we all have experienced it in one form or another. Static electricity varies widely in energy level, from a miniscule level where one barely notices an annoying spark at the end of one's finger as one touches a metal object in a dry environment after walking across a carpet, all the way up to the highly dramatic and dangerous lightning flashes during a summer thunderstorm. Both are examples of static electricity discharge.
Static electricity is a bigger problem in dry climates such as the southwest U.S. than in humid climates such as the northeast U.S., because water vapor in places of high humidity forms a natural leakage path for the static electricity. All motor vehicles, trucks, cars, buses etc., can build up static electricity charge relative to ground because their rubber tires can act as insulators between the body of the vehicle and Earth.
Under the wrong conditions, motor vehicle static electricity discharge can be a hazardous event. For example, if a gasoline tanker truck builds up static charge and somehow discharges that static electricity in the presence of fumes from the gasoline in the truck, then an enormous explosion may occur. It is, therefore, important to safely discharge static electricity from vehicles.
Most of us are familiar with the image of a gasoline tanker truck driving down the highway while dragging a steel chain behind, along the roadway. This is a prior art approach which discharges the static electricity while the truck is in motion because of the scraping of the electrically-conductive metal chain against the roadway. Referring to FIG. 1 (Prior Art) truck 100 is shown with truck body 101 , front wheels 102 and rear wheels 103 supported by roadway 104 . Truck body 101 has a metal chain 105 mounted from a conductive contact such as an axel located underneath the truck. The chain is shown to be in substantial contact with roadway 104 . This contact is maintained regardless of whether the truck is in forward motion, is stopped, or is in reverse motion. This may be an effective way to reduce static electricity buildup, but it is only good if the chain is in contact with the roadway. At some point, after a long haul across the country, or after other excessive usage, road friction eventually causes the chain to wear out, and the effective discharge path to ground through the chain becomes intermittent or non-existent. When the truck driver exits the truck through door 106 there could be a static electricity discharge through that individual to ground, if the chain had worn away during transit, and if the driver touches the truck and ground at the same time which is very likely.
Also, there are other kinds of vehicles which can benefit from a safe static discharge path. The assignee of the present invention is a telecommunications company presently involved in installing a fiber to the premises (FTTP) infrastructure. The trucks used by the assignee's installers for this purpose contain a substantial amount of sensitive fiber splicing equipment and other sensitive equipment such as, e.g., line card installation equipment. All of this equipment can be very susceptible to, and negatively affected by, static electricity buildup. Thus, in addition to being a hazard to the technician installer who is driving the truck and who can, unknowingly, form a discharge path through his/her body from the truck to ground upon opening door 106 and setting foot on the ground while touching the truck, static electricity buildup can also wreak havoc with this sensitive equipment inside the truck.
Therefore, there is a need to always have a safe discharge path for static electricity in place from the truck to ground prior to any occupants in that truck opening the door to egress. This requires a technique for avoiding wear-out of the discharge path from road friction. Applicant provides such a technique with the present invention which addresses the problems noted in the prior art.
SUMMARY OF THE INVENTION
Embodiments of the present invention include apparatus and methodology for discharging static electricity from a vehicle on a roadway. Flexible and electrically-conductive material is suspended from beneath the vehicle. The material is sufficiently long to normally be in contact with the roadway when the vehicle is stopped. The material is oriented in a direction relative to the direction of forward motion of the vehicle, and is sufficiently lightweighted, to enable a wind that is created by the forward motion to automatically lift the material from the roadway and break the contact during occurrence of the forward motion. Thereby, the static electricity is discharged from the vehicle through the material to the roadway when the vehicle is stopped, and the material does not experience frictional force from the roadway when the vehicle is moving in a forward direction. In a particular embodiment, the material can be a 6-12 inch wide (approximate) strip of flexible, non-corrosive, electrically-conductive mesh or ribbon fabricated from a suitable alloy such as, for example, stainless steel alloy, brass alloy, etc.
In another embodiment of the present invention, a wind-engagement mechanism is suspended from the vehicle and supports the material. The mechanism is oriented in a direction to encounter wind resistance when the vehicle is moving forward. This causes the mechanism to raise the material from the roadway and break the contact.
In yet another embodiment, the electrically-conductive material can be fabricated from a flexible metal rod or spring. If the material encounters debris and/or holes in the roadway when the vehicle is moving in the reverse direction, damage to the wind-engagement mechanism is avoided by the conductive material being formed from the flexible metal rod or spring, because the end of the rod or spring which makes contact with the roadway is curved upward to permit it to ride over the debris and slide over the holes. Alternatively, the end of the rod can be affixed to a rotatable and electrically conductive metal wheel which makes contact with the roadway and can roll over the debris and the holes. The rod or spring can, likewise, be made from stainless steel or brass or other suitable non-corrosive and electrically-conductive metal.
It is thus a general object of the present invention to provide an improved technique for discharging static electricity from a vehicle.
It is another general object of the present invention to provide an improved technique for discharging static electricity from a vehicle without allowing vehicle motion to wear-out the electrically conductive discharge path between the vehicle and ground.
Other objects and advantages shall become apparent after reviewing the detailed description of the preferred embodiments in conjunction with the drawings in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a prior art technique for static electricity discharge from a vehicle;
FIG. 2 is an exemplary diagram of an embodiment of the present invention when viewing it from the rear of a stationary vehicle from which it is mounted;
FIG. 3 is an exemplary diagram of the embodiment of FIG. 2 when viewing it from the rear of a forward-moving vehicle from which it is mounted.
FIG. 4 is another view of the embodiment of FIG. 3 showing directions of vehicle motion and wind force;
FIG. 5 depicts another embodiment of the present invention which avoids malfunction during vehicle back-up due to debris and/or holes in the roadway; and
FIG. 6 depicts yet another embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 2 is an exemplary diagram of an embodiment 200 of the present invention when viewing it from the rear of a stationary vehicle from which it is mounted. Axel or truck chassis 201 is located underneath the truck body (not shown in this Fig.). Connected to axel 201 is flexible, electrically conductive material strip 205 having a width of several inches and a length sufficient to touch roadway 104 when the truck is not moving, as shown. Material 205 is lightweight and can be lifted or lofted into the air by a breeze or wind created by forward movement, thereby avoiding frictional forces while the truck is moving forward. Wind-engagement screen (or sail or wing) 204 is suspended from axel 201 by flexible supports 202 and 203 . Material 205 is connected to, and supported by, wind screen 204 which projects a larger surface area than material strip 205 projects by itself, and which can, therefore, catch the air flow more efficiently than that being caught by the material strip alone.
However, in another embodiment (not shown) wind screen 204 is not used and apparatus 202 , 203 and 204 do not appear. Flexible material 205 is suspended solely from axel 201 and is lofted by air flow directly. In this other embodiment, as well as the embodiment of FIG. 2 , stones or holes or other obstructions in the roadway during backing-up are not an issue because the flexible material merely accommodates the obstruction by flexing over or around it (e.g., a rock) or sliding through it (e.g., a pothole).
FIG. 3 shows embodiment 200 a , which is the apparatus of FIG. 2 from the same rear viewpoint but under conditions of a forward moving truck. (The “a” designation is used merely to suggest that FIG. 3 is the same as FIG. 2 but under a state of forward motion of the truck. The dimensions of the components look shorter in this view because the components have been raised or lofted because the truck is moving forward, but the components are otherwise identical to those of FIG. 2 ). In this view, material 205 a is the same as material 205 , but lofted so that a clearance of distance “D” is achieved between the end of material 205 a and roadway 104 . Wind-screen 204 a is suspended by flexible supports 202 a and 203 a from axel 201 , as in FIG. 2 . The bracket at the far left of FIG. 3 is merely to indicate that all that is shown in that view is within FIG. 3 .
Referring to FIG. 4 , the components of FIG. 3 are shown in side view. Axel 201 is shown on end. Support 203 a is shown on edge, connecting to wind-screen 204 a which is also shown on edge. Conductive strip 205 a is shown on edge being supported by wind-screen 204 a . Clearance “D” is shown in this Fig. as well, and is the same distance “D” shown in FIG. 3 . Wind force is directed from the left of the diagram, as shown, as truck 100 moves forward, to the left side in FIG. 1 . Wind-screen 204 a may typically be sized with dimensions of three feet by one foot, but the dimensions can vary depending on the size and shape of the truck under which it is attached. The material from which the wind-screen is made can also vary; it needs to be lightweight and weather-resistant. A light, stiff plastic material or other similar material would he suitable for this purpose.
In operation, referring to FIGS. 1-4 , assuming truck 100 was carrying embodiment 200 / 200 a under its carriage rather than chain 105 , as truck 100 drives to the left and picks up speed, the wind or breeze created underneath the truck by virtue of its velocity directs wind force against windscreen 204 which causes it to rotate around an axis co-linear with axel 201 . That rotation lifts flexible conductive material 205 into the air and creates a clearance of dimension “D” between the end of the conductive material and road surface 104 . This clearance reduces the wear opportunities which otherwise would occur upon conductive material 205 , and greatly enhances the life of this material. Otherwise, friction forces from road surface 104 being in contact with conductive material 205 while the truck is driving down the road would wear away the material until it no longer made contact with the road surface whereby its effectiveness in grounding the static electricity charge on truck 100 would be substantially if not completely reduced.
Thereafter, when truck 100 comes to a stop, the wind forces on structure 204 are reduced to zero and the force of gravity causes material 205 to make contact with roadsurface 205 (with the Earth). This happens prior to the truck completely stopping and well-prior to anyone inside the truck opening door 106 and disembarking. This is important because it prevents the possibility of the truck driver/passenger from experiencing a static electricity shock, since the grounding from the truck is automatic, instantaneous and in place before the truck occupants open the door (the door is not opened until the truck stops and the static discharge contact between material 205 and roadway 104 is made just as the truck is stopping and before the door is opened.) A motion-limiting strap (not shown) could be attached between windscreen 204 a and the underside of the chassis of the truck so that the downward displacement of windscreen 204 a is limited to a safe clearance above the roadway. It is not important, or desirable, for windscreen 204 a to contact the roadway when the vehicle is stopped; it is important only for the flexible conductive strip to contact the roadway when the vehicle is stopped.
In the embodiment earlier mentioned in which apparatus 202 , 203 and 204 are not used, where material 205 is suspended only by axel 201 , the fluttering material 205 during vehicle forward motion may possibly still come in contact with the roadway intermittently, depending on vehicle speed, weather conditions, etc. But, this is not equivalent to, and a vast improvement over, the constant wear of the chain discharge mechanism of the prior art. However, if one were to use the embodiment with windscreen 204 , this may be an improvement because windscreen 204 may add loft stability to the fluttering discharge material, thereby reducing frequency of contact between material and roadway or eliminating it completely.
FIG. 5 depicts an embodiment which addresses a backing-up situation where there may be obstructions or potholes in the roadway. In the prior Figs., this was not an issue because material 205 is flexible and therefore would not get locked on a stone lying on the roadway, or in a pot hole formed in the roadway. The flexible material would simply flex around the obstruction or within the hole. However, if other embodiments of the present invention are utilized, such as a conductive rod or spring, although it would not have an issue in proper functioning when moving forward, it could jam against a rock or lodge in a pot hole when the truck is moving backward. In FIG. 5 , electrically-conductive rod or spring 505 is depicted which, in this view, has a similar thickness appearance to that of conductive strip 205 a . However, although rod or spring 505 is flexible, it is not as flexible as material 205 . Therefore, a large curve is formed in the rod or spring to enable it to ride over rocks in the roadway and to slide across potholes in the roadway.
An alternative embodiment in Fig. 6 would connect rod 505 , labeled 605 in Fig. 6 , to a conductive rotatable metallic wheel 606 where the wheel is in contact with roadway 104 and has the ability to roll-over rocks and roll across potholes when the truck is moving in a reverse direction. Axel 201 , depicted in Fig. 6 as axel 601 , of a vehicle chassis underside 600 supports metal rod 605 at one end, the other end of the rod being connected to wheel hub 608 of rotatable metal wheel 606 with metal spokes 607 . Wheel 606 rolls over roadway 104 when the vehicle moves.
Other more elaborate controls can be instituted as well. A magnetic mechanism 602 which directs a magnetic field 603 from the under chassis 600 to the metal rod 605 can be fashioned, where such field is automatically energized anytime the transmission of the truck is placed in reverse gear. That magnetic force can be used to lift the rod so that it avoids all contact with the roadway when the truck is moving in reverse. Additional controls can be instituted, utilizing the magnetic mechanism, where the rod is held in place above the roadway when the transmission of the truck is placed in any forward gear. Thus, the rod can be held off the ground e.g., at position 604 , by magnetic force during forward motion of the truck as well. The critical factor is that contact is made with the roadway no later than the opening of the doors of the truck, and an interlock mechanism with the doors can be used for that purpose, where any door opening causes an over-ride to the energizing of the magnetic mechanism which, in turn, causes the metal rod to fall to the ground. However, these are more elaborate and more expensive controls, and the windscreen technique embodiment and/or the flexible conductive mesh without the windscreen embodiment can perform satisfactorily.
While several illustrative embodiments of the present invention have been shown and described, numerous variations and alternative embodiments may occur to those skilled in the art. Such variations and alternative embodiments are contemplated, and can be made without departing from the spirit and scope of the present invention as defined in the appended claims. | Apparatus and methodology for discharging static electricity from a vehicle which uses a discharge mechanism that does not contact the roadway (Earth) when the vehicle is in forward motion to reduce, or completely avoid, frictional wear on the discharge mechanism. In one embodiment, the displacement between the discharge mechanism and the roadway is obtained by way of wind force generated by the motion of the vehicle itself. A properly oriented and hinged windscreen attached to the conductive path discharge mechanism can be used for this purpose. Other embodiments including magnetically controlled lifting and holding devices can be used. | 1 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of International Application No. PCT/EP2015/062363, filed Jun. 3, 2015, which claims priority to German patent application No. 10 2014 210 518.8, filed Jun. 3, 2014.
TECHNICAL FIELD
[0002] The technical field relates to a steering angle sensor for detecting a steering angle.
BACKGROUND
[0003] A steering angle sensor is known from the document DE 10 2004 023 801 A1 that can detect a steering angle of a steering column over a range of angles of greater than 360° in a vehicle.
[0004] It is an object to improve the known steering angle sensor.
BRIEF SUMMARY
[0005] According to one aspect, a steering angle sensor for detecting a steering angle of a steering column over a range of angles greater than 360° in a vehicle comprises a transmitter element for exciting a transmitter field and a measuring sensor for stimulating an output signal depending on the reception of the transmitter field, wherein the measuring sensor and the transmitter element are disposed so that the transmitter field received by the measuring sensor is a function of the detected angle of rotation of the steering column, and a counting element with a non-volatile memory for counting and outputting a number of revolutions of the transmitter element relative to a reference angle of rotation.
[0006] The specified steering angle sensor is based on the idea that the steering angle could be used for detecting a driver's intention. This can be used in vehicle components, such as current driver assistance systems, such as, for example, the electronic stability program known as ESP or in steering assistance systems known as EPS, in order to derive therefrom a target value. Just recently, the detection of the steering angle over a plurality of revolutions of the steering column is required for this, even if the steering angle sensors are not supplied with electrical energy over a certain period of time. Such sensors are known as True Power On Sensors.
[0007] The steering angle sensor is such a True Power On Sensor and is equipped with a mechanical gearbox for determining an absolute angular position over a plurality of revolutions. The gearbox and the resulting transmission ratio enable a plurality of signals to be generated using sensor elements. In this case the periodicity or the phase position of the individual signals relative to each other, i.e. the relationship thereof to each other, enables the determination of the absolute angular position over a plurality of revolutions of the steering column.
[0008] A disadvantage of a prior art steering angle sensor is the large number of components used, since for each signal line a transmitter element known as a measuring element, for example in the form of a magnet and a measuring sensor, as well as a computing unit for determining the absolute position based on the different signal lines, are also necessary.
[0009] This is where the specified steering angle sensor implements the proposal of counting the number of revolutions with a counting element. This enables only one signal line to be necessary for determining the absolute angular position. So that the specified steering angle sensor can be used as a True Power On Sensor, the result of the counting element is placed in a non-volatile memory, which can also be read out if the steering angle sensor has not been supplied with electrical energy over a period of time.
[0010] In a development of the specified steering angle sensor, the transmitter field is a magnetic field. This enables a suitable magnetic measuring sensor, such as a magnetoresistive measuring sensor based on the AMR effect, the TMR effect or the GMR effect or a magnetic measuring sensor directly detecting the magnetic field, which are inexpensive, accurate and robust, to be used as a measuring sensor.
[0011] In an additional development of the specified steering angle sensor, the non-volatile memory comprises at least two magnetizable memory elements that are connected together in series, the magnetization of which can be adjusted by a magnetic source depending on the number of revolutions of the transmitter field. Owing to the series connection of the two magnetizable memory elements, a counting effect can be achieved directly, since the magnetic source cannot magnetize all the magnetizable memory elements connected in series at once, but only sequentially with each full revolution of the steering column. This enables a certain degree of magnetization of the individual magnetizable memory elements that are connected in series to be uniquely associated with a completely defined number of full revolutions of the steering column. During this the full revolutions in both directions of rotation of the steering column are automatically taken into account using a corresponding sign.
[0012] In a particular development of the specified steering angle sensor, the memory elements are disposed in a spiral, as a result of which the magnetization that is described above of the individual magnetizable memory elements that are connected in series can be carried out most effectively sequentially.
[0013] In an additional development, the specified steering angle sensor comprises a readout device for reading out the magnetization of the memory elements and for outputting the number of revolutions of the transmitter element depending on the magnetization of the memory elements that has been read out. As the individual magnetizable memory elements that are connected in series influence the overall magnetization by boosting it or clearing it, depending on the magnetization direction, a definite number of full revolutions of the steering column can be associated with a certain range of values for the overall magnetization. Therefore, the readout device could be a characteristic curve for example.
[0014] Alternatively, the readout device could also read out the magnetization of the individual memory elements separately and thus a digital value for the number of full revolutions of the steering column could be obtained based on the individual magnetizations.
[0015] In another development of the specified steering angle sensor, the transmitter element is designed to output a transmitter field in the axial direction of the shaft. This enables the measuring sensor and the counting element to be disposed one above the other looking in the axial direction of the shaft, so that a single transmitter field can be used in order to count the number of full revolutions of the steering column and to detect the angular position of the steering column within a full revolution at the same time.
[0016] In yet another development of the specified steering angle sensor, the transmitter element comprises a first semicircular circle segment disk for outputting a first pole of the transmitter field and a second semicircular circle segment disk for outputting a second pole of the transmitter field, the segment section regions of which are disposed facing each other. This enables the counting of the full revolutions of the steering column to be achieved with the lowest number of magnetizations of the aforementioned magnetizable memory elements.
[0017] In a preferred development of the specified steering angle sensor, the transmitter element is disposed on a gear wheel that is disposed coaxially to the steering column and that is driven by a peripheral toothing disposed around the steering column. This enables the transmitter element to be positioned axially offset to the steering column in order that the transmitter field can be output in the aforementioned way in the axial direction to the steering column.
[0018] In a particularly preferred development, the specified steering angle sensor comprises further toothing disposed peripherally around the steering column, whereby a torsion element is disposed axially between the two toothings. The torsion element is then elastically twisted during a steering process, so that the steering torque applied by the driver can be determined therefrom. This enables the information that can be detected with the specified steering angle sensor to be increased further.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The properties, features and advantages that are described above, as well as the manner in which the same are achieved, are clearly and fully understandable in combination with the following description of the exemplary embodiments, which are described in detail in combination with the figures, wherein:
[0020] FIG. 1 shows a vehicle with a steering system in a schematic view according to one exemplary embodiment,
[0021] FIG. 2 shows the steering system from FIG. 1 in a schematic view,
[0022] FIG. 3 shows a steering angle sensor in the steering system of FIG. 2 in a schematic top view,
[0023] FIG. 4 shows a steering angle sensor in the steering system of FIG. 2 in a perspective view,
[0024] FIG. 5 shows a measuring sensor in the steering angle sensor of FIGS. 3 and 4 in a schematic top view, and
[0025] FIG. 6 shows a steering angle sensor of another exemplary embodiment in a perspective view.
[0026] In the figures, identical technical elements are provided with identical reference characters and are only described once.
[0027] Reference is made to FIG. 1 , which shows a basic representation of the vehicle 2 with a driving dynamics controller installed in the vehicle. Details of a driving dynamics controller can be obtained from DE 10 2011 080 789 A1 for example.
[0028] Each wheel 6 of the vehicle 2 can be decelerated relative to the chassis 4 by means of a brake 8 that is fixedly attached to the chassis 4 in order to slow down the movement of the vehicle 2 on a road that is not shown further.
[0029] In doing so, it can happen in a way that is known to the person skilled in the art that the wheels 6 of the vehicle 2 can lose the adhesion thereof to a road that is not shown further and that the vehicle 2 can even be deviated from a trajectory that is predetermined for example by means of a steering wheel that is not shown further by understeer or oversteer. The trajectory can, for example, be predetermined from a steering angle 12 detected by means of a further motion detecting sensor in the form of a steering angle sensor 10 . This is prevented by known control circuits such as ABS (anti brake locking system) and ESP (electronic stability program). In such control circuits, measurement data are detected by sensors. Controllers compare the measurement data with target data and control the measurement data to the target data by means of final control elements.
[0030] In the present implementation, the vehicle 2 comprises as sensors the revolution rate sensors 14 on the wheels 6 that detect as measurement data the respective revolution rates 16 of the wheels 6 . The vehicle 2 further comprises as a sensor the inertial sensor 18 , which detects the vehicle dynamic data 20 of the vehicle 2 as measurement data.
[0031] Based on the detected revolution rates 16 and vehicle dynamic data 18 , a controller 22 can determine in a way known to the person skilled in the art whether the vehicle 2 is skidding on the road or even deviating from the aforementioned predetermined trajectory and can react thereto accordingly with a known controller output signal 24 . The controller output signal 24 can then be used by a control device 26 to activate by means of control signals 28 control elements such as the brakes 8 , which respond to skidding and deviation from the predetermined trajectory in a known way.
DETAILED DESCRIPTION
[0032] We refer to FIG. 2 , which shows a steering system 30 for the vehicle of FIG. 1 .
[0033] The steering system 30 comprises a steering wheel 32 mounted on a steering column 34 , which is in turn disposed to be rotatable about a rotation axis 36 . Using the steering wheel 32 , a driver of the vehicle, which is not shown further, predetermines the steering angle 12 that is to be detected, with which the wheels 6 of the vehicle are to be turned by means of a steering gearbox 37 . For this purpose, the driver of the vehicle turns the steering wheel 32 with a torsional force or rotational force 38 until the wheels 6 have reached the desired steering angle 12 . The rotational force 38 that is to be applied to turn the steering wheel 32 can however be very tiring for some drivers.
[0034] Therefore, within the context of the present implementation the rotational force 38 exerted on the steering column 34 is measured with the steering angle sensor 10 in addition to the angle of rotation 12 and is output to a driving device 40 in the form of a drive motor. The driving device 40 turns the steering column 34 in the same direction as the rotational force 38 and thus keeps the rotational force 38 to be applied by the driver below a defined threshold value, so that the driver can turn the steering wheel 32 with comparatively little effort.
[0035] We refer to FIG. 3 and FIG. 4 , which show the steering angle sensor 10 without a detection capability for the rotational force 38 in a schematic view.
[0036] The steering angle sensor 10 comprises a first gear wheel 42 that is rotationally fixedly mounted on the steering column 34 and that is coupled to a second gear wheel 44 by meshing. A transmitter element 46 in the form of an encoder magnet is disposed on the second gear wheel 44 , being formed by a semicircular segment-shaped North magnetic pole 48 and a semicircular segment-shaped South magnetic pole 50 that stimulate a magnetic transmitter field 52 in the axial direction of the steering column 34 . During the rotation of the steering column 34 , the transmitter magnetic field 52 rotates with the column with the steering angle 12 relative to the chassis 4 of the vehicle 2 , so that the steering angle 12 can be detected by means of the transmitter magnetic field 52 .
[0037] The transmitter magnetic field 52 passes through a magnetoresistive measuring sensor 54 that is disposed positionally fixedly relative to the chassis 4 and that is configured to detect the transmitter magnetic field 52 that is rotatable with the steering column 34 relative to the chassis 4 . In doing so the strength of the transmitter magnetic field 52 detected by the magnetoresistive measuring sensor 54 depends on the rotational position angle of the transmitter magnetic field 52 relative to the chassis 4 and as a result on the steering angle 12 that is to be detected. Accordingly, a measurement signal that is not shown further and that is a function of the steering angle 12 can be generated with the magnetoresistive measuring sensor 54 and can be output for example to the controller 22 as shown in FIG. 1 .
[0038] Besides the magnetoresistive measuring sensor 54 , the steering angle sensor 10 further comprises a counting element 56 . The counting element 56 is intended to detect the number of revolutions of the steering column 34 and is illustrated in detail below using FIG. 5 .
[0039] The counting element 56 comprises a domain generator 58 , through which the magnetic transmitter field 52 passes. A series circuit of magnetizable memory elements 60 is connected to the domain generator 58 . The magnetizable memory elements 60 are made of a magnetizable material that is divided without an external magnetic field into Weiss regions separated by means of Bloch walls, the magnetic fields of which cancel each other out in total. The domain wall generator 58 applies an external magnetic field based on the transmitter magnetic field 52 to the magnetizable memory elements 60 , which aligns the individual Weiss regions of the magnetizable memory elements 60 bounding on the domain generator 58 up to a domain wall 62 at the end of the magnetizable memory element 60 in a preferred direction dependent on the transmitter magnetic field 52 . If the transmitter magnetic field 52 rotates by 180°, then a further domain wall 62 is generated at the end of the adjacent next magnetizable memory element 62 , during which the Weiss regions in the magnetizable memory element 62 are also aligned. The process repeats with each rotation of the transmitter magnetic field 52 by 180°, whereby the entire counting element 56 acts as a shift register. If, however the direction of the transmitter magnetic field 52 changes, then initially the domain walls 62 are again sequentially disrupted in a descending sequence and thereby the shift register is cleared until, once all domain walls 62 have been cleared, new domain walls can be built up.
[0040] Thus in order to determine the number of revolutions of the steering column 34 , the overall magnetization of the individual magnetizable memory elements 62 only needs to be read out. This can be carried out in any arbitrary manner, such as for example by determining the total magnetic resistance of the series circuit of the magnetizable memory elements 60 .
[0041] If the number of revolutions of the steering column 34 is determined in the previously described manner, the steering angle 12 together with the aforementioned measurement signal that is dependent on the steering angle 12 can be indicated in a range of more than 360°.
[0042] The steering angle sensor 10 can, as shown in FIG. 6 , be extended by a further first gear wheel 64 that is axially spaced apart from the first gear wheel 42 and that meshes with a further second gear wheel 66 that is axially spaced apart from the second gear wheel 44 , so that the further second gear wheel 66 is rotated during the rotation of the steering column 34 . A further transmitter element 68 that is constructed similarly to the transmitter element 46 is mounted on the further second gear wheel 66 , the further transmitter field of which, which is not shown, is detected by a further measuring sensor 70 . This enables the steering angle 12 of the steering column 34 to be detected at two different axially spaced positions of the steering column 34 . Between the two axially spaced positions, a torsion element 72 is disposed that is torsioned during rotation of the steering column 34 . Owing to the torsion element 72 , there is an angle difference between the two axially spaced positions that is dependent on the steering force of the driver for rotation of the steering column 34 , so that the steering force can be determined based on the angle difference and the torsional properties of the steering column 34 .
[0043] The present invention has been described herein in an illustrative manner, and it is to be understood that the terminology which has been used is intended to be in the nature of words of description rather than of limitation. Obviously, many modifications and variations of the invention are possible in light of the above teachings. The invention may be practiced otherwise than as specifically described within the scope of the appended claims. | The invention relates to a steering angle sensor for detecting a steering angle of a steering column over an angular range of more than 360° in a vehicle, comprising—a transmitter element for exciting a transmitter field and a measuring sensor for exciting an output signal dependent on a reception of the transmitter field, wherein the measuring sensor and the transmitter element are arranged such that the transmitter field received by the measuring sensor is dependent on the steering column rotational angle to be detected, and—a counter element with a non-volatile storage unit for counting and outputting a number of revolutions of the transmitter field with respect to a reference rotational angle. | 1 |
BACKGROUND OF THE INVENTION
The present invention relates to a method for surface treatment of friction members like brake discs, drums, clutch parts and, more particularly, to treatment of PMMC based members and friction members provided thereby.
Conventional brake discs are presently made of ferrous alloys/cast iron having satisfactory performance and remaining operative even at substantially elevated temperatures up to and above 700° C.
However, the present tendency in the automotive industry to reduce the total weight of vehicles challenges new lighter materials to also penetrate this particular segment of vehicle construction. Furthermore, improved corrosion resistance, as well as wear resistance, which increase the lifetime of the friction members up to the expected life period of the vehicles, are traits when looking for replacement of the present ferrous materials.
Consequently, several patent applications have been filed world-wide recently disclosing use of PMMC (Particle Metal Matrix Composite, such as an Al-alloy matrix reinforced by ceramic particles) based components used for different actual applications in vehicles. Shortcomings in common for all these applications based on PMMC base material are a softening phenomena at elevated temperatures, something which results in scoring and even plastic deformation of the members' surface, thus considerably limiting the maximum allowed operating temperatures of the members. Therefore, as a remedy, it is instrumental to provide the basic PMMC-made friction members either with a special composite/-ceramic coating layer (thermal spraying of ceramics), or with a transfer surface layer.
The provision of an alternative transfer layer requires the layer to be both stable (adherent to the substrate and reliable) and homogeneous. Furthermore, fast formation of the layer having a sufficient thickness is also important both from a manufacturing, cost and performance point of view.
One feasible way to cope with the task of increasing the maximum operating temperature is simply to increase the volume percentage of reinforcing particles. Unfortunately, two major disadvantages connected with this “solution”, namely increased costs of the PMMC base material and difficulties related to production/casting and especially cutting/-machining of the surface, eliminate this as a possibility for a cost efficient manufacturing method.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a novel, fast and cost efficient method of manufacturing friction members that avoid the above mentioned drawbacks and difficulties connected to the conventional methods and products. Another object of the present invention is to provide a fast developing and homogeneous transfer layer exhibiting more stable friction properties, especially at high operating temperatures. Still another object of the present invention is to provide better protection for the base matrix material against scoring. Still another object of the present invention is to provide better protection for the base matrix material against scoring. These and other objects and features of the present invention are met by a method of manufacturing friction members as discussed below.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described in detail in the following by way of examples of preferred embodiments of the manufacturing method and the resulting members referring to FIGS. 1-4, wherein:
FIG. 1 is a perspective view showing a typical disc brake system;
FIG. 2 is a schematic view illustrating, in principle, the novel surface topography of the friction member treated in accordance with the present invention;
FIG. 3 is a microscope image of an untreated surface; and
FIG. 4 is a microscope image showing the same surface of FIG. 3, but after exposure to an etching agent as described in the following under Examples.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIGS. 1 and 2, FIG. 1 shows a disc brake system 1 in which the brake disc 11 is the rotating part which together with the friction linings 15 held in place by the caliper 13 creates the friction. Although a brake disc is shown in the drawings, the present invention is also applicable to clutch plates.
The novel surface treatment according to the invention is applied to the friction surfaces 12 of the brake disc.
FIG. 2 illustrates schematically a detailed view of the surface of the member (disc) 12 treated in accordance with the present invention.
Contrary to the present practice and trend to add a special surface layer (e.g., in the form of a composite or sprayed ceramic layer) the gist of the present novel treatment method lies in a selective partial removal of the base matrix material from the active to be frictional surface(s) of the member.
FIG. 2 shows in a cross sectional view the (top) surface 2 of the brake disc 11 in which the original top layer depicted as 23 is removed, most advantageously by chemical etching. This treatment results in a novel surface topography including a surface with reinforcing (ceramic) particles 22 protruding from the matrix 21 . Later, during the initial break-in activation of the brake system, the particles 22 become an integrated part of the transfer layer created through initial wear and material transfer from the lining (pad) material. The resulting increased reinforcement of the transfer layer will provide better protection of the matrix alloy from temperature and shear forces.
Tests conducted on samples of PMMC discs surface treated in accordance with this method confirm formation of a fast developing adherent and homogenous transfer layer exhibiting substantially improved performance characteristics of the treated member.
Furthermore, tests have shown that etching increases the pad wear during the initial use of the disc during the creation of the transfer layer. The degree of etching should therefore be chosen to reach an acceptable initial pad wear. After creation of the transfer layer the actual pad wear falls to a lower level.
EXAMPLES
Samples of brake discs made of two different AlSiMg matrix alloys reinforced by SiC particles in an amount of 10 to 30 vol % having a size in a range from 5-30 μhave been subjected to chemical etching applying a solution of NaOH in concentrations from 5-30% up to 20 minutes. Comparison to the reference samples based on the measurement of surface roughness, friction and performance at elevated temperatures shows improved characteristics on all measured parameters.
A relatively short etching time proved to be adequate to remove a sufficient amount of the aluminium matrix, allowing the SiC particles to protrude from the surface of the brake disc as illustrated by the attached FIGS. 3 and 4 showing sample surfaces before and after the etching treatment according to the present invention, respectively.
The actually-applied disc brake samples were made of AlSiMg alloy added 20 weight % of SiC particles. The surfaces 2 of the brake discs 11 were exposed for a period of 2 minutes to 12 weight % water solution of NaOH. (Reference number 3 depicts an Al-foil material applied on the samples as protection for the surfaces prior to microscopic evaluation of the achieved results).
As clearly illustrated in FIG. 4, an exposure time of 2 minutes was sufficient to provide an etched surface 2 with SiC particles 4 protruding from the surface 2 .
Generally, an etching time from 1-3 minutes and an application of 12.5 weight % NaOH solution at room temperature is apparently sufficient to achieve an adequate degree of etching of the surface. Prolonged etching (in excess of 5 minutes) can result in loosening of SiC particles. The temperature and the control of the flow of the etching agent will determine the choice of optimal etching time.
The present invention is not limited to the above-described examples of the preferred mode of the surface treatment. Thus, other (similar) methods of surface treatment (such as electrochemical pickling or chemical etching by means of an appropriate acid) could be used without departing from the spirit and scope of the present invention. In addition, alkali-based etching agents other than the exemplified NaOH, such as KOH, could be used. Also, other types of PMMC material with other reinforcing particles like Al 2 O 3 instead of the above described SiC-reinforced Al-matrix are the most practical alternatives. | A method of surface treatment of friction members includes providing a friction member made of PMMC material. A transfer layer is formed on the active surface of the friction member of removing the top layer of the matrix material to expose a surface with the embedded reinforcing particles. | 2 |
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